Carbon materials

Abstract

There is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, the method comprising the steps of: heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor; further heating the meltable organic precursor to a predetermined treatment temperature to form a treated organic precursor, the predetermined treatment temperature being at least 200°C in excess of the melting point of the meltable organic precursor; and cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material. Related methods and products are also provided.

Description

[0001] P / 91817

[0002] CARBON MATERIALS SUMMARY

[0003] This invention relates to carbon materials and composites derived from polymers, with a particular focus on thermoplastic polymers, and more specifically waste thermoplastic polymers, along with their various applications. Aspects of the invention include polymer-derived glassy carbon materials, methods for their preparation, and their uses. The disclosed glassy carbon materials may exhibit diverse morphologies and structures, such as crystallineshaped particles, particles with smooth or textured surfaces, porous glassy carbon particles, and porous glassy carbon particles integrated with carbonate rod-like crystals, such as calcite. These glassy carbon particles are applicable to a variety of uses, including electrodes for metal-ion batteries, abrasives, and more. The invention further discloses the consolidation of such glassy carbon particles to fabricate consolidated objects for specific applications. Additionally, the invention discloses nano-crystalline graphitic coating or glassy carbon coatings, methods for their production, and their applications. The thermoplastic polymer-derived carbon materials described herein, available as particles, composites, consolidated objects and coating, demonstrate superior physical, mechanical, chemical, and / or electrochemical properties compared to certain other materials. These properties make them suitable for a wide range of applications, including, but not limited to, inert electrodes for electrolysers, such as inert anodes used in molten oxide and molten salt electrolysers for metal and alloy production, supports for catalysts, energy storage devices, precursor materials for diamond production, and materials for consumer goods, automotive and related applications.

[0004] TECHNICAL FIELD AND CHALLENGES

[0005] This invention relates to the technical fields of materials science and chemical engineering, with a particular focus on fabrication methods for materials comprising particles, composites, objects, and coatings containing carbon materials derived from precursor materials comprising virgin or waste thermoplastic polymers. The invention addresses methods of production and various applications of such materials, contributing to the broader technical field of waste valorisation. This is a demanding topic since the utilisation of waste thermoplastic polymers for the preparation of advanced materials for high-end applications provides both economic and environmental benefits. For instance, thermoplastics were produced at an unprecedented annual rate exceeding 398 million tons in 2020, with projections predicting over 501 million tons by 2030 and 598 million tons by 2050 (www.statista.com). This significant increase in production contributes substantially to plastic waste, particularly due to the widespread single-use nature of many thermoplastic products, which leads to the accumulation of these plastics after they are retired from use. These prospects highlight the challenge of preventing these predominantly non-biodegradable substances from being disposed of in landfills, nature, and eventually oceans, while also providing economic value to offset the resources spent on the waste collection and sorting. Additionally, this invention relates to carbon materials in various forms, such as objects, composites, and coatings, derived from thermoplastic polymers, which exhibit enhanced properties compared to certain other alternative materials for certain practical applications. The production of high-performing materials using low-cost glassy carbon materials disclosed in this application can ease the extensive utilisation of critical materials, including critical minerals, by their partial or total substitution.

[0006] BACKGROUND

[0007] This invention refers to glassy carbon as a term used to describe a carbon material characterised by a disordered or low-crystalline carbon structure with a vitreous appearance, and a limited number of sp2open-ended bonds, including regions of small graphite-like units that are partly stacked but mismatched with terminated edges. The term glassy carbon may include carbon materials containing nano-crystalline graphitic domains. These characteristics may conferP / 91817

[0008] the glassy carbon materials enhanced properties compared to certain other carbon materials, such as graphitic carbons. These include greater resistance to thermal, chemical, and electrochemical oxidation, as well as higher hardness and improved resistance to corrosion, mechanical erosion, and abrasion. As such, glassy carbons can offer advantages in various applications where the aforementioned properties are critical or desirable.

[0009] In defining the morphological aspects of the glassy carbon particles various terms are used. Porous surfaces can have two types of holes defined as through-holes (holes that pass entirely through the particle, being open on both sides, allowing light or material to pass through) and blind holes (holes that are open at the surface but have a closed bottom, meaning they do not extend through the entire particle).

[0010] Glassy carbon materials are produced by carbonising precursors formed through the moulding and curing of thermosetting resins, such as furan-based or phenol-based resins (JP49027266B, JP63064906A, US20030161781A1) or aromatic epoxy resins (US9428389), in a non-oxidising gas atmosphere. During the curing process, a cross-linked structure forms via a polycondensation reaction of the thermosetting resin precondensate, rendering the polymers rigid. As a result, the carbonisation proceeds in the solid phase, expelling a significant amount of volatile components generated during the thermal decomposition of the precursor resin. While these methods are well-suited for producing small-sized objects, the preparation of larger objects poses considerable challenges. In precursors with greater thickness, pyrolysis gases cannot be efficiently discharged from the solid phase, leading to defects such as voids, swelling, and cracks in the resultant carbon materials. Consequently, producing glassy carbon materials with thicknesses typically exceeding one centimetre has proven difficult and expensive using conventional technologies. This limitation significantly increases the cost, and restricts the production of large-sized glassy carbon objects, thereby impeding their broader industrial applications. In contrast to traditional methods that utilise thermosetting polymers, this invention employs thermoplastic polymers as precursor materials for the preparation of glassy carbon. This approach offers opportunities to fabricate a diverse range of glassy carbon morphologies and structures. Consequently, it enables the production of glassy carbon particles, objects, and coatings of various sizes, which exhibit enhanced properties for specific applications compared to conventional materials.

[0011] SUMMARY OF INVENTION

[0012] Various aspects of this disclosure are set out below.

[0013] First aspect - general method

[0014] According to a first aspect of the disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, the method comprising the steps of:

[0015] heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor;

[0016] further heating the meltable organic precursor to a predetermined treatment temperature to form a treated organic precursor, the predetermined treatment temperature being at least 200°C in excess of the melting point of the meltable organic precursor;

[0017] optionally maintaining the treated organic precursor at, or above, the predetermined treatment temperature for a predetermined period of time; and

[0018] cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material.

[0019] Features set out below, before the next aspect is introduced, are applicable to the first aspect. They may also be applicable to other aspects.

[0020] Advantageously, the method may produce glassy carbon, a material useful for many applications.P / 91817

[0021] The thermal treatment of the meltable organic precursor may include all of the heating, further heating, maintaining (where present), and cooling steps.

[0022] Optionally, the predetermined treatment temperature is in excess of 400°C, for example in excess of 450°C, for example in excess of 500°C, or in excess of 550°C, or in excess of 600°C. Advantageously, a higher temperature may increase yield of suitable, for example glassy, carbon material.

[0023] Optionally, the meltable organic precursor is heated to a maximum predetermined treatment temperature of 3000°C or lower, for example 2000°C or lower, or 1500°C or lower, preferably in which the maximum predetermined treatment temperature is 1300°C or lower, for example 1200°C or lower, or 1100°C or lower, or 1000°C or lower. Advantageously, a lower temperature may save energy.

[0024] Optionally, the predetermined treatment temperature is between 500°C and 2000°C, for example between 500°C and 1500°C, for example between 550°C and 1200°C, for example between 600°C and 1000°C, for example between 700°C and 900°C, for example between 750°C and 850°C or between 700°C and 800°C. It may be particularly preferable that the predetermined treatment temperature is between 700°C and 900°C. Advantageously, such ranges may provide a good yield of suitable, for example glassy, carbon material without excessive energy usage.

[0025] The features relating to the predetermined treatment temperature in the above three paragraphs may apply to the predetermined treatment temperature of any aspect of this disclosure.

[0026] Optionally, the predetermined period of time that the treated organic precursor is maintained at, or above, the predetermined treatment temperature is between 0.1 seconds and 48 hours, for example between 1 second and 12 hours, preferably between 30 seconds and 6 hours, for example between 60 seconds and 2 hours, or between 2 minutes and 1 hour, for example between 5 minutes and 45 minutes. Advantageously, such ranges may provide a good yield of suitable, for example glassy, carbon material without excessive energy usage.

[0027] Optionally, thermal treatment of the meltable organic precursor, such as one or both of the steps of heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor and further heating the meltable organic precursor to a predetermined treatment temperature, includes the step of heating the meltable organic precursor at a heating rate of between 1°C per minute and 100°C per minute, for example between 2°C per minute and 75°C per minute, for example between 5°C per minute and 50°C per minute. Advantageously, such heating rates may provide a good yield of suitable, for example glassy, carbon material.

[0028] Optionally, thermal treatment of the meltable organic precursor, such as the step of cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material, includes the step of cooling the treated organic precursor at a cooling rate of between 1°C per minute and 100°C per minute, for example between 2°C per minute and 75°C per minute, for example between 5°C per minute and 50°C per minute. Advantageously, such cooling rates may provide a good yield of suitable, for example glassy, carbon material.

[0029] Optionally, the carbon, preferably glassy carbon, material is in the form of carbon, preferably glassy carbon, particles. Optionally, the particles have an average particle size of at least 1, 2 or 5 microns. Optionally, the particles have an average particle size no more than 1000, 800, 500 or 400 microns. Optionally, the particles have an average particle size of between 1 micron and 1000 microns, for example between 2 microns and 800 microns, for example between 4 microns and 500 microns, or between 5 microns and 400 microns.

[0030] Optionally, the carbon, preferably glassy carbon, material is in the form of a carbon, preferably glassy carbon, coating formed on an object.P / 91817

[0031] Optionally, the carbon, preferably glassy carbon, material comprises graphitic nano-crystallites. Optionally, the graphitic nano-crystallites have maximum dimensions of at least 0.5 or 1 nanometre (nm). Optionally, the graphitic nano-crystallites have maximum dimensions of no more than 5 or 3 nm. Optionally, the graphitic nano-crystallites have maximum dimensions in the range of 0.5 nm to 5 nm, for example 1 nm to 3 nm.

[0032] Optionally, the carbon, preferably glassy carbon, material has a d002 plane spacing, measured for example by XRD, of between 0.35 nm and 0.45 nm, for example between 0.36 nm and 0.44 nm, for example between 0.37 nm and 0.42 nm.

[0033] Optionally, the carbon, preferably glassy carbon, material has a Raman ID / IG value of between 0.9 and 1.3, for example between 1.0 and 1.2. As the skilled person would understand, this value may be obtained by a Raman spectroscopy method.

[0034] Optionally, the method comprises the further step of loading the meltable organic precursor into a crucible. Optionally, the meltable organic precursor comprises, or is entirely formed from, one or more polymeric materials. Optionally, the meltable organic precursor comprises, or is entirely formed from, one or more resin materials. Optionally, the meltable organic precursor comprises, or is entirely formed from, one or more thermoplastic materials. Optionally, the meltable organic precursor comprises, or is entirely formed from, one or more thermoplastic materials selected from the list consisting of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polycarbonate, and polyethylene terephthalate. Preferably, the meltable organic precursor comprises, or is entirely formed from, polyethylene terephthalate.

[0035] Optionally, the meltable organic precursor has a melting point of between 75°C and 300°C, for example between 100°C and 280°C, for example between 200°C and 260°C.

[0036] Optionally, carbonisation yield of the meltable organic precursor is between 25% and 50%, for example between 30% and 45%.

[0037] Optionally, the meltable organic precursor comprises, or consists of, reclaimed thermoplastic material, for example from treated thermoplastic waste. Advantageously, such material may be inexpensive and using such material may be environmentally friendly.

[0038] Optionally, the meltable organic precursor comprises one or more organic acids. The organic acid, or each of the organic acids, preferably has a molecular weight less than 300 grams per mole, more preferably less than 200 grams per mole. For example, the meltable organic precursor may comprise one or more of: citric acid, tartaric acid, malic acid, succinic acid, glutaric acid, and malonic acid. Optionally, the meltable organic precursor comprises one or more polyols. For example, the meltable organic precursor may comprise sorbitol. Advantageously, such meltable organic precursors are low-cost and may result in a carbon material with desirable properties.

[0039] Optionally, the meltable organic precursor is in the form of precursor elements or precursor particles each having a minimum dimension of less than 1 mm, for example less than 0.75 mm, for example less than 0.5 mm. Each of the precursor elements or precursor particles may be defined by a length, width, and height, the length width and height being mutually perpendicular. The minimum dimension of a precursor element or precursor particle may be the smallest of the length, width and height of the precursor element or precursor particle. Advantageously, a smaller minimum dimension may increase carbonisation yield.

[0040] Optionally, the meltable organic precursor is in the form of precursor elements or precursor particles formed by cutting thermoplastic waste, for example formed by cutting thermoplastic products such as sheets or bottles into precursor elements. The precursor elements or precursor particles may have length and width dimensions of betweenP / 91817

[0041] 0.5 centimetres (cm) and 3 cm, for example between 0.75 cm and 2 cm, for example about 1 cm. The precursor elements or precursor particles may have a thickness dimension, or minimum dimension, of less than 1 mm. The precursor elements or precursor particles may have a length of between 0.5 cm and 3 cm, a width of between 0.5 cm and 3 cm, and a thickness of less than 1 mm.

[0042] Optionally, the method comprises the further step of milling the carbon particles, for example ball milling the carbon particles, to produce milled carbon particles.

[0043] Optionally, a total thermal treatment time includes a time for increasing the temperature of the meltable organic precursor to the predetermined treatment temperature, a time that the meltable organic precursor is maintained at, or above, the predetermined thermal treatment temperature, and a time for cooling the treated organic precursor from the predetermined treatment temperature. The total thermal treatment time and the predetermined treatment temperature may be controlled to produce carbon, preferably glassy carbon, material with desired d002 spacings. Desired d002 spacings may be greater than 0.36 nm, preferably greater than 0.37 nm, or 0.38 nm, or 0.39 nm, or 0.40 nm.

[0044] Optionally, the thermal treatment is conducted under a selected atmosphere, the selected atmosphere being one of an oxidising atmosphere, a reducing atmosphere and an inert atmosphere, preferably in which selection of the atmosphere depends on the desired surface area of the carbon, preferably glassy carbon, product.

[0045] Optionally, the thermal treatment is conducted in an oxidising atmosphere, and the carbon, preferably glassy carbon, particles have a BET surface area greater than 500 m2 / g. the method may further comprising a step of milling the carbon, preferably glassy carbon, particles to produced milled carbon, preferably glassy carbon, particles having a BET surface area greater than 600 m2 / g. Advantageously, a high surface area may be beneficial for some applications, such as for use as a catalyst.

[0046] Optionally, the thermal treatment is conducted in a reducing atmosphere and the carbon, preferably glassy carbon, particles have a BET surface area less than 50 m2 / g. Advantageously, a low surface area may be beneficial for some applications, such as for use as an inert electrode in an electrolytic cell.

[0047] The carbon material may have a density of between 1 and 3, preferably between 1.2 and 2.5, grams per centimetre cubed. Where the thermal treatment is conducted in a reducing atmosphere, the carbon material may have a density of between 1.5 and 2.5 grams per centimetre cubed. Where the thermal treatment is conducted in an oxidising atmosphere, the carbon material may have a density of between 1.2 and 2.2 grams per centimetre cubed. The densities of this paragraph were measured using helium pycnometry with a Micromeritics device at 21°C. The measurements were performed with approximately 1 g of sample, a chamber size of 3.5 cm3, and 20 purge cycles, based on which the average volume and density of the powders were determined. However, any suitable method may be used.

[0048] Optionally, after the step of cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material, the method comprises a step of heating the carbon, preferable glassy carbon, material. The step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature greater, for example at least 50, 100 or 200 °C greater, than the predetermined treatment temperature. The step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature in the range of 510 °C to 2000 °C. The step of heating the carbon, preferable glassy carbon, material may be conducted in an inert or reducing atmosphere. If in a reducing atmosphere, features described below in relation to the reducing atmosphere of the second aspect may be applicable to the reducing atmosphere of the step of heating the carbon, preferable glassy carbon, material. Advantageously, this additionalP / 91817

[0049] heating of the carbon material may allow tailoring of the pore structure and material properties to meet specific application requirements, such as optimisation for metal-ion battery applications.

[0050] Second aspect - inert or reducing atmosphere

[0051] According to a second aspect of this disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to the first aspect, in which the carbon material is carbon, preferably glassy carbon, particles, the method comprising the steps of:

[0052] heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor;

[0053] further heating the meltable organic precursor to a predetermined treatment temperature to form a treated organic precursor, the predetermined treatment temperature being at least 200°C in excess of the melting point of the meltable organic precursor;

[0054] optionally maintaining the treated organic precursor at, or above, the predetermined treatment temperature for a predetermined period of time; and

[0055] cooling the treated organic precursor to produce the carbon, preferably glassy carbon, particles, in which the thermal treatment is conducted in a reducing atmosphere and the BET surface area of the resulting carbon, preferably glassy carbon, particles is lower than 50 m2 / g.

[0056] Features set out below, before the next aspect is introduced, are applicable to the second aspect. They may also be applicable to other aspects.

[0057] Advantageously, the use of a reducing atmosphere may reduce a BET surface area of the carbon material produced. This may be advantageous in certain applications.

[0058] The thermal treatment of the meltable organic precursor may include all of the heating, further heating, maintaining (where present), and cooling steps.

[0059] Optionally, the BET surface area of the resulting carbon, preferably glassy carbon, particles is lower than 30 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g.

[0060] Optionally, the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g.

[0061] Optionally, the predetermined treatment temperature is at least 400, 600, 700, 800, 850, or 900 degrees Celsius. Advantageously, higher temperatures may provide a good yield of suitable, for example glassy, carbon material.

[0062] Optionally, the predetermined treatment temperature is no more than 3000, 2000, 1500, 1200, 1100, or 1000 degrees Celsius. Advantageously, lower temperatures may avoid excessive energy usage.

[0063] Optionally, the predetermined treatment temperature is between 400°C and 3000°C, for example between 600°C and 2000°C, for example between 700°C and 1500°C, for example between 800°C and 1200°C, for example between 850°C and 1100°C, for example between 900°C and 1000°C. Advantageously, such ranges may provide a good yield of suitable, for example glassy, carbon material without excessive energy usage.

[0064] Optionally, the thermal treatment is conducted in a reducing atmosphere containing hydrogen, for example gaseous hydrogen in the form of H2, for example in which the hydrogen concentration of the reducing atmosphere is between 0.1 percent by volume (vol%) and 100 vol%, for example between 1 vol% and 90 vol%, or between 1 vol%P / 91817

[0065] and 5 vol%, or between 2.5 vol% and 80 vol%, or between 5 vol% and 70 vol%, or between 7.5 vol% and 60 vol%, or between 10 vol% and 50 vol%, or between 15 vol% and 40 vol%, or between 20 vol% and 30 vol%.

[0066] A hydrogen concentration of between 1 vol% and 5 vol% may be preferred. This concentration may be sufficiently reducing to minimise oxidation whilst allowing a relatively safe and / or relatively inexpensive atmosphere.

[0067] Optionally, the thermal treatment is conducted in a reducing atmosphere containing hydrogen and an inert gas, for example hydrogen and one or more inert gas selected from the list consisting of nitrogen, argon, helium, neon, and xenon, particularly preferably wherein the reducing atmosphere contains hydrogen and nitrogen. Nitrogen may be preferred as a cost-effective inert gas.

[0068] Optionally, the predetermined period of time that the meltable organic precursor is maintained at, or above, the predetermined treatment temperature is between 0.1 second and 1 month, for example between 1 second and 12 hours, preferably between 30 seconds and 6 hours, for example between 60 seconds and 5 hours, or between 2 minutes and 1 hour, for example between 5 minutes and 45 minutes.

[0069] Optionally, the carbon material or carbon particles comprise at least 99 weight percent (wt%) carbon, oxygen (if present) and hydrogen (if present). Optionally, the carbon material or carbon particles comprise at least 90 or 95 weight percent (wt%) carbon.

[0070] Optionally, the thermal treatment is conducted for sufficient time and / or at sufficient temperature for the carbon, preferably glassy carbon, particles have a bulk carbon concentration of greater than 90 mass%, for example between 95 mass % and 99 mass %, for example in which the predetermined treatment temperature is in excess of 1000°C and the bulk carbon concentration is greater than 90 mass%, and / or in which the predetermined treatment time is greater than 10 minutes and the bulk carbon concentration is greater than 90 mass%.

[0071] Optionally, the thermal treatment is conducted for sufficient time and / or at sufficient temperature for the carbon, preferably glassy carbon, particles have a surface carbon concentration of greater than 80 mass%, for example between 80 mass % and 90 mass %, for example in which the predetermined treatment temperature is in excess of 1000°C and the surface carbon concentration is greater than 80 mass%, and / or in which the predetermined treatment time is greater than 5 minutes and the surface carbon concentration is greater than 80 mass%.

[0072] Optionally, the carbon, preferably glassy carbon, particles have a crystalline-like morphology, for example an angular or cubic morphology, or a morphology having substantially parallel sides, for example a plate-like morphology.

[0073] Optionally, the carbon, preferably glassy carbon, material has a single-point adsorption total pore volume of between 0.010 and 0.001 cm3 / g.

[0074] Optionally, the carbon, preferably glassy carbon, material has adsorption average pore diameter (4V / A by BET) of between 2 nm and 5 nm.

[0075] Optionally, the carbon, preferably glassy carbon, particles have a d002 spacing of between 0.36 nm and 0.45 nm, preferably between 0.37 nm and 0.43 nm.

[0076] Optionally, the thermal treatment is conducted for a short enough time and / or at low enough temperature for the carbon, preferably glassy carbon, particles to have a d002 spacing of between 0.36 nm and 0.45 nm, preferably between 0.37 nm and 0.43 nm.

[0077] Optionally, the predetermined treatment temperature is lower than 1200°C, for example lower than 1000°C, and the d002 spacing is between 0.36 nm and 0.45 nm. Optionally, the predetermined treatment time is lower than 5 hours, for example lower than 1 hour, and the d002 spacing is between 0.36 nm and 0.45 nm. Optionally, the predetermined treatment temperature is lower than 1200°C, for example lower than 1000°C, and the predeterminedP / 91817

[0078] treatment time is lower than 5 hours, for example lower than 1 hour, and the d002 spacing is between 0.36 nm and 0.45 nm.

[0079] Optionally, after the step of cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material, the method comprises a step of heating the carbon, preferable glassy carbon, material. The step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature greater, for example at least 50, 100 or 200 °C greater, than the predetermined treatment temperature. The step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature in the range of 510 °C to 2000 °C. The step of heating the carbon, preferable glassy carbon, material may be conducted in an inert or reducing atmosphere. If in a reducing atmosphere, features described above in relation to the reducing atmosphere may be applicable to the reducing atmosphere of the step of heating the carbon, preferable glassy carbon, material. Advantageously, this additional heating of the carbon material may allow tailoring of the pore structure and material properties to meet specific application requirements, such as optimisation for metal-ion battery applications.

[0080] Third aspect - oxidising atmosphere

[0081] According to a third aspect, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to the first aspect, in which the carbon, preferably glassy carbon, material is carbon, preferably glassy carbon, particles having high specific surface area, the method comprising the steps of:

[0082] heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor;

[0083] further heating the meltable organic precursor to a predetermined treatment temperature to form a treated organic precursor, the predetermined treatment temperature being at least 200°C in excess of the melting point of the meltable organic precursor;

[0084] optionally maintaining the treated organic precursor at, or above, the predetermined treatment temperature for a predetermined period of time; and

[0085] cooling the treated organic precursor to produce the carbon, preferably glassy carbon, particles, in which the thermal treatment is conducted in an oxidising atmosphere and the BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 400 m2 / g.

[0086] Features set out below, before the next aspect is introduced, are applicable to the third aspect. They may also be applicable to other aspects.

[0087] Advantageously, the use of an oxidising atmosphere may increase a BET surface area of the carbon material produced. This may be advantageous in certain applications.

[0088] The thermal treatment of the meltable organic precursor may include all of the heating, further heating, maintaining (where present), and cooling steps.

[0089] Optionally, the BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g, for example greater than 550 m2 / g, or greater than 600 m2 / g, for example greater than 650 m2 / g, or greater than 700 m2 / g,. The BET surface area of the resulting carbon, preferably glassy carbon, particles may be between 400 m2 / g and 700 m2 / g, for example between 500 m2 / g and 600 m2 / g.P / 91817

[0090] Optionally, the maximum predetermined treatment temperature is 1500°C or lower, for example in which the predetermined treatment temperature is between 400°C and 1000°C, for example between 500°C and 900°C, for example between 600°C and 800°C, for example between 650°C and 750°C.

[0091] Optionally, the thermal treatment is conducted in an oxidising atmosphere containing oxygen, for example gaseous oxygen in the form of O2. The oxygen concentration of the reducing atmosphere may be between 0.1 vol% and 100 vol%, for example between 1 vol% and 40 vol%, or between 2.5 vol% and 30 vol%, or between 5 vol% and 25 vol%, or between 7.5 vol% and 22 vol%. The oxidising atmosphere may be or comprise air or oxygen-enriched air.

[0092] Optionally, the predetermined period of time that the meltable organic precursor is maintained at, or above, the predetermined treatment temperature is between 0.1 second and 6 hours, for example between 1 second and 2 hours, preferably between 10 seconds and 1 hour, for example between 20 seconds and 30 minutes, or between 30 seconds and 20 minutes, for example between 1 minute and 10 minutes.

[0093] Optionally, the carbon, preferably glassy carbon, particles comprise a number of surfaces, optionally in which the number of surfaces is all of the surfaces of the carbon particles, a proportion of the number of surfaces being smooth surfaces and a proportion of the number of surfaces being highly textured surfaces. Optionally, between 10% and 70% of the number of surfaces are highly textured surfaces, for example in which between 20% and 60% of the number of surfaces are highly textured surfaces, for example between 30% and 50% of the number of surfaces are highly textured surfaces.

[0094] Optionally, the method comprises the further step of milling, for example ball milling, the carbon, preferably glassy carbon, particles to increase their surface area. Optionally, the method comprises milling until the BET specific surface area is increased by between 10% and 300%, for example between 20% and 200%, for example between 30% and 100%. Optionally, the milled carbon, preferably glassy carbon, particles have a BET surface area greater than 600 m2 / g, for example greater than 700 m2 / g, or greater than 750 m2 / g, for example greater than 800 m2 / g, or greater than 850 m2 / g. Optionally, the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 600 m2 / g and 900 m2 / g, for example between 700 m2 / g and 800 m2 / g.

[0095] Optionally, after the step of cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material, the method comprises a step of heating the carbon, preferable glassy carbon, material. The step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature greater, for example at least 50, 100 or 200 °C greater, than the predetermined treatment temperature. The step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature in the range of 510 °C to 2000 °C. The step of heating the carbon, preferable glassy carbon, material may be conducted in an inert or reducing atmosphere. If in a reducing atmosphere, features described below in relation to the reducing atmosphere of the second aspect may be applicable to the reducing atmosphere of the step of heating the carbon, preferable glassy carbon, material. Advantageously, this additional heating of the carbon material may allow tailoring of the pore structure and material properties to meet specific application requirements, such as optimisation for metal-ion battery applications.

[0096] Fourth aspects - salt

[0097] According to a fourth aspect of the disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method as set out above, optionally according to any of the first, second, or third aspects, in which the carbon, preferably glassy carbon, material is carbon, preferably glassy carbon, particles having high specific surface area, the method comprising the steps of:P / 91817

[0098] arranging the meltable organic precursor in contact with at least one inorganic salt having a melting point greater than 300°C;

[0099] controlling temperature of the meltable organic precursor and the at least one inorganic salt to a predetermined treatment temperature in excess of the melting point of the inorganic salt to form a treated precursor;

[0100] optionally maintaining the treated organic precursor and at least one inorganic salt at, or above, the predetermined treatment temperature for a predetermined period of time;

[0101] cooling the treated precursor; and

[0102] washing the at least one inorganic salt from the treated precursor to produce the carbon, preferably glassy carbon, particles, in which BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 400 m2 / g.

[0103] According to an alternative fourth aspect of the disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to the previous paragraph, in which the carbon, preferably glassy carbon, material is carbon, preferably glassy carbon, particles having high specific surface area, the method comprising the steps of:

[0104] combining the meltable organic precursor with at least one inorganic salt to form a precursor mixture, the at least one inorganic salt having a melting point greater than 300°C;

[0105] heating the precursor mixture to a temperature above the melting point of the meltable organic precursor; further heating the precursor mixture to a predetermined treatment temperature in excess of the melting point of the at least one inorganic salt to form a treated precursor;

[0106] optionally maintaining the treated precursor at or above the predetermined treatment temperature for a predetermined period of time;

[0107] cooling the treated precursor; and

[0108] washing the at least one inorganic salt from the treated precursor to produce the carbon, preferably glassy carbon, particles, in which BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 400 m2 / g.

[0109] For the fourth aspect, the thermal treatment of the meltable organic precursor may include all of the controlling, maintaining (where present), and cooling steps. For the alternative fourth aspect, the thermal treatment of the meltable organic precursor may include all of the heating, further heating, maintaining (where present), and cooling steps.

[0110] Features set out below, before the next aspect is introduced, are applicable to the fourth and alternative fourth aspects. They may also be applicable to other aspects.

[0111] Advantageously, the use of a salt may increase carbonisation yield.

[0112] Optionally, the BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g, for example greater than 550 m2 / g, or greater than 600 m2 / g, for example greater than 650 m2 / g, or greater than 700 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 700 m2 / g, for example between 500 m2 / g and 600 m2 / g.

[0113] Optionally, the at least one inorganic salt is one or more of: an alkali metal halide, an alkaline earth metal halide, an alkali metal nitrate and an alkaline earth metal nitrate.

[0114] Optionally, the at least one inorganic salt is at least one salt from the list consisting of calcium chloride (CaCI2), magnesium chloride (MgCI2), strontium chloride (SrCI2), barium chloride (BaCI2), calcium fluoride (CaF2), magnesium fluoride (MgF2), strontium fluoride (SrF2), barium fluoride (BaF2), beryllium chloride (BeCI2), and beryllium fluorideP / 91817

[0115] (BeF2), sodium chloride (NaCI), potassium chloride (KCI), lithium chloride (LICI), sodium fluoride (NaF), potassium fluoride (KF), lithium fluoride (LIF), sodium bromide (NaBr), potassium bromide (KBr), lithium bromide (LiBr), sodium iodide (Nal), potassium iodide (KI), lithium iodide (Lil), sodium nitrate (NaNO3), potassium nitrate (KNO3), lithium nitrate (LiNO3), rubidium nitrate (RbNO3), cesium nitrate (CsNO3), calcium nitrate (Ca(NO3)2), magnesium nitrate (Mg(N03)2), barium nitrate (Ba(N03)2), and strontium nitrate (Sr(N03)2).

[0116] Optionally, the at least one salt is calcium-free. Optionally, the at least one salt does not include a calcium based salt, for example in which the at least one inorganic salt is at least one salt from the list consisting of magnesium chloride (MgCI2), strontium chloride (SrCI2), barium chloride (BaCI2), magnesium fluoride (MgF2), strontium fluoride (SrF2), barium fluoride (BaF2), beryllium chloride (BeCI2), and beryllium fluoride (BeF2), sodium chloride (NaCI), potassium chloride (KCI), lithium chloride (LICI), sodium fluoride (NaF), potassium fluoride (KF), lithium fluoride (LIF), sodium bromide (NaBr), potassium bromide (KBr), lithium bromide (LiBr), sodium iodide (Nal), potassium iodide (KI), lithium iodide (Lil), sodium nitrate (NaNO3), potassium nitrate (KNO3), lithium nitrate (LINO3), rubidium nitrate (RbNO3), cesium nitrate (CsNO3), magnesium nitrate (Mg(N03)2), barium nitrate (Ba(N03)2), and strontium nitrate (Sr(N03)2),

[0117] Preferably, the at least one inorganic salt is at least one salt from the list consisting of magnesium chloride (MgClz), sodium chloride (NaCI), potassium chloride (KCI), and lithium chloride (LICI).

[0118] Optionally, the at least one inorganic salt is a salt mixture of two or more inorganic salts, preferably in which the composition of the salt mixture is selected to control the melting point of the salt mixture. Preferably, where the at least one inorganic salt is a salt mixture of two or more inorganic salts, the salt mixture is a eutectic or near-eutectic mixture of the two or more inorganic salts. Preferably, the at least one inorganic salt is a salt mixture of NaCI and KCI, for example a eutectic or near-eutectic mixture of NaCI and KCI. Advantageously, a eutectic or near-eutectic mixture may have a lower melting point than other mixtures.

[0119] Optionally, the predetermined treatment temperature is at least 100, 200 or 300 degrees Celsius in excess of the melting point of the at least one inorganic salt.

[0120] Optionally, the predetermined treatment temperature is no more than 500, 400, or 300 degrees Celsius in excess of the melting point of the at least one inorganic salt.

[0121] Optionally, the predetermined treatment temperature is between 400°C and 1200°C, preferably between 500°C and 1000°C, for example between 600°C and 900°C.

[0122] Optionally, the method further comprises the further step of milling, for example ball milling, the carbon, preferably glassy carbon, particles to increase their surface area, preferably milling until the BET specific surface area is increased by between 10% and 300%, for example between 20% and 200%, for example between 30% and 100%. Optionally, the milled carbon, preferably glassy carbon, particles have a BET surface area greater than 600 m2 / g, for example greater than 700 m2 / g, or greater than 750 m2 / g, for example greater than 800 m2 / g, or greater than 850 m2 / g. Optionally, the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 600 m2 / g and 900 m2 / g, for example between 700 m2 / g and 800 m2 / g.

[0123] Optionally, the thermal treatment is conducted in an oxidising atmosphere, for example in an atmosphere comprising or consisting of air or oxygen-enriched air. Optionally, particularly if the thermal treatment is conducted in an oxidising atmosphere, the BET surface area of the resulting particulate product is greater than 300, 350, 400, 450 or 500 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles isP / 91817

[0124] between 350 m2 / g and 600 m2 / g, for example between 400 m2 / g and 550 m2 / g. Features described in relation to an oxidising atmosphere for the third aspect may be applicable to the oxidising atmosphere here.

[0125] Optionally, the thermal treatment is conducted in a reducing atmosphere, for example a hydrogen containing atmosphere. Optionally, particularly if the thermal treatment is conducted in a reducing atmosphere, the BET surface area of the resulting carbon, preferably glassy carbon, particles is lower than 50, 20 or 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g. Features described in relation to a reducing atmosphere for the second aspect may be applicable to the reducing atmosphere here.

[0126] Optionally, after the step of washing the at least one inorganic salt from the treated precursor to produce the carbon, preferably glassy carbon, particles, the method comprises a step of heating the carbon, preferable glassy carbon, material. The step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature greater, for example at least 50, 100 or 200 °C greater, than the predetermined treatment temperature. The step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature in the range of 510 °C to 2000 °C. The step of heating the carbon, preferable glassy carbon, material may be conducted in an inert or reducing atmosphere. If in a reducing atmosphere, features described above in relation to the reducing atmosphere of the second aspect may be applicable to the reducing atmosphere of the step of heating the carbon, preferable glassy carbon, material. Advantageously, this additional heating of the carbon material may allow tailoring of the pore structure and material properties to meet specific application requirements, such as optimisation for metal-ion battery applications.

[0127] Fifth aspects - calcium-containinq salt

[0128] According to a fifth aspect, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method as set out above, optionally according to any of the first, second, third or fourth aspects, in which the carbon, preferably glassy carbon, material is a particulate carbon, preferably glassy carbon, composite comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix, the method comprising the steps of:

[0129] heating the meltable organic precursor in contact with at least one inorganic salt to a predetermined treatment temperature to form a treated precursor, the at least one inorganic salt containing calcium and having a melting point greater than 300°C;

[0130] optionally maintaining the treated precursor and salt mixture at, or above, the predetermined treatment temperature for a predetermined period of time;

[0131] cooling the treated precursor; and

[0132] washing the at least one inorganic salt from the treated precursor to produce an initial particulate product, the particles of the initial particulate product comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix.

[0133] According to an alternative fifth aspect, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to the previous paragraph, in which the carbon, preferably glassy carbon, material is a particulate carbon, preferably glassy carbon, composite comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix, the method comprising the steps:P / 91817

[0134] combining the meltable organic precursor with at least one inorganic salt to form a precursor mixture, the at least one inorganic salt comprising calcium and having a melting point greater than 300°C;

[0135] heating the precursor mixture to a temperature above the melting point of the meltable organic precursor; further heating the precursor mixture to a predetermined treatment temperature in excess of the melting point of the inorganic salt to form a treated precursor;

[0136] optionally maintaining the treated precursor at, or above, the predetermined treatment temperature for a predetermined period of time;

[0137] cooling the treated precursor; and

[0138] washing the at least one inorganic salt from the treated precursor to produce an initial particulate product, the particles of the particulate product comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix.

[0139] Features set out below, before the next aspect is introduced, are applicable to the fifth and alternative fifth aspects. They may also be applicable to other aspects.

[0140] Advantageously, the use of a salt may increase carbonisation yield. Further, the use of a calcium-containing salt may allow production of a calcium carbonate crystals and highly porous carbon material, for example carbon material with holes. This can be advantageous in certain applications, such as when making composites.

[0141] The thermal treatment of the meltable organic precursor may include all of the heating, further heating, maintaining (where present), and cooling steps.

[0142] Optionally, the at least one inorganic salt comprises a calcium halide salt, for example calcium chloride, preferably in which the at least one inorganic salt is a mixture of a calcium halide salt and at least one other inorganic salt, for example in which the at least one inorganic salt is a mixture of sodium chloride and calcium chloride.

[0143] Optionally, the at least one inorganic salt is a mixture of two or more inorganic salts, preferably in which the composition of the mixture of two or more inorganic salts is selected to control the melting point of the salt mixture, for example in which the at least one inorganic salt is a eutectic or near-eutectic mixture.

[0144] Optionally, the at least one inorganic salt is a NaCI-CaC mixture, or a CaCl2-NaCI-MgCl2 mixture, or a CaC -NaCI-KCI-MgCl2 mixture, or a CaCI2-NaCI-KCI mixture, or a CaCI2-LiCI-KCI mixture.

[0145] Optionally, the predetermined treatment temperature is at least 100, 150 or 200 degrees Celsius in excess of the melting point of the at least one inorganic salt.

[0146] Optionally, the predetermined treatment temperature is no more than 500, 400 or 300 degrees Celsius in excess of the melting point of the at least one inorganic salt.

[0147] Optionally, the predetermined treatment temperature is between 400°C and 1200°C, preferably between 500°C and 1000°C, for example between 600°C and 900°C.

[0148] Optionally, the particulate product comprises particles having an average particle size of between 1 micron and 1000 microns, for example between 2 microns and 800 microns, for example between 4 microns and 500 microns, or between 5 microns and 400 microns.

[0149] Optionally, the calcium carbonate crystals have a rod-like morphology, optionally with a length to diameter ratio of between 30:1 and 1.5:1. The term "diameter” in this context and similar contexts may refer to an average transverse dimension of the calcium carbonate crystals along a length of the calcium carbonate crystals, the transverse dimension being measured perpendicularly to the length.P / 91817

[0150] Optionally, the calcium carbonate crystals have a rod-like morphology with a diameter of between 20 and 500 nm, for example between 40 and 400 nm, for example in which the calcium carbonate crystals have a calcite-rhombohedral crystalline structure.

[0151] Optionally, the calcium carbonate crystals have a rod-like morphology with a length of between 30 nm and 15 micron, for example between 60 nm and 12 micron.

[0152] Optionally, the calcium carbonate crystals have a crystal size, measured perpendicular to the (104) planes of the crystals, of between 10 nm and 200 nm, for example between 20 nm and 100 nm.

[0153] Optionally, XRD analysis of the calcium carbonate crystals shows a peak, preferably a sharp peak, at a two-theta value of 29.399° ±0.2.

[0154] Optionally, the thermal treatment is conducted in an oxidising atmosphere, for example in an atmosphere comprising or consisting of air or oxygen-enriched air. Optionally, particularly if the thermal treatment is conducted in an oxidising atmosphere, the BET surface area of the resulting particulate product is greater than 300, 350, 400, 450 or 500 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 350 m2 / g and 600 m2 / g, for example between 400 m2 / g and 550 m2 / g. Features described in relation to an oxidising atmosphere for the third aspect may be applicable to the oxidising atmosphere here.

[0155] Optionally, the thermal treatment is conducted in a reducing atmosphere, for example a hydrogen containing atmosphere. Optionally, particularly if the thermal treatment is conducted in a reducing atmosphere, the BET surface area of the resulting carbon, preferably glassy carbon, particles is lower than 50, 20 or 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g. Features described in relation to a reducing atmosphere for the second aspect may be applicable to the reducing atmosphere here.

[0156] Optionally, the carbon, preferably glassy carbon, matrix is porous.

[0157] Optionally, the carbon, preferably glassy carbon, matrix comprises holes, for example one or both of blind holes and through-holes, preferably through-holes, optionally wherein an average diameter of the holes is between 2 nm and 500 nm, or 5 nm and 200 nm, optionally wherein the holes have a substantially circular or semi-circular cross-sectional shape. Advantageously, these holes can provide interfaces for making well-integrated composite materials. For example, a composite material such as a metallic material may enter or pass through the holes to make a well-integrated composite material. A metallic material in this context may be a metal, alloy or intermetallic.

[0158] Optionally, in the initial particulate product, at least some of the calcium carbonate crystals are at least partially located in at least some of the holes of the carbon, preferably glassy carbon, matrix.

[0159] Optionally, after the step of washing the at least one inorganic salt from the treated precursor to produce the initial particulate product, the method comprises a step of heating the initial particulate product. The step of heating the initial particulate product may comprise heating the initial particulate product to a temperature greater, for example at least 50, 100 or 200 °C greater, than the predetermined treatment temperature. The step of heating the initial particulate product may comprise heating the initial particulate product to a temperature in the range of 510 °C to 2000 °C. The step of heating the initial particulate product may be conducted in an inert or reducing atmosphere. If in a reducing atmosphere, features described above in relation to the reducing atmosphere of the second aspect may be applicable to the reducing atmosphere of the step of heating the initial particulate product. Advantageously, this additional heating of the carbon material may allow tailoring of the pore structure and material properties to meet specific application requirements, such as optimisation for metal-ion battery applications.P / 91817

[0160] Sixth aspects - calcium-containinq salt and wash

[0161] According to a sixth aspect of the disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method as described above, optionally according to any of the first, second, third or fourth aspects, in which the carbon material is carbon, preferably glassy carbon, particles, the method comprising the steps of:

[0162] heating the meltable organic precursor in contact with at least one inorganic salt to a predetermined treatment temperature to form a treated precursor, the at least one inorganic salt containing calcium and having a melting point greater than 300°C;

[0163] optionally maintaining the treated precursor and at least one inorganic salt at, or above, the predetermined treatment temperature for a predetermined period of time;

[0164] cooling the treated precursor;

[0165] washing the at least one organic salt from the treated precursor to produce an initial particulate product, particles of the particulate product comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix: and

[0166] washing the initial particulate product in an acidic solution to remove at least a portion of the calcium carbonate crystals, preferably in which a BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g.

[0167] According to an alternative sixth aspect of the disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to the above paragraph, in which the carbon, preferably glassy carbon, material is a particulate carbon, preferably glassy carbon, composite comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix, the method comprising the steps of:

[0168] combining the meltable organic precursor with at least one inorganic salt to form a precursor mixture, the at least one inorganic salt comprising calcium and having a melting point greater than 300°C;

[0169] heating the precursor mixture to a temperature above the melting point of the meltable organic precursor; further heating the precursor mixture to a predetermined treatment temperature in excess of the melting point of the at least one inorganic salt to form a treated precursor;

[0170] optionally maintaining the treated precursor mixture at, or above, the predetermined treatment temperature for a predetermined period of time;

[0171] cooling the treated precursor; and

[0172] washing the at least one organic salt from the treated precursor to produce an initial particulate product, the particles of the particulate product comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix: and

[0173] removing at least a portion of the calcium carbonate crystals, for example by washing the initial particulate product in an acidic solution to remove at least a portion of the calcium carbonate crystals or by heating the initial particulate product to melt or evaporate and thereby remove at least a portion of the calcium carbonate crystals, preferably in which BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g.

[0174] Features set out below, before the next aspect is introduced, are applicable to the sixth and alternative sixth aspects. They may also be applicable to other aspects.P / 91817

[0175] Advantageously, the use of a salt may increase carbonisation yield. Further, the use of a calcium-containing salt may allow production of a calcium carbonate crystals and highly porous carbon material, for example carbon material with holes. This can be advantageous in certain applications, such as when making composites.

[0176] The thermal treatment of the meltable organic precursor may include all of the heating, further heating, maintaining (where present), and cooling steps.

[0177] Optionally, the steps of washing the at least one organic salt from the treated precursor and removing at least a portion of the calcium carbonate crystals are conducted simultaneously by washing the treated precursor in an acidic solution to remove the salt and at least a portion of the calcium carbonate crystals.

[0178] Optionally, the step of washing in acidic solution is conducted until at least 50% of the calcium carbonate crystals are removed, preferably at least 60%, preferably at least 70%, or at least 80%, or at least 90%, particularly preferably until substantially all of the calcium carbonate crystals are removed.

[0179] Optionally, the resulting carbon, preferably glassy carbon, particles are highly porous particles, preferably in which the particles comprise rounded, semi-circular and / or through holes that extend through individual carbon, preferably glassy carbon, particles.

[0180] Optionally, the carbon, preferably glassy carbon, particles comprise a plurality of holes, for example one or both of blind holes and through-holes. Preferably, the holes have a diameter or cross-sectional dimension of between 5 nm and 500 nm, for example between 10 nm and 400 nm.

[0181] Optionally, the BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500, 600, 700, 750 or 800 m2 / g. Optionally, the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 500 m2 / g and 900 m2 / g, for example between 600 m2 / g and 800 m2 / g.

[0182] Optionally, the at least one inorganic salt comprises a calcium halide salt, for example calcium chloride. Optionally, the at least one inorganic salt is a mixture of a calcium halide salt and at least one other inorganic salt, for example in which the at least one inorganic salt is a mixture of sodium chloride and calcium chloride.

[0183] Optionally, the at least one inorganic salt is a mixture of two or more inorganic salts. Optionally, the composition of the mixture of two or more inorganic salts is selected to control the melting point of the salt mixture. Optionally, the at least one inorganic salt is a eutectic or near-eutectic mixture. Optionally, the at least one inorganic salt is a mixture of NaCI and CaCl2, for example a eutectic or near-eutectic mixture of NaCI and CaCh. Optionally, the at least one inorganic salt is a CaCl2-NaCI-MgCl2 mixture, or a CaCl2-NaCI-KCI-MgCl2 mixture, or a CaCI2-NaCI-KCI mixture, or a CaCI2-LiCI-KCI mixture.

[0184] Optionally, the predetermined treatment temperature is at least 100, 150, or 200°C in excess of the melting point of the at least one inorganic salt.

[0185] Optionally, the predetermined treatment temperature is no more than 500, 400 or 300°C in excess of the melting point of the at least one inorganic salt.

[0186] Optionally, the predetermined treatment temperature is between 400°C and 1200°C, preferably between 500°C and 1000°C, for example between 600°C and 900°C.

[0187] Optionally, the particulate product comprises particles have an average particle size of between 1 micron and 1000 microns, for example between 2 microns and 800 microns, for example between 4 microns and 500 microns, or between 5 microns and 400 microns.

[0188] Optionally, the acidic solution has a pH value of between 0.5 and 7, for example between 1 and 4.Optionally, a salt recovery step is conducted after the washing step to recover the at least one inorganic salt from the wash. Alternatively, or in addition, a calcium carbonate recovery step may be conducted to recover calcium carbonate from the acidic solution.

[0189] Optionally, the thermal treatment is conducted in an oxidising atmosphere, for example in an atmosphere comprising or consisting of air or oxygen-enriched air. Features described in relation to an oxidising atmosphere for the third aspect may be applicable to the oxidising atmosphere here.

[0190] Optionally, the thermal treatment is conducted in a reducing atmosphere, for example a hydrogen containing atmosphere. Features described in relation to a reducing atmosphere for the second aspect may be applicable to the reducing atmosphere here.

[0191] Optionally, the method comprises the further step of milling, for example ball milling, the carbon, preferably glassy carbon, particles to increase the surface area. Preferably, the method comprising milling until the BET specific surface area is increased by between 10% and 300%, for example between 20% and 200%, for example between 30% and 100%. Preferably, the milled carbon, preferably glassy carbon, particles have a BET surface area greater than 600, 700, 800, 850, or 900 m2 / g. Preferably, the BET surface area of the milled carbon, preferably glassy carbon, particles is between 600 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g, or between 800 m2 / g and 900 m2 / g.

[0192] Optionally, after the step of washing the initial particulate product in an acidic solution to remove at least a portion of the calcium carbonate crystals in the sixth aspect, or after the step of removing at least a portion of the calcium carbonate crystals in the alternative sixth aspect, the method comprises a step of heating the carbon, preferably glassy carbon, particles or matrix. The step of heating the carbon, preferably glassy carbon, particles or matrix may comprise heating the carbon, preferably glassy carbon, particles or matrix to a temperature greater, for example at least 50, 100 or 200 °C greater, than the predetermined treatment temperature. The step of heating the carbon, preferably glassy carbon, particles or matrix may comprise heating the carbon, preferably glassy carbon, particles or matrix to a temperature in the range of 510 °C to 2000 °C. The step of heating the carbon, preferably glassy carbon, particles or matrix may be conducted in an inert or reducing atmosphere. If in a reducing atmosphere, features described above in relation to the reducing atmosphere of the second aspect may be applicable to the reducing atmosphere of the step of heating the carbon, preferably glassy carbon, particles or matrix. Advantageously, this additional heating of the carbon material may allow tailoring of the pore structure and material properties to meet specific application requirements, such as optimisation for metal-ion battery applications.

[0193] Seventh aspects - coating

[0194] According to a seventh aspect of the disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method as described above, such as according to the first aspect, in which the carbon, preferably glassy carbon, material is a coating on a carbon, preferably glassy carbon, coated object, the method comprising the steps of:

[0195] coating a meltable organic precursor onto a surface of an object thereby forming a meltable organic coating; heating the meltable organic coating to a temperature above the melting point of the meltable organic coating; further heating the meltable organic coating to a predetermined treatment temperature in excess of 300°C; optionally maintaining the meltable organic coating at or above the predetermined treatment temperature for a predetermined period of time thereby forming a treated organic coating; and

[0196] cooling the treated organic coating to produce the carbon, preferably glassy carbon, coated object.According to an alternative seventh aspect of the disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method as described above, such as according to the first aspect, in which the carbon, preferably glassy carbon, material is a coating on a carbon, preferably glassy carbon, coated object the method comprising the steps of:

[0197] heating a meltable organic precursor thereby forming a molten organic precursor; arranging for the object to contact the molten organic precursor thereby forming a molten organic coating on at least one surface of the object;

[0198] further heating the molten organic coating to a predetermined treatment temperature in excess of 300°C; optionally maintaining the molten organic coating at or above the predetermined treatment temperature for a predetermined period of time thereby forming a treated organic coating; and

[0199] cooling the treated organic coating to produce the carbon, preferably glassy carbon, coated object.

[0200] Features set out below, before the next aspect is introduced, are applicable to the seventh and alternative seventh aspects. They may also be applicable to other aspects.

[0201] Advantageously, the object coated with glassy carbon may be well-protected, from example from oxidation or certain types of radiation. The coated object may also have enhanced physical properties, for example enhanced strength or stiffness.

[0202] The thermal treatment of the meltable organic precursor may include all of the heating, further heating, maintaining (where present), and cooling steps.

[0203] Optionally, in which the thermal treatment is conducted in an oxidising atmosphere. Optionally, particularly if the thermal treatment is conducted in an oxidising atmosphere, the carbon, preferably glassy carbon, coating has a BET surface area greater than 200 m2 / g, for example greater than 300 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 200 m2 / g and 600 m2 / g, for example between 300 m2 / g and 550 m2 / g. Features described in relation to an oxidising atmosphere for the third aspect may be applicable to the oxidising atmosphere here.

[0204] Optionally, the thermal treatment is conducted in a reducing atmosphere. Optionally, particularly if the thermal treatment is conducted in a reducing atmosphere, the carbon, preferably glassy carbon, coating has a BET surface area less than 50 m2 / g, for example less than 20 m2 / g, or less than 10 m2 / g, or less than 5 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, coating is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g. Features described in relation to a reducing atmosphere for the second aspect may be applicable to the reducing atmosphere here.

[0205] Optionally, the object is an electrode and the resulting product is a carbon, preferably glassy carbon, coated electrode, for example in which the object is a graphite electrode and the resulting product is a carbon, preferably glassy carbon, coated graphite electrode.

[0206] Optionally, the object is a fuel rod and the resulting product is a carbon, preferably glassy carbon, coated fuel rod.

[0207] Optionally, the object is a medical implant and the resulting product is a carbon, preferably glassy carbon, coated medical implant.

[0208] Optionally, the object is plurality of particles and the resulting product is a plurality of carbon, preferably glassy carbon, coated particles, for example in which each of the plurality of particles is coated with carbon, preferably glassy carbon.Optionally, the plurality of particles are a plurality of metallic particles, or a plurality of ceramic particles, or a plurality of alloy particles, or a plurality of intermetallic particles.

[0209] Optionally, the object is a container such as a waste container and the resulting product is a container such as a waste container coated with carbon, preferably glassy carbon,, for example coated on the inside and / or outside with carbon, preferably glassy carbon,.

[0210] Optionally, the object is a nuclear material, for example a nuclear waste container, or nuclear waste material.

[0211]

[0212] According to an eighth aspect of the disclosure, there is provided a method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method as described above, such as according to any previous aspect, in which the carbon, preferably glassy carbon, material is upcycled carbon, preferably glassy carbon, material formed from thermoplastic waste, the method comprising the steps of: comminuting thermoplastic waste to form a recycled thermoplastic precursor;

[0213] heating the recycled thermoplastic precursor to a temperature above the melting point of the recycled thermoplastic precursor;

[0214] further heating the recycled thermoplastic precursor to a predetermined treatment temperature in excess of 300°C;

[0215] optionally maintaining the recycled thermoplastic precursor at, or above, the predetermined treatment temperature for a predetermined period of time thereby forming a treated precursor; and

[0216] cooling the treated precursor to produce the upcycled carbon, preferably glassy carbon, material.

[0217] Features set out below, before the next aspect is introduced, are applicable to the eighth aspect. They may also be applicable to other aspects.

[0218] Advantageously, the use of a recycled thermoplastic precursor may be cost-effective and environmentally friendly.

[0219] The thermal treatment of the meltable organic precursor may include all of the heating, further heating, maintaining (where present), and cooling steps.

[0220] Optionally, the recycled thermoplastic precursor is formed by comminuting, for example by cutting, waste thermoplastic products, such as sheets or bottles, into precursor elements. The precursor elements may have length and width dimensions of between 0.5 cm and 3 cm, for example between 0.75 cm and 2 cm, for example about 1 cm, for example in which the precursor elements have a length of between 0.5 cm and 3 cm, a width of between 0.5 cm and 3 cm.

[0221] The precursor elements preferably have a thickness, or smallest dimension as described earlier, of less than 1 mm. Advantageously, a smaller thickness or smallest dimension may improve carbonisation yield.

[0222] Optionally, the thermoplastic waste is washed before and / or after the comminution step.

[0223] Optionally, the thermoplastic waste comprises, or is, used drinks bottles, for example used PET bottles.

[0224] Ninth aspects - forming product

[0225] According to a ninth aspect of the disclosure, there is provided a method of forming a product comprising carbon, preferably glassy carbon, particles, the method comprising the steps of:

[0226] forming carbon, preferably glassy carbon, particles by a method of producing carbon, preferably glassy carbon, material, for example a method as described above, such as according to any previous aspect; and consolidating the carbon, preferably glassy carbon, particles to form the product.According to an alternative ninth aspect of the disclosure, there is provided a method of forming a product comprising carbon, preferably glassy carbon, particles according to the above paragraph, comprising the step of: mixing the carbon, preferably glassy carbon, particles with at least one consolidation agent, for example at least one of a lubricant, a binder, and a sintering aid, to form a product precursor mixture; and

[0227] consolidating the product precursor mixture.

[0228] Features set out below, before the next aspect is introduced, are applicable to the ninth and alternative ninth aspects. They may also be applicable to other aspects.

[0229] Advantageously, products comprising this carbon material may be useful in many applications, as described elsewhere in this disclosure.

[0230] Optionally, consolidation is effected by traditional or advanced powder metallurgical techniques, for example in which consolidation is effected by a process selected from the list consisting of pressing, sintering, selective laser sintering, printing, hot isostatic pressing, or cold isostatic pressing.

[0231] Optionally, the product precursor mixture comprises a sintering aid or a binder. Optionally, the sintering aid or the binder is a polymeric material, a ceramic material, or a metallic material. Preferably, the sintering aid or the binder is a metal, for example a refractory metal.

[0232] Optionally, the product precursor mixture comprises a metallic object or metallic particles. Optionally, the product precursor mixture is consolidated at a sufficient temperature to form a metal carbide interface between the carbon, preferably glassy carbon, particles and the metallic object or metallic particles.

[0233] Optionally, the product precursor mixture comprises further filler particles, for example further carbonaceous particles, for example particles of carbon, or particles of graphite, or particles of carbon nanostructures such as graphene or nanotubes.

[0234] Optionally, the step of consolidating the carbon, preferably glassy carbon, particles, for example the product precursor mixture that comprises the carbon, preferably glassy carbon, particles, is conducted at a temperature of greater than 300°C, for example greater than 500°C, for example greater than 1000°C.

[0235] Optionally, the step of consolidating the carbon, preferably glassy carbon, particles, for example the product precursor mixture that comprises the carbon, preferably glassy carbon, particles, is conducted in a reducing atmosphere or an inert atmosphere. Features described in relation to a reducing atmosphere or an inert atmosphere for the second aspect may be applicable to the a reducing atmosphere or an inert atmosphere here.

[0236] Optionally, the product precursor mixture comprises metallic particles, in which the product precursor mixture comprises between 1 vol% and 25 vol % metallic particles, for example between 2.5 vol% and 20 vol % metallic particles, for example between 5 vol% and 15 vol % metallic particles

[0237] Optionally, the product precursor mixture comprises at least one organic binder.

[0238] Optionally, consolidation of the product precursor mixture comprising the at least one organic binder involves a step of forming the product precursor mixture into a shape, or coating the product precursor mixture onto a substrate, and drying the product precursor mixture.

[0239] Optionally, the method comprises the step of forming carbon, preferably glassy carbon, particles by a method of producing carbon, preferably glassy carbon, material as described previously, for example with a method according to any previous aspect defining a method of producing carbon, preferably glassy carbon, material or particles.

[0240] Optionally, the method comprises the step of mixing the carbon, preferably glassy carbon, material or particles with a binder and conductive particles, preferably conductive carbon particles, forming a product precursor mixture.P / 91817

[0241] Optionally, the method comprises the step of consolidating the product precursor mixture to form the product. Optionally, the method comprises the steps of:

[0242] forming carbon, preferably glassy carbon, particles by a method of producing carbon, preferably glassy carbon, material as described previously, for example with a method according to any previous aspect defining a method of producing carbon, preferably glassy carbon, material or particles;

[0243] mixing the carbon, preferably glassy carbon, material or particles with a binder and conductive particles, preferably conductive carbon particles, forming a product precursor mixture; and

[0244] consolidating the product precursor mixture to form the product.

[0245] Optionally, the product precursor mixture comprises between 50 mass% and 90 mass% of the carbon, preferably glassy carbon, particles, between 25 mass % and 5 mass% of binder and between 25 mass% and 5 mass % conductive carbon particles.

[0246] Optionally, the carbon, preferably glassy carbon, particles, or the product precursor mixture that comprises the carbon, preferably glassy carbon, particles, is consolidated onto, or in contact with, an electrically conductive substrate to form an electrode.

[0247] Optionally, the method comprises a further step of grading the carbon, preferably glassy carbon, particles, for example by sieving, for example in order to obtain a preferred particle size and / or particle size distribution.

[0248] Optionally, the method comprises a further step of milling the carbon, preferably glassy carbon, particles, for example to obtain a desired particle size and / or a desired surface area.

[0249] Tenth aspects - forming electrode, for example for a battery or electrolytic cell

[0250] According to a tenth aspect of the disclosure, there is provided a method of forming a product comprising carbon, preferably glassy carbon, particles, for example a method as described above, such as according to the ninth or alternative ninth aspects, the method being a method of forming an electrode, for example for a metal ion battery, the method comprising the steps of:

[0251] forming carbon, preferably glassy carbon, particles by a method of producing carbon, preferably glassy carbon, material according to any preceding aspect;

[0252] forming an electrode precursor mixture comprising or consisting of the carbon, preferably glassy carbon, particles;

[0253] arranging the electrode precursor mixture in contact with a conductive substrate; and

[0254] consolidating the electrode precursor mixture to the conductive substrate to form the electrode.

[0255] Features set out below, before the next aspect is introduced, are applicable to the tenth aspect. They may also be applicable to other aspects.

[0256] Advantageously, electrodes comprising this carbon material may have superior performance over other electrodes, as described elsewhere in this disclosure.

[0257] In this context and similar contexts, the term "conductive substrate” may refer to an electrically conductive substrate, for example a substrate having an electrical resistivity of no more than 1 x105, preferably no more than 1x10-6, Ohm metres at 20 degrees Celsius.

[0258] Optionally, the conductive substrate is a current collector, for example a foil or mesh, optionally comprises or formed of a conductive metal or alloy, for example Al, Ou, Ni, Ti, or stainless steel.

[0259] Optionally, the electrode precursor mixture is formed into a slurry, applied to the conductive substrate, and dried to consolidate the electrode precursor mixture to the conductive substrate.P / 91817

[0260] Optionally, the electrode precursor mixture comprises the carbon, preferably glassy carbon, particles and an organic binder, for example carboxymethyl cellulose (CMC) and / or Polyvinylidene Fluoride (PVDF).

[0261] Optionally, the electrode precursor mixture comprises the carbon, preferably glassy carbon, particles and conductive carbon particles.

[0262] Optionally, the electrode precursor mixture comprises between 50 mass% and 95 mass% of the carbon, preferably glassy carbon, particles, between 25 mass % and 2.5 mass% of an organic binder and between 25 mass% and 2.5 mass % conductive carbon particles, preferably between 50 mass% and 90 mass% of the carbon, preferably glassy carbon, particles, between 25 mass % and 5 mass% of an organic binder and between 25 mass% and 5 mass % conductive carbon particles.

[0263] Optionally, the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a d002 plane spacing, measured for example by XRD, of between 0.36 nm and 0.45 nm, for example between 0.37 nm and 0.44 nm, for example between 0.38 nm and 0.42 nm, for example in which the product is an electrode for a lithium ion battery or a sodium ion battery or a potassium ion battery or a zinc ion battery.

[0264] Optionally, the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a BET surface area of lower than 50 m2 / g, for example lower than 30 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g, for example in which the product is an electrode for a lithium ion battery or a sodium ion battery.

[0265] Optionally, the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g, for example in which the product is an electrode for a lithium ion battery or a sodium ion battery or a potassium ion battery or a zinc ion battery.

[0266] According to an alternative tenth aspect, there is provided a method of forming a product comprising carbon, preferably glassy carbon, particles, for example a method as described above, such as according to the ninth or alternative ninth aspects, the method being a method of forming an electrode, for example for an electrolytic cell.

[0267] Features set out below, before the next aspect is introduced, are applicable to the alternative tenth aspect. They may also be applicable to other aspects.

[0268] Optionally, the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a d002 plane spacing, measured for example by XRD, of between 0.36 nm and 0.45 nm, for example between 0.37 nm and 0.44 nm, for example between 0.38 nm and 0.42 nm.

[0269] Optionally, the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a BET surface area of lower than 50 m2 / g, for example lower than 30 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g.

[0270] Optionally, the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of theP / 91817

[0271] resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g.

[0272] Optionally, the electrode is for use as an anode of a Hall-Heroult cell for aluminium production, or an anode of a molten oxide cell, or an anode of a molten salt electrolysis cell. The Hall-Heroult cell for aluminium production may operate at a temperature of between 800 and 1100 degrees Celsius. The molten oxide cell may operate at a temperature of between 1300 and 2500 degrees Celsius. The molten salt electrolysis cell may operate at a temperature of between 300 and 1000 degrees Celsius.

[0273] Optionally, the electrode is for use as an anode of a molten oxide cell used for metal production such as iron or steel production, or an anode of a molten salt electrolysis cell used for the preparation of metals and alloys, or an anode of a molten salt electrolysis cell containing hydrogen cations used for the preparation of metals, alloys and hydrogen.

[0274] Eleventh aspects - material

[0275] According to an eleventh aspect of the disclosure, there is provided a particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles, each carbon, preferably glassy carbon, particle comprising, or consisting of, carbon, preferably glassy carbon, material, preferably in which the carbon, preferably glassy carbon, material is formed by a method as described above, such as according to any previous aspect that is a method of forming carbon, preferably glassy carbon, material or particles.

[0276] According to an alternative eleventh aspect of the disclosure, there is provided a particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles, for example a particulate carbon, preferably glassy carbon, product according to the above paragraph, each carbon, preferably glassy carbon, particle comprising, or consisting of, carbon, preferably glassy carbon, material, in which the carbon, preferably glassy carbon, material is characterised by a d002 plane spacing, measured for example by XRD, of between 0.35 nm and 0.45 nm, for example between 0.36 nm and 0.44 nm, for example between 0.37 nm and 0.42 nm.

[0277] Features set out below, before the next aspect is introduced, are applicable to the eleventh and alternative eleventh aspects. They may also be applicable to other aspects.

[0278] Advantageously, this carbon material may be useful in many applications, as described elsewhere in this disclosure.

[0279] Optionally, the carbon, preferably glassy carbon, material comprises graphitic nano-crystallites having maximum dimensions in the range of 0.5 nm to 5 nm, for example 1 nm to 3 nm.

[0280] Optionally, the carbon, preferably glassy carbon, material has a Raman ID / IG value of between 0.9-1.3, for example between 1.0 and 1.2.

[0281] Optionally, the carbon, preferably glassy carbon, particles have an average particle size of between 1 micron and 1000 microns, for example between 2 microns and 800 microns, for example between 4 microns and 500 microns, or between 5 microns and 400 microns.

[0282] Optionally, the carbon, preferably glassy carbon, particles have a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the carbon, preferably glassy carbon, particles is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g.

[0283] Optionally, the carbon, preferably glassy carbon, particles have a BET surface area of lower than 50 m2 / g, for example lower than 30 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BETP / 91817

[0284] surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g.

[0285] Optionally, the carbon, preferably glassy carbon, particles are characterised by possessing both smooth and highly textured surfaces, for example in which the textured surfaces have a volcanic-like morphology, for example in which the carbon, preferably glassy carbon, particles comprise between 10% and 50% textured surfaces.

[0286] Optionally, the carbon, preferably glassy carbon, particles are characterised by a highly crystalline appearance, for example in a cuboid or cubic structure, for example in which a high proportion of particles possess sharp edges and a trihedral corner.

[0287] Optionally, the carbon, preferably glassy carbon, particles are highly porous particles, preferably in which the particles comprise rounded, semi-circular and / or through holes that extend through individual carbon, preferably glassy carbon, particles.

[0288] Optionally, the carbon, preferably glassy carbon, particles comprise a plurality of holes, and the holes have a diameter or cross-sectional dimension of between 5 nm and 500 nm, for example between 10 nm and 400 nm.

[0289] Optionally, the carbon, preferably glassy carbon, material has a single-point adsorption total pore volume of between 0.010 and 0.001 cm3 / g.

[0290] Optionally, the carbon, preferably glassy carbon, material has adsorption average pore diameter (4V / A by BET) of between 2 nm and 5 nm.

[0291] Optionally, the carbon, preferably glassy carbon, material comprises calcium carbonate crystals in a carbon, preferably glassy carbon, matrix.

[0292] Optionally, the calcium carbonate crystals have a rod-like morphology with a length to diameter ratio of between 30:1 and 1.5:1.

[0293] Optionally, the calcium carbonate crystals have a rod-like morphology with a diameter of between 20 and 500 nm, for example between 40 and 400 nm, for example in which the calcium carbonate crystals have a calcite-rhombohedral crystalline structure.

[0294] Optionally, the calcium carbonate crystals have a rod-like morphology with a length of between 30 nm and 15 micron, for example between 60 nm and 12 micron.

[0295] Optionally, the calcium carbonate crystals have a crystal size, measured perpendicular to the (104) planes of the crystals, of between 10 nm and 200 nm, for example between 20 nm and 100 nm.

[0296] Optionally, each of the particles comprises a core of a first material coated with, or encapsulated by, the carbon, preferably glassy carbon, material, for example in which the first material is a metal, alloy, ceramic, or intermetallic material, preferably in which the plurality of carbon, preferably glassy carbon, particles have an average particle size of between 1 micron and 10 mm, for example between 2 micron and 5 mm, or 5 micron and 1 mm.

[0297] Twelfth aspect - product precursor

[0298] According to a twelfth aspect of the disclosure, there is provided a product precursor mixture comprising a particulate carbon, preferably glassy carbon, product according to the eleventh or alternative eleventh aspects, the product precursor mixture further comprising one or more of a filler, a binder, and a sintering aid.

[0299] Features set out below, before the next aspect is introduced, are applicable to the twelfth aspect. They may also be applicable to other aspects.

[0300] Advantageously, such a product precursor may be used to form products comprising carbon material which are useful in many applications, as described elsewhere in this disclosure.P / 91817

[0301] Optionally, the product precursor mixture comprising a filler, for example a conductive filler component, for example conductive filler particles, preferably in which the filler component is a functional filler component, for example conductive carbon particles, preferably in which between 5 mass % and 50 mass% of the product precursor mixture comprises the filler.

[0302] Optionally, the product precursor mixture comprising a binder, for example a metallic binder, a polymeric binder, or a ceramic binder, preferably in which between 5 mass % and 25 mass% of the product precursor mixture comprises the binder.

[0303] Optionally, the product precursor mixture comprising a sintering aid, for example a metallic sintering aid or a ceramic sintering aid, preferably in which between 5 mass % and 25 mass% of the product precursor mixture comprises the sintering aid.

[0304] Optionally, the product precursor mixture comprising between 1 vol% and 25 vol % metallic particles, for example between 2.5 vol% and 20 vol % metallic particles, for example between 5 vol% and 15 vol % metallic particles.

[0305] Optionally, the product precursor mixture comprises between 50 mass% and 90 mass% of the particulate carbon, preferably glassy carbon, product, between 25 mass % and 5 mass% of a binder, for example an organic binder such as carboxymethyl cellulose (CMC) and / or Polyvinylidene Fluoride (PVDF), and between 25 mass% and 5 mass % conductive carbon particles.

[0306] Thirteenth aspects - product by consolidation

[0307] According to a thirteenth aspect of the disclosure, there is provided a non-particulate carbon, preferably glassy carbon, product comprising, or consisting of, carbon, preferably glassy carbon, material, in which the non-particulate carbon, preferably glassy carbon, product is formed by a method of forming a carbon, preferably glassy carbon, product described herein, for example as described in relation to the ninth or tenth aspects.

[0308] According to an alternative thirteenth aspect of the disclosure, there is provided a non-particulate carbon, preferably glassy carbon, product comprising, or consisting of, carbon, preferably glassy carbon, material, for example a non-particulate carbon, preferably glassy carbon, product according to the above paragraph, in which the non-particulate carbon, preferably glassy carbon, product is formed by consolidation of a particulate carbon, preferably glassy carbon, product according to the eleventh aspect, for example by consolidation of a product precursor mixture according to the twelfth aspect.

[0309] According to a further alternative thirteenth aspect of the disclosure, there is provided a non-particulate carbon, preferably glassy carbon, product comprising carbon, preferably glassy carbon, material coated onto an object, for example a non-particulate carbon, preferably glassy carbon, product formed according to a method as defined in the seventh or alternative seventh aspects.

[0310] According to an even further alternative thirteenth aspect of the disclosure, there is provided a non-particulate carbon, preferably glassy carbon, product comprising, or consisting of, carbon, preferably glassy carbon, material, for example a carbon, preferably glassy carbon, product according to the thirteenth or alternative thirteenth aspects, the non-particulate carbon, preferably glassy carbon, product comprising, or consisting of, carbon, preferably glassy carbon, material, in which the carbon, preferably glassy carbon, material is characterised by a d002 plane spacing, measured for example by XRD, of between 0.35 nm and 0.45 nm, for example between 0.36 nm and 0.44 nm, for example between 0.37 nm and 0.42 nm.P / 91817

[0311] Features set out below, before the next aspect is introduced, are applicable to the thirteenth, alternative thirteenth, further alternative thirteenth, and even further alternative thirteenth aspects. They may also be applicable to other aspects.

[0312] Advantageously, products comprising this carbon material may be useful in many applications, as described elsewhere in this disclosure.

[0313] Optionally, the carbon, preferably glassy carbon, product is a catalyst comprising carbon, preferably glassy carbon, material coated onto a substrate, preferably in which the carbon, preferably glassy carbon, material has a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g.

[0314] Optionally, the carbon, preferably glassy carbon, product is a catalyst for use in an energy production device, for example a water splitting reactor or a fuel cell.

[0315] Optionally, the carbon, preferably glassy carbon, product is a component for use in an energy storage device, preferably in which the carbon, preferably glassy carbon, material has a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g.

[0316] Optionally, the carbon, preferably glassy carbon, product is a component for use in an energy storage device, for example a battery or a capacitor.

[0317] Optionally, the carbon, preferably glassy carbon, product is an electrode for a metal ion battery, the electrode comprising carbon, preferably glassy carbon, material arranged in contact with a current collector, for example carbon, preferably glassy carbon, material coated onto a current collector, or consolidated in contact with a current collector.

[0318] Optionally, the carbon, preferably glassy carbon, product is a metal ion battery, at least one of the anode and the cathode of the metal ion battery comprising carbon, preferably glassy carbon, material arranged in contact with a current collector, for example carbon, preferably glassy carbon, material coated onto a current collector, or consolidated in contact with a current collector.

[0319] Optionally, the carbon, preferably glassy carbon, product is a vehicle battery for a vehicle such as a car or a truck, at least one of the anode and the cathode of the vehicle battery comprising carbon, preferably glassy carbon, material arranged in contact with a current collector, for example carbon, preferably glassy carbon, material coated onto a current collector, or consolidated in contact with a current collector.

[0320] Fourteenth aspect - electrode for metal-ion battery

[0321] According to a fourteenth aspect of the disclosure, there is provided an electrode for a metal-ion battery comprising carbon, preferably glassy carbon, material, in which the electrode is formed by a method according to the tenth aspect.

[0322] Features set out below, before the next aspect is introduced, are applicable to the fourteenth aspect. They may also be applicable to other aspects.

[0323] Advantageously, electrodes comprising this carbon material may have enhanced performance in metal-ion batteries, as described elsewhere in this disclosure.1

[0324] P / 91817

[0325] Optionally, the carbon, preferably glassy carbon, material is characterised by a d002 plane spacing, measured for example by XRD, of between 0.35 nm and 0.45 nm, for example between 0.36 nm and 0.44 nm, for example between 0.37 nm and 0.42 nm.

[0326] Optionally, the metal-ion battery is a lithium-ion battery or a sodium-ion battery or a potassium-ion battery or a zinc-ion battery.

[0327] Optionally, the carbon, preferably glassy carbon, material comprises graphitic nano-crystallites having maximum dimensions in the range of 0.5 nm to 5 nm, for example 1 nm to 3 nm.

[0328] Optionally, the carbon, preferably glassy carbon, material has a Raman ID / IG value of between 0.9-1.3, for example between 1.0 and 1.2.

[0329] Optionally, the carbon, preferably glassy carbon, material has a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the carbon, preferably glassy carbon, material is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g.

[0330] Optionally, the carbon, preferably glassy carbon, material has a BET surface area of lower than 50 m2 / g, for example lower than 30 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BET surface area of the carbon, preferably glassy carbon, material is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g.

[0331] Optionally, the carbon, preferably glassy carbon, material has a single-point adsorption total pore volume of between 0.010 and 0.001 cm3 / g.

[0332] Optionally, the electrode is an electrode for a sodium-ion battery and in which the carbon, preferably glassy carbon, material has a reversable sodium ion storage capacity of at least 150 mAh / g after 100 cycles at a current density of 30 mA / g, for example at least 175 mAh / g, or at least 200 mAh / g, preferably with a capacity retention rate of at least 85% after 100 cycles, for example at least 90%, or at least 91%.

[0333] Optionally, the electrode is an electrode for a sodium-ion battery and in which the carbon, preferably glassy carbon, material has a reversable sodium ion storage capacity of at least 90 mAh / g after 1000 cycles at a current density of 30 mA / g, for example at least 100 mAh / g, or at least 105 mAh / g.

[0334] Optionally, the electrode comprises the carbon, preferably glassy carbon, material and a current collector in electrical contact with the carbon, preferably glassy carbon, material, for example in which the current collector is a foil or mesh, preferably a foil or mesh comprising or formed from aluminium, copper, titanium, nickel, or stainless steel.

[0335] Optionally, the electrode comprises carbon, preferably glassy carbon, material, for example in which the electrode is formed by a method according to any of the tenth aspects.

[0336] Optionally, the electrode comprises is for use as an anode of a Hall-Heroult cell for aluminium production, or an anode of a molten oxide cell, or an anode of a molten salt electrolysis cell.

[0337] Optionally, the electrode comprises is for use as an anode of a molten oxide cell used for metal production such as iron or steel production, or an anode of a molten salt electrolysis cell used for the preparation of metals and alloys, or an anode of a molten salt electrolysis cell containing hydrogen cations used for the preparation of metals, alloys and hydrogen.

[0338] Fifteenth - sodium-ion

[0339]

[0340] According to a fifteenth aspect of the disclosure, there is provided a sodium-ion battery comprising an anode and a cathode, in which at least one of the anode and the cathode is an electrode according to the fourteenth aspect.P / 91817

[0341] Features set out below, before the next aspect is introduced, are applicable to the fifteenth aspect. They may also be applicable to other aspects.

[0342] Advantageously, electrodes comprising this carbon material may have enhanced performance in sodium-ion batteries, as described elsewhere in this disclosure.

[0343] Optionally, an initial charge capacity of the sodium-ion battery is in the range of 100 to 200 mAh / g at a current density of 30 mA / g.

[0344] Optionally, a first cycle sodium-ion storage Coulombic efficiency of the battery is between 70% and 85%. Optionally, a second cycle sodium-ion storage Coulombic efficiency of the battery is at least 90%.

[0345] Optionally, a reversable sodium ion storage capacity of the battery is at least 150 mAh / g after 100 cycles at a current density of 30 mA / g, for example at least 175 mAh / g, or at least 200 mAh / g.

[0346] Sixteenth aspect - composite

[0347] According to a sixteenth aspect of the disclosure, there is provided a composite comprising a particulate carbon, preferably glassy carbon, product according to the eleventh aspect and at least one further material.

[0348] Features set out below, before the definition section, are applicable to the sixteenth aspect. They may also be applicable to other aspects.

[0349] Advantageously, composites comprising this carbon material may be useful for many applications.

[0350] Optionally, the carbon product comprises holes, as discussed previously. Optionally, the at least one further material may extend into the holes, preferably all the way through the holes, in the carbon product.

[0351] Optionally, the at least one further material comprises a metal, and the composite is in the form of carbon, preferably glassy carbon, particles within a metallic matrix.

[0352] Optionally, the at least one further material comprises a ceramic, and the composite is in the form of carbon, preferably glassy carbon, particles within a ceramic matrix, for example in which the composite is a cement or concrete comprising the carbon, preferably glassy carbon, particles.

[0353] Optionally, the at least one further material comprises a polymer, and the composite is in the form of carbon, preferably glassy carbon, particles within a polymeric matrix.

[0354] Optionally, the at least one further material comprises calcium carbonate, and the composite is in the form of calcium carbonate particles within a carbon, preferably glassy carbon, matrix.

[0355] Optionally, the at least one further material comprises a metal, and the composite is in the form of carbon, preferably glassy carbon, particles within a metallic matrix, in which the composite further comprises a metal carbide, for example in which a metal carbide layer forms between the metal and the carbon, preferably glassy carbon, during processing of the composite, preferably in which the metal carbide is a refractory carbide, for example in which the metal carbide is a carbide selected from the list consisting of titanium carbide, tungsten carbide, zirconium carbide, molybdenum carbide, niobium carbide, tantalum carbide, vanadium carbide, hafnium carbide.

[0356] Features applicable to multiple aspects

[0357] As the skilled person would understand, features described in relation to one aspect above may apply to another aspect. In addition, also as the skilled person would understand, features described in relation to methods may be applicable to products, and vice versa.

[0358] DEFINITIONS

[0359] As used herein, and particularly as used in the above aspects of the disclosure:P / 91817

[0360] The term "glassy carbon” may refer to a single-phase carbon material. The term "glassy carbon” may refer to a material where carbon, oxygen (if present) and hydrogen (if present) make up at least 99 weight percent (wt%) of the material, and carbon makes up at least 90 wt% of the material. The term "glassy carbon” may refer to material which, when undergoing EDS analysis, shows that carbon, oxygen (if present) and hydrogen (if present) make up at least 99 weight percent (wt%) of the material, and carbon makes up at least 90 wt% of the material. The term "glassy carbon” may refer to material having only two peaks in the XRD pattern. The only two peaks may consist of a first peak appearing in the range of 20-27, preferably 20-26, degrees and a second peak appearing in the range 40-48 degrees (two-theta). The peaks may be broad peaks. The peaks may be broad peaks in the sense that a full width half maximum (FWHM) of each peak is greater than 0.3, preferably greater than 0.4, degrees. The term "glassy carbon” may refer to a material with a d002 spacing between 0.36 and 0.45 nanometres (nm). The term "glassy carbon” may refer to a material with a Raman ID / IG value of between 0.8 and 1.5, preferably between 0.9 and 1.3. The term "glassy carbon” may refer to a carbon material with a hardness of at least 3, 5 or 10 GPa. Hardness may be measured by any suitable method, such as an indentation method, such as a nanoindentation technique. This method involves recording the force acting on an indenter and a depth of indentation.

[0361] Thus, preferably, the term "glassy carbon” refers to a material where: carbon, oxygen (if present) and hydrogen (if present) make up at least 99 weight percent (wt%) of the material; carbon makes up at least 90 wt% of the material; the material has only two peaks in the XRD pattern (preferably a first peak appearing in the range of 20-26 degrees and a second peak appearing in the range 40-48 degrees (two-theta), each peak preferably having a full width half maximum (FWHM) of greater than 0.3 degrees). The material preferably has one or both of a d002 spacing between 0.36 and 0.45 nanometres (nm) and a Raman ID / IG value of between 0.8 and 1.5, preferably between 0.9 and 1.3.

[0362] Thus, particularly preferably, the term "glassy carbon” refers to a material where: carbon, oxygen (if present) and hydrogen (if present) make up at least 99 weight percent (wt%) of the material; carbon makes up at least 90 wt% of the material; the material has only two peaks in the XRD pattern (a first peak appearing in the range of 20-26 degrees and a second peak appearing in the range 40-48 degrees (two-theta), each peak having a full width half maximum (FWHM) of greater than 0.3 degrees); the material has a d002 spacing between 0.36 and 0.45 nanometres (nm); and the material has a Raman ID / IG value of between 0.8 and 1.5, preferably between 0.9 and 1.3.

[0363] The term "near-eutectic” may refer to a mixture of components having a eutectic point, where no component of the mixture is no more than 20 relative percent from its eutectic proportion. Thus, where a mixture consisting of a first component and a second component has a eutectic point where the first component makes up 40 weight percent (wt%) of the mixture, and the second component makes up 60 wt% of the mixture, then the term "near eutectic”, with reference to this mixture, covers any mixture where the first component makes up 32 to 48 wt% of the mixture, and the second component makes up 68 to 52 wt% of the mixture.

[0364] The term "particle size” may refer to a single dimension and may be used to characterise the size of a given particle. The dimension may be the diameter of a spherical particle occupying the same volume as the given particle. Particle sizes herein may be obtained using any suitable technique, such as scanning electron microscopy (SEM).

[0365] Where not otherwise specified, the term "density” may be used to refer to true density. Thus, where not otherwise specified, the density of a powder or plurality of particles may refer to the true density of the powder or plurality of particles (rather than the bulk density of the powder or plurality of particles, which can vary greatly depending on how the powder or plurality of particles are handled). The measurement of true density can be done using a numberP / 91817

[0366] of standard methods, these methods often being based on Archimedes' principle. The most widely used method, when used to measure the true density of a powder, entails the powder being placed inside a container (a pycnometer) of known volume, and weighed. The pycnometer is then filled with a fluid of known density, in which the powder is not soluble. The volume of the powder is determined by the difference between the volume as shown by the pycnometer, and the volume of liquid added (i.e. the volume of air displaced).

[0367] The term "carbonisation yield” may refer to a yield measured as a mass percent of carbon in a product produced by carbonisation or a method comprising carbonisation.

[0368] The term "metallic” may refer to a metal, alloy, intermetallic or any combination thereof.

[0369] The term "melting point”, when used with reference to two or more inorganic salts in a given proportion, may refer to the temperature at which the two or more inorganic salts would melt in that given proportion. Thus, the melting point of the two or more inorganic salts may be lower than a melting point of any of the individual inorganic salts of the two or more inorganic salts.

[0370] SOME FURTHER INNOVATION POINTS OF THE INVENTION

[0371] The current invention provides solutions to the above mentioned challenge by suggesting the utilisation of thermoplastic polymers or thermoplastic resins, through which carbonisation proceeds via the liquid-gas phase, enabling more efficient discharge of the gas phase and offering opportunities for the preparation of novel glassy carbon materials. For the purpose of definition, resin is a broad term referring to a solid or highly viscous substance of plant or synthetic origin that can typically be converted into polymers. Resins are used in various applications, including adhesives, varnishes, and as raw materials for producing plastics. One example is rosin, a natural resin obtained from the oleoresin of pine trees and other conifers. Rosin is the non-volatile fraction of the oleoresin and is primarily composed of resin acids such as abietic acid and pimaric acid. Thermoplastic resins are a subset of polymers used, for instance, as a matrix in composite materials, particularly in fibre-reinforced thermoplastics. Thermoplastic polymers form a broader category, encompassing any polymer characterized by their ability to melt when heated and harden when cooled, a process that can be repeated multiple times without significant degradation. Without being restricted by these definitions, aspects of the invention cover all thermoplastic polymers, thermoplastic resins, and rosin. Thermoplastic polymers differ from thermosetting polymers, which are characterised by their ability to form irreversible chemical bonds during the curing process, making them stable and resistant to melting upon reheating.

[0372] Common thermoplastic polymers applicable in this invention as glassy carbon precursors include polyethylene (C2H4)nwith a carbon content of around 85-92% and a melting point of 100-130°C, polypropylene (CaHeJn with about 88-91% carbon and a melting point of 160-170°C, polyvinyl chloride (CaHsCIJn, containing approximately 38-42% carbon and melting at around 75-105°C, polystyrene (CsHsJn with a carbon content of about 92% and a melting point of 240°C, polycarbonate (CieHuOsJn, which has a carbon content of 63% and melts at around 230-250°C, and polyethylene terephthalate (CwHsO^n with a carbon content of around 60% and a melting point of approximately 250-260°C. The thermoplastic polymers applicable in this invention can include naturally derived polymeric biomaterials, such as rosin and its derivatives, including polymerized rosin, which has a melting point of approximately 75-80 °C. While this invention includes various thermoplastic polymers, specific attention might be given to polyethylene terephthalate (PET), as it is widely used in single-use applications such as drink bottles and packaging materials, leading to the continuous production of large amounts of PET waste. Therefore, aspects of the current invention relate to waste-to-glassy carbon methods, and specifically plastic waste-to-glassy carbon methods.P / 91817

[0373] This invention also provides methods for preparing glassy carbon particles with one or more properties, including those characterised by smooth, textured, or porous surfaces containing circular holes, and / or crystalline-shaped glass particles. These glassy carbon particles are ideal materials for the preparation of glassy carbon objects in various sizes and shapes using conventional powder metallurgical processes, where specific polymers, ceramic materials, metals or metallic alloys can be used as binders and / or to enhance specific properties of the prepared glassy carbon objects, depending on the intended application, including thermal and electrical conductivity.

[0374] The current invention also provides methods for preparing glassy carbon coatings on objects of various sizes and shapes, imparting specific properties to their surfaces, including corrosion resistance against acidic and alkaline environments with various pH values at various temperatures, oxidation resistance, electrochemical oxidation resistance, and enhanced mechanical surface durability, such as increased resistance to wear and erosion, and hardness.

[0375] The applications of the glassy carbon materials mentioned above are extensive, requiring one or more properties, including resistance to corrosion in acidic and alkaline environments, resistance to electrochemical oxidation, and desirable electrical and / or thermal conductivity at various temperatures ranging from zero to approximately 3000°C. Potential applications include inert anodes for electrolysis units that utilise various liquid electrolytes, such as aqueous solutions, organic solvents, ionic liquids, molten salts, and molten oxides. These electrolysers can serve various purposes, including hydrogen evolution and the production of metals or alloys, such as in iron and steel manufacturing. Additionally, glassy carbon materials can be used as structural materials, particularly in applications where the aforementioned conditions are required. The methods disclosed in the invention can also be used for preparation of hybrid materials containing glassy carbon and one or more of other materials, including calcium carbonate with specific characteristics. These materials can be used in various other applications, including polymer, ceramic, and metallic composites, where the presence of glassy carbon and related materials (such as calcium carbonate) serves as fillers, enhancing specific mechanical and / or physical properties. For example, composites comprising glassy carbon materials integrated with metals and alloys, including but not limited to iron, aluminum, copper, nickel, zinc, manganese, and molybdenum, exhibit enhanced specific properties of the constituent metals and alloys. These enhancements include improved resistance to corrosion and erosion, alongside a significant reduction in material density. The described composites can be tailored to optimize performance across a range of applications where such enhanced properties are critical. Alternative applications of glassy carbon particles disclosed in this invention include energy storage systems, such as the anodes of Na-ion batteries. Some of these applications and their importance are discussed briefly in the following sections.

[0376] PRODUCTION OF IRON, STEEL AND SOME OTHER METALS AND ALLOYS

[0377] Iron and steel are fundamental materials for modern society and the global economy. With global production reaching approximately 1.9 billion tons in 2023, steel is predominantly produced using the integrated blast furnace-basic oxygen furnace (BF-BOF) route, where iron ore, scrap metal, and coke are used to produce impure molten iron. This is then refined in the BOF, generating CO2 and hazardous emissions such as SO2 and NOXfrom the oxidation of sulfur, nitrogen, and other impurities in coal and coke. Consequently, the iron and steel industry accounts for approximately 7% of global CO2 emissions, exceeding 2.5 billion tons of CO2 annually [J. Cleaner Prod. 441, 2024, 140933; Steel Times Int. 46, 2020 53-55], The depletion of high-quality metallurgical coke reserves and associated environmental concerns have driven the development of alternative technologies. Among these is the direct reduced iron-electric arc furnace (DRI-EAF) process, where natural gas, primarily methane (CH4), is often used as a reducing agent, resultingP / 91817

[0378] in reduced emissions. However, limited natural gas availability and its impurities like H2S make this option less attractive for large-scale production.

[0379] In this context, hydrogen-based production of metals and alloys has gained significant interest due to its environmentally friendly byproduct, water. However, this technology faces several challenges, including high energy requirements for water electrolysis, corrosion of electrolysis equipment (especially electrodes) in acidic or alkaline environments, and dependence on costly electrocatalysts for anodes and cathodes. Additionally, hydrogen transport from production to utilisation sites presents safety risks and adds costs. To overcome these challenges, the development of durable, corrosion-resistant, and efficient materials for both electrodes and containers is essential. A promising approach combines hydrogen and metal reduction within a single unit. This method utilises the dissolution of water in high-temperature molten salts (typically composed of hygroscopic alkali or alkali metal halide), followed by the electrolysis of hydrogen cations in the melt at approximately 500-800°C. Metal oxides, including oxides of iron, nickel, cobalt, chromium, manganese, vanadium, and tantalum, serve as cathodes in this process. Consequently, cathodic hydrogen is generated and reduces the oxides to their corresponding metals and alloys [US11897780], As the result, oxygen anions are oxidised at the anode, and using a graphite anode results in CO / CO2 formation. Thus, the development of inert anodes that primarily produce oxygen is highly desirable.

[0380] An alternative method involves the de-oxidation of metal oxides, which serve as cathodes in dried molten salts (typically a dry alkali or dry alkali metal halide such as CaCI2), at approximately 850-1000°C [US6712952], In this process, oxygen from the metal oxides, such as oxides of titanium, vanadium, tantalum, and chromium, dissolves into the molten salt and is subsequently oxidized at the anode. The use of inert anodes capable of withstanding high-temperature electrochemical oxidation conditions is highly desirable for this approach.

[0381] Molten oxide electrolysis (MOE) offers another pathway for iron and steel production [US816142], This method employs an ionically conductive electrolyte composed of molten oxide mixtures, primarily SIO2, CaO, AI2O3, and MgO, acting as solvents for dissociating iron-based oxides, and enabling ionic mass transport. During MOE, typically at temperatures in the range 1500°C to 2000 °C, metallic cations are reduced to liquid metal or ferroalloys at the cathode, while oxygen anions are oxidised at the anode. Inert anodes produce oxygen gas, whereas graphite anodes form CO / CO2.

[0382] For all the technologies mentioned above, the development of inert anodes that combine properties such as desirable electrical conductivity, physical, chemical and mechanical stability at the desired temperature, as well as the corrosion and electrochemical oxidation resistance is vital to achieving sustainable and green production of iron, steel, and other metals and alloys that can be produced by these techniques.

[0383] ALUMINIUM PRODUCTION

[0384] As the second most widely used metal globally, after iron and steel, aluminium is produced at a capacity of approximately 40 million metric tons per year, primarily through the Hall-Heroult electrolytic process. This process involves dissolving alumina (AI2O3) in molten cryolite (NaaAIFe) and electrolysing it at temperatures typically around 950-1000°C to produce molten aluminium. Graphite anodes, commonly used in this process, are consumed during the anodic reaction, resulting in the formation of carbon dioxide and other emissions, including perfluorocarbons. In contrast, inert anodes can eliminate these emissions by producing oxygen instead of CO2. Therefore, the development of inert anodes that predominantly produce oxygen at the anode of aluminium electrolysers is of great significance.

[0385] INERT ANODESP / 91817

[0386] Inert anodes proposed for the electro-production of iron, steel, aluminium and other metals and alloys include rare earths or expensive metals / alloys such as Pt, Ir, Pt-Rh and Ir-W alloys. Other suggested materials include NIFe2O4 spinel, TIB2, Cr-Fe, TIO2-RuO2, Ni-Fe-Cu, Cu-AI, and Al-Ti-Cu-M alloys [For example: US2004074625A1, CN111534837B, US2008023321A1], However, challenges related to inadequate corrosion resistance, high material costs, low electrical conductivity, and / or low thermal stability of such anode materials continue to pose significant obstacles to their widespread application in electrolysers. This is unfortunate, as the availability of high-performance inert anodes is crucial for reducing CO2 emissions and minimising or eliminating anode consumption in metal production processes, offering both environmental and economic benefits, paving the way for greener metal production. The current invention proposes thermoplastic polymer-derived glassy carbon materials as alternative candidates for inert anodes in the electro-production of iron, steel, aluminium, and other metals and alloys. The application of the proposed materials as inert anodes in the mentioned electrolysis processes offers advantages, comprising reducing or eliminating CO2 emissions, minimising or eliminating anode consumption, lowering anodic overpotential during electrolysis, maintaining structural integrity under thermal and mechanical stresses, and resisting severe corrosion or dissolution (e.g., less than 100, 80, 60, 40, 30, 25, 20, 15, 10, or 5 mm / year). Additionally, the proposed anode materials can be produced at low cost using abundant precursors, with the potential for large-scale manufacturing.

[0387] CUSTOMER GOODS AND AUTOMOTIVE APPLICATIONS

[0388] Scratch resistance is a critical property for consumer goods, such as mobile and watch cases, as it ensures aesthetic durability, maintains functionality, and enhances consumer satisfaction. Likewise, in the automotive industry, scratch resistance is crucial for maintaining the appearance and perceived quality of both interior and exterior parts. To achieve this, materials with high hardness and low density are ideal, offering resistance to abrasion while keeping products lightweight and ergonomic. For some of these applications, electromagnetic shielding property of the materials used is an important criteria of the materials used. Common solutions include ceramic composites, polymer composites with hard particles (e.g., silicon carbide or boron nitride), and metal alloys with durable coatings such as PVD (physical vapor deposition) or DLC (diamond-like carbon). These materials are processed using advanced techniques like plasma spraying, chemical vapor deposition, or 3D printing to optimize properties, ensuring uniform particle dispersion and avoiding surface defects. Such designs not only prevent scratches but also provide resistance to wear, corrosion, and environmental damage, making them suitable for applications beyond mobile and watch cases, including eyewear frames, sports equipment, and lightweight tools, thereby meeting the demands for durability and functionality in modern consumer goods.

[0389] GLASSY CARBON FIBRE

[0390] Automotive, aviation, defence, wind energy, electronics, sports goods and civil engineering sectors increasingly seek carbon fibre (CF) due to its exceptional mechanical properties, including high strength and modulus, lightweight properties, good corrosion and low impact resistance, low coefficient of thermal expansion, and high electrical conductivity. Carbon fibres are commercially produced through the pyrolysis of organic precursors based on rayon, polyacrylonitrile (PAN), and mesophase pitch, among which PAN-based fibre is the predominant precursor for the production of commercial CFs.

[0391] The production process of CFs from PAN consists of the synthesis of precursor polymer, spinning of precursor fibres, oxidative stabilisation at 200-300 °C in an air atmosphere, preventing the fibres from melting or decomposing during subsequent high-temperature carbonisation in an inert atmosphere at high temperatures [D. Jang et al., Carbon 186, 2022, 644-677], Although PAN-based carbon fibre is the most widely available type, its excessively high cost preventsP / 91817

[0392] its widespread use. Research efforts are increasing globally to develop inexpensive carbon fibres using coal tar pitch and low-value petroleum feedstocks, such as asphaltenes, as alternatives to the present PAN-based (polyacrylonitrile) carbon fibres [M.M. Amin et al., Ind. Eng. Chem. Res. 63, 2024, 15613-15636],

[0393] Aspects of this invention propose glassy carbon particles, preferentially the glassy carbon particles fabricated according to the methods disclosed in this invention, as an interesting material for the fabrication of glassy carbon fibres or glassy carbon-containing composite fibres that transfer the distinguished properties of glassy carbon particles into fibrous configurations, applicable to various applications that are generally expected for carbon fibres. According to aspects of this invention, the glassy carbon fibres can be fabricated using glassy carbon particles, without being restricted by the method, for example, using conventional methods, for example, using a wet-spinning method, similar to the method used for the preparation of graphene oxide fibres [Ma et al., J. Electroanal. Chem. 975, 2024, 118740] and MXene composite fibres [Yang et al., J. Colloid Interf. Sci. 682, 2025, 875-883],

[0394] CALCIUM CARBONATE CRYSTALS

[0395] Aspects of the current invention relate to hybrid materials composed of glassy carbon and calcium carbonate, which demonstrate properties superior to those of certain other materials. Calcium carbonate (CaCOa) exists in several polymorphic forms: calcite, aragonite, and vaterite, among them calcite is the most stable form, characterised by a rhombohedral crystal structure. Aragonite is a metastable form with an orthorhombic crystal structure, while vaterite is the least stable and rarest form, featuring a hexagonal crystal structure. Calcium carbonate is a versatile, environmentally friendly compound with numerous applications across various industries, including construction, paper production, plastics and polymers, paints, coatings, and the rubber industry. It is a primary component in the production of cement and concrete, contributing significantly to their strength and durability. Synthetic high-purity calcium carbonate can be produced through a recarbonization process, involving the conversion of limestone into calcium oxide and carbon dioxide via calcination at high temperatures, followed by the preparation of water-based milk of lime, purification, and recarbonization using the carbon dioxide generated during the first stage. This process comprises multiple steps, including the generation of carbon dioxide. In view of the extensive applications of calcium carbonate, the development of methods for preparing this compound with high purity and desirable morphologies through environmentally friendly techniques represents a commercially and environmentally significant advancement.

[0396] Aspects of the current invention relate to high-purity synthetic calcium carbonate crystals with specific properties, such as unique morphologies, that offer advantages for certain applications compared to certain other materials. Aspects of the invention relates to hybrid structures comprising glassy carbon particles and calcium carbonate crystals, which exhibit advantages for specific applications, including polymer, ceramic, and metallic composites, comparing to certain other materials. Additionally, aspects of the invention relate to methods for preparing these novel structures, which are simpler, more environmentally friendly, and / or more cost-effective than certain existing methods used for producing comparable materials for similar applications.

[0397] ANODE OF SODIUM ION BATTERIES

[0398] Efficient and low-cost renewable energy storage remains a challenge for widespread applications across various sectors. Currently, Li-ion batteries (LIBs) are the state-of-the-art energy storage technology due to their high energy density and technological maturity. However, alternative technologies, such as sodium-ion batteries (SI Bs) have gained increasing attention as a cost-effective alternative to the more expensive LIBs, offering advantages such as the abundance and low cost of sodium resources. A SIB consists of negative (anode) and positive (cathode) electrodes, along with an electrolyte, and the development of low-cost, high-performance electrode materials is a key goal for theP / 91817

[0399] further advancement of these batteries. Current mainstream SIB anode materials, including hard carbon materials, metal oxides and alloys often suffer from poor Na-ion storage capacity and / or cycling performance, limiting the further development of SIBs. Moreover, the green and low-cost production of such materials is essential, with waste valorisation being an attractive approach. In this context, the carbonisation of various waste materials including biomass [US2021242462] has been proposed for possible Na-ion storage applications. In comparison with biomass waste, the conversion of plastic materials into carbons for energy storage applications has received considerably limited attention, due to alternative approaches including the recycling of plastic waste. Aspects of this invention relate to glassy carbon materials and their preparation methods for Na-ion storage application.

[0400] CARBON-CATALYST SYSTEMS FOR DIAMOND SYNTHESIS

[0401] Carbon is a versatile element found in over ten million compounds, including hydrocarbons, carbonates, carbon dioxide, and various elemental allotropes such as glassy carbon, graphite, and diamond. Among these, diamond stands out as the most expensive carbon material due to its exceptional properties, including unmatched hardness, highest known thermal conductivity, remarkable chemical resistance and beauty. These attributes make diamond invaluable across multiple industries, sparking significant scientific and economic interest in converting other carbon forms into diamond. The transformation of hexagonal graphite into cubic diamond can be achieved through the high-pressure, high-temperature (HPHT) method, which requires pressures exceeding 12 GPa and temperatures above 2000 °C. Alternatively, graphite can be dissolved in a catalyst, allowing carbon atoms to re-precipitate as diamond under less extreme conditions [US 2947608, US 2947609, US 2947610], Various catalysts, predominantly Group VIII metals such as Fe, Ni, Co, and their alloys (especially iron-based alloys) have been extensively utilised for diamond synthesis under HPHT conditions. For example, the Fe64Ni36 alloy is widely used in both industrial production and scientific research for synthesizing synthetic diamond [J. Wang et al., CrystEngComm, 2023, 25, 1884-1893], using which the diamond formation could be achieved at 5.7 GPa (1300 °C) over a duration exceeding 23 hours [S. Fang et al., CrystEngComm, 2021, 23, 1406-1414], A catalyst containing Ni (69 wt%), Fe (26 wt%), and Co (5 wt%) could form diamond at 5.5 GPa (1380 °C) over a duration in the range from 50 to 200 hours [US9039832B2], During this process, the catalyst is likely to become supersaturated by absorbing carbon from graphite, leading to the precipitation of cementite (FeaC) and the subsequent nucleation of diamond [H. Li et al., Carbon, 2010, 48, 3003], However, as the conventional HOHT process demands prolonged periods under harsh conditions, reducing the required time, pressure, and temperature for diamond nucleation and growth offers significant economic and technological advantages.

[0402] Certain aspects of the present invention involve the use of a carbon-catalyst system with a large interface, preferably adopting a core-shell morphology for diamond formation. Specifically, the invention relates to a carbon-catalyst system where a carbon phase encapsulates a catalyst, enabling a high diffusion rate of carbon into the catalyst. In some embodiments, the carbon phase consists of a nanostructured graphitic carbon. In other embodiments, the encapsulated catalyst has dimensions of less than 10 pm, 5 pm, 1 pm, 500 nm, 300 nm, 100 nm, 10 nm, or even 5 nm, while remaining larger than 1 nm. This close interaction between the encapsulated catalyst and the carbon phase offers a significant advantage, as it facilitates the HPHT process by substantially reducing the processing time, the processing temperature, and or the processing pressure in comprising with traditional HPHT process. Further embodiments of the invention involve a carbon-catalyst system where a carbide layer is present between the nanostructured graphitic carbon phase and the encapsulated catalyst. In this carbon-carbide-catalyst system, the carbide layer plays a role in enhancing diamond nucleation and growth during the HPHT process. Additional aspects of the invention relate to methods for preparing the carbon-catalyst and carbon-carbide-catalyst systems. TheseP / 91817

[0403] methods may include the use of a thermoplastic polymer as the carbon source, providing a practical and efficient route for synthesising these systems.

[0404] NANOPOLYCRYSTALLINE DIAMOND

[0405] Nanopolycrystalline diamond (NPD), composed of randomly oriented diamond nanoparticles (for instance 10-20 nm) with abundant grain boundaries, exhibits exceptional hardness (110-140 GPa), thermal stability (-1200 °C in inert atmospheres), wear resistance, fracture toughness, and optical transparency from ultraviolet to far-infrared [T. Irifune, Nature, 2003, 421, 599-600], These properties make NPD ideal for cutting, grinding, and polishing tools, thermal management in high-power electronics, high-power laser lenses, and durable coatings for extreme environments such as space and reactors. Its biocompatibility and functionalisation potential enable applications in drug delivery, molecular imaging, and neural interfacing electrodes, while lattice defects make it valuable for quantum and magnetic technologies. NPD is synthesized by subjecting high-purity polycrystalline graphite to ultra-high pressures (12-25 GPa) and temperatures (2300-2500 °C), but the limited availability and high cost of this precursor drive efforts to explore alternative carbon sources for production. Using a C60 precursor, NPD with a grain size of 5-12 nm can be synthesised at 20 GPa and =2000 °C for 60 minutes, followed by quenching or slow cooling [Diamond and Related Materials, 2005, 14, 16-22], Another method involves producing glassy carbon by pyrolyzing thermosetting furfuryl alcohol (FFA) at temperatures above 1500 °C in vacuum. This process includes multiple steps: adding nitric acid to an FFA solution at room temperature, allowing the mixture to stand for 24 hours, aging it for several hours, pyrolyzing the aged resin under vacuum at high temperatures for one hour, pulverizing the resulting product, and loading it into a high-pressure sample cell for NPD production [O. Fukunaga et al., Diamond and Related Materials, 2005, 14, 160-166], Other methods use commercially available glassy carbon (e.g., Tokai Carbon, Japan) to produce cubic diamond with particle sizes ranging from 50 to 200 nm and hardness values of 95-112 GPa by treating it at 21 GPa and 2250 °C for 6 minutes [Journal of Materials Research, 22, 2007, 2345-2351], However, the existing methods for producing carbon precursors like C60 and glassy carbon are costly due to their complexity, highlighting the need for simpler and more economical approaches to preparing carbon precursor materials with the ability to control their structure, morphology, and surface properties.

[0406] Certain aspects of the present invention relate to the use of glassy carbon materials, as disclosed herein, as precursor materials for diamond nucleation and / or growth. The glassy carbon materials disclosed in this invention offer significant advantages over other glassy carbon materials due to their unique preparation process, as described herein, which enables the fabrication of various forms of glassy carbon materials, at potentially low-cost. These forms include crystalline-shaped glassy carbon particles, glassy carbon particles with textured surfaces, and porous glassy carbon particles, and metal / alloy-encapsulated carbon. Accordingly, the scope of this invention encompasses the disclosed glassy carbon materials in all their forms, irrespective of their production process, as well as the glassy carbon materials in combination with their associated production processes.

[0407] GLASSY CARBON AND POROUS GLASSY CARBON POWDER

[0408] Glassy carbon offers several advantages due to its unique properties, including high corrosion and oxidation resistance, making it ideal for harsh chemical and high-temperature environments. Its exceptional hardness makes it suitable for durable, wear-resistant components, while its tuneable electrical conductivity and electrochemical properties allows for applications in electrochemical sensors, energy storage, and electronic devices. Additionally, glassy carbon is biocompatible and electrochemically inert, making it useful in medical devices like neural electrodes and microneedles. Its stability at high temperatures enables its use in moulds for manufacturing, and its precision processing capabilitiesP / 91817

[0409] are valuable in microfabrication for industries like aerospace and medical devices. However, the preparation of monolithic glassy carbon using conventional methods involving moulding, curing, and firing of thermosetting resins faces high costs and scalability issues, which arise from the formation of defects during the removal of gas species from the resin and significant shrinkage that occurs during carbonization. Moreover, the Glassy carbon's brittleness and high hardness present challenges in machining using conventional techniques, often requiring specialised methods such as laser ablation or reactive ion etching.

[0410] To address these challenges, aspects of the present invention propose the use of powder metallurgical processes to fabricate monolithic glassy carbon, utilising pre-fabricated glassy carbon particles or powders of various dimensions. This approach is particularly advantageous for fabricating larger objects, ranging from, for example, 1 cm to 10 cm, or preferably 10 cm to 3 m, where traditional methods of manufacturing monolithic glassy carbon are not applicable. The invention enables the formation of glassy carbon into three-dimensional objects through established powder metallurgical techniques. Additionally, this method eliminates or reduces the need for machining, thereby reducing costs and simplifying the overall process.

[0411] While aspects of the present invention relate to the powder metallurgical processing of glassy carbon powders in general, certain aspects specifically relate to the powder metallurgical processing of glassy carbon particles fabricated using the methods disclosed herein. These aspects of the invention are critical in the powder metallurgical processing of glassy carbon objects, as traditional methods of producing glassy carbon particles or powders are typically multi-step processes that are expensive to operate.

[0412] For instance, JP 6359963 discloses a multi-step method for producing glassy carbon particles by dropping an initial condensate of a phenol resin into a solution containing a curing agent to form and cure granules, followed by calcination and carbonization to obtain glassy carbon granular bodies. This method yields a minimum particle size of approximately 1 mm, which does not qualify as a powder and necessitates additional pulverisation steps. Due to the exceptional hardness of glassy carbon materials, such pulverisation is particularly challenging, significantly increasing production complexity and cost. Similarly, JP 3164416 proposes the use of a foam of thermosetting resin as the raw material, which is pulverised either before or after firing. However, this method faces limitations due to particle agglomeration during firing. Another approach, disclosed in JP H05163007A, describes the production of spherical glassy carbon powder by forming thermosetting resin microspheres, subjecting them to a two-stage curing process involving acid immersion followed by heating (150-300 °C), and subsequently carbonizing in a non-oxidizing atmosphere at 800-1500 °C. While this method achieves spherical powder, the reliance on acid treatment and the complexity of the process further limit its practicality. Moreover, the method described in CN106187192 for preparing glassy carbon demonstrates complexity, involving multiple intricate steps. These include dispersing graphene in deionized water with the aid of a surfactant to create a graphene solution, followed by the addition of phenolic resin to form a slurry. The slurry is subsequently dried and subjected to ball milling for 5 hours at a rotation speed of 400 rpm. The resulting powder is then pressed to form a green body, which undergoes curing for several hours. This is followed by a multistage carbonization process conducted in an oxygen-free or inert atmosphere at progressively higher temperatures, including 350°C, 750°C, 1000°C, and finally 2500°C, requiring precise control and extended durations at each stage to achieve the desired glassy carbon structure.

[0413] Consequently, the available glassy carbon powder is currently prohibitively expensive, for instance, with costs exceeding 2000 USD per kilogram, thereby limiting its economic viability for many industrial applications. One commercially available grade, SIGRADUR, comprises spherical particles with diameters ranging from 0.4 to 15P / 91817

[0414] microns, produced through the pyrolysis of thermosetting phenolic resins at temperatures between 1000°C and 2200°C in inert atmosphere. These particles exhibit closed voids approximately 1 to 2 nm in diameter, a density of 1.5 g / cm3, and a limited BET surface area of approximately 2 m2 / g [A. Braun et al., Carbon 40, 2002, 375-382], Aspects of the present invention address these limitations by providing innovative and cost-efficient methods for the sustainable fabrication of glassy carbon particles. These methods enable the control over the production of a wide variety of glassy carbon powders, offering tuneable properties such as BET surface area, pore volume, and morphological characteristics. The powders produced by these methods facilitates the efficient fabrication of monolithic glassy carbon objects, composites, and coatings while overcoming the cost and scalability barriers of existing techniques.

[0415] A specific morphology that can be obtained using the methods disclosed in the present invention is porous glassy carbon. This material exhibits a broad spectrum of potential applications, including serving as a corrosion -resistant, thermally stable, and electrically conductive support for catalysts. These include catalysts for fuel cells, such as those facilitating oxygen reduction reactions (ORR); water electrolysers, such as those enabling oxygen evolution reactions (OER) and hydrogen evolution reactions (HER); and other electrochemical cells, such as the electrodes used in batteries, including lithium-air (Li-air) batteries, for example, the air-cathode catalyst.

[0416] Examples of such catalysts include compounds based on elements such as platinum (Pt), ruthenium (Ru), gold (Au), nickel (Ni), cobalt (Co), iron (Fe), molybdenum (Mo), and manganese (Mn). Additionally, the catalysts may comprise advanced materials such as metal-organic networks (e.g., heterobimetallic organic catalysts featuring single iron and cobalt atoms) and borophene-based compounds.

[0417] The methods disclosed in the present invention for the preparation of porous glassy carbon suitable for use as a catalyst support offer significant advantages over certain existing methods for the preparation of porous glassy carbon. These advantages include increased simplicity, enhanced environmental cleanliness, reduced cost, and improved quality and specific characteristics of the resulting product.

[0418] For example, JP2006294468 discloses a method for the preparation of porous glassy carbon. In this method, a mixture of rayon pulp and softwood pulp is subjected to a papermaking process to produce a sheet. A solution is prepared by dissolving phenol resin (50 wt%) in ethanol. The sheet is then impregnated with the phenol resin solution, thermally cured, and subsequently subjected to carbonization treatment in a nitrogen gas atmosphere at 1000°C. During this process, the rayon and softwood pulps are thermally decomposed, while the phenolic resin undergoes pyrolysis and carbonization. The resulting carbonized material is transferred to an activation furnace and activated at 950°C to produce porous glassy carbon. Finally, the obtained porous glassy carbon is pulverized using a ball mill for 12 hours to generate a porous glassy carbon powder.

[0419] In contrast to the prior art, the present invention discloses both methods and products that utilise a thermoplastic polymer in conjunction with a rapid conversion process. These methods enable the fabrication of porous glassy carbon with a diverse range of morphologies and characteristics. The resulting products are suitable for various applications, offering enhanced versatility and performance compared to existing technologies.

[0420] SOME ASPECTS OF THE INVENTION

[0421] (A) Glassy Carbon Materials

[0422] Some aspects of the present invention relate to glassy carbon particles with smooth, textured, or porous surfaces. Other aspects relate to glassy carbon particles in physical contact with calcite crystals. In certain embodiments, the glassy carbon particles are porous, featuring circular or semi-circular holes, and / or the calcite crystals exhibit rod-likeP / 91817

[0423] morphologies. Further aspects of the invention relate to crystalline-shaped glassy carbon particles. Additional aspects relate to glassy carbon particles containing graphitic domains with sizes ranging from less than 10 nm, 9 nm, 8 nm, 7 nm, 6 nm, 5 nm, 4 nm, or 2 nm to greater than 1 nm. The invention also includes glassy carbon coatings applied to various substrates, including polymer materials, carbon materials (such as graphite), ceramic materials, or metals / metallic alloys. In some embodiments, the glassy carbon coating is applied to a ceramic or metal / metallic alloy substrate, with an interlayer phase present at the interface between the glassy carbon coating and the substrate. The interfacial material may, in some embodiments, comprise a carbide.

[0424] While the above-mentioned aspects of the invention describe the glassy carbon materials in general, other aspects of the invention relate to glassy carbon products featuring the described characteristics, fabricated using the methods disclosed herein. Additionally, certain aspects of the invention relate to monolithic objects constructed from glassy carbon particles prepared using these methods. The invention comprehensively covers both the materials and the methods of their preparation. In some embodiments, these methods employ thermoplastic polymers as the carbon source for producing the described products, making them suitable for a wide range of applications.

[0425] (B) Production of Glassy Carbon Materials

[0426] While some aspects of the invention relate to the preparation of glassy carbon, some other aspects relate to the preparation of composites or hybrid materials incorporating the glassy carbon, preferentially combining its unique properties with those of other materials to create high-performance components for specific applications. Accordingly, this invention encompasses both glassy carbon materials and methods for their production, processing, and integration into diverse applications. These applications include, but are not limited to, inert anodes for the electro-production of metals such as iron, steel, aluminium, and other alloys. Additional applications include energy storage systems, such as electrodes for sodium-ion batteries, as well as electrodes and structural components for acidic and alkaline watersplitting systems utilised in hydrogen production.

[0427] Some aspects of the invention involve the green, fast, and efficient preparation of glassy carbon materials, including glassy carbon particles with specific characteristics, followed by consolidation of the glassy carbon materials to fabricate monolithic objects of interest.

[0428] In these embodiments, monolithic refers to a consolidated body that can include materials made from a single material, as well as composites, hybrid materials, and coated samples. In this context, monolithic materials are unified and solid, formed into a cohesive, continuous structure without the discrete units or loose particles characteristic of powders or individual particles. This term encompasses both materials made from one type of substance and those formed by combining multiple components into a unified whole, in contrast to the separate, non-consolidated nature of powders and particles.

[0429] The production methods for the preparation of glassy carbon particles may involve the thermal treatment of a thermoplastic polymer or a mixture comprising at least one thermoplastic polymer at temperatures exceeding the melting point of the thermoplastic polymer.

[0430] In certain embodiments, the thermal treatment is conducted in a reducing atmosphere, for instance in an atmosphere containing 0.5 to 100% H2, resulting in glassy carbon particles characterized by the crystalline shapes and smooth surfaces.

[0431] In certain embodiments, the thermal treatment is performed in an air atmosphere, resulting in glassy carbon particles exhibiting smooth and volcanic-like textured surfaces. The particle sizes may range from approximately 1 pm to 300 pm, including, for example, particles with dimensions of 1.9 pm, 29.5 pm, 73.0 pm, 65.7 pm, 91.8 pm, 125.7 pm, 133.0P / 91817

[0432] pm, 159.9 pm, 163.3 pm, 224.2 pm, and 237.3 pm. The particles obtained through the disclosed methods may be sieved to achieve uniform size distribution without the need for additional processing steps, such as ball milling, which can be challenging due to the inherent hardness of the glassy carbon particles. In certain embodiments, the presence of glassy carbon particles with a range of sizes offers distinct advantages in powder metallurgical processing. Specifically, the varied particle sizes facilitate improved packing density and consolidation during the processing of glassy carbon powders, thereby enhancing the efficiency and quality of the resulting consolidated materials. This capability represents a significant benefit of the methods described in this invention. The glassy carbon particles may further be characterized by sharp edges and trihedral corners with fractured, jagged, and vesicular features. Additionally, the particles may exhibit porosity, including blind spherical holes with dimensions ranging from approximately 1 pm to 7 pm. Without being limited to a specific mechanism, it is believed that the formation of the volcanic-like textures results from the transition of the material from a liquid phase to a solid phase, combined with the escape of gases during the carbonisation process. This mechanism produces features resembling those observed in volcanic eruptions, contributing to the unique surface morphology of the alumina particles. In some embodiments, the carbonisation yield ranges from 30% to 60%, depending on the carbonisation temperature and duration. In some embodiments, the sharpest peak in the XRD pattern of the glassy carbon positions at a two-theta values in the range 22.0°C to 23.0°C, with doo2 value in the range 0.380 nm to 0.410 nm, depending on the carbonisation temperature and duration. For example, a carbonisation yield of 44.8% can be achieved at a temperature of 800°C with a short dwell time of 10 minutes at the maximum temperature, producing a glassy carbon with sharpest peak located at the two-theta values 22.16°. In certain embodiments, the presence of textured surfaces on the glassy carbon particles provides advantages for specific applications, including their use as electrodes in metal-ion batteries and in the consolidation of powders to produce composites using sintering aids. The textured surfaces enhance the functional properties of the resulting materials, such as improved adhesion, surface area, and interfacial bonding. In certain embodiments, the glassy carbon particles exhibit N2adsorption-desorption isotherms with an H4 hysteresis loop, as classified by IUPAC [K. Sing, Pure & Appl. Chem. 57, 1985, 603—619], This behaviour is indicative of narrow slit-shaped pores or a combination of complex mesopores and micropores. The particles are characterized by a BET surface area ranging from approximately 400 to 700 m2 / g, for example, 515.2 m2 / g. Furthermore, the extent and complexity of the textured surfaces can be enhanced through the use of inorganic salts, as described in greater detail below. This modification offers additional versatility and performance optimisation for various industrial and technological applications. In certain embodiments, the said feedstock mixture, in addition to the thermoplastic polymer, comprises one or more inorganic salts. In these embodiments, the thermal treatment is conducted in an atmosphere comprising or consisting of air, an inert gas, or a reducing gas, and the thermal treatment results in glassy carbon particles characterised by the presence of textured surfaces with a volume fraction of more than 10%, more than 20%, more than 30%, more than 40%, more than 50%, more than 60%, more than 70%, or more than 80%, and a maximum of 99%.

[0433] In these embodiments, the inorganic salts are chemical compounds composed of positively charged ions (cations) and negatively charged ions (anions) held together by ionic bonds, exhibiting high solubility in polar solvents, and preferentially in water; for example, between 10-200 g per 100 mL of water at 0°C to 100°C. The inorganic salts preferentially have a melting point of less than 1500°C, less than 1400°C, less than 1300°C, less than 1200°C, less than 1100°C, less than 1000°C, less than 900°C, less than 800°C, less than 700°C, less than 600°C, less than 500°C, less than 400°C, less than 300°C, or less than 200°C, and greater than 100°C, greater than 200°C, greater thanP / 91817

[0434] 300°C, greater than 400°C, greater than 500°C, or greater than 600°C. The appropriate melting point of the salt can be determined based on the melting temperature of the thermoplastic polymer and its carbonisation temperature. In certain embodiments, the inorganic salt comprises an alkali metal halide, an alkaline earth metal halide, an alkali metal nitrate or an alkaline earth metal nitrate. In some embodiment, the inorganic salt comprises of calcium chloride (CaCI2), magnesium chloride (MgCI2), strontium chloride (SrCI2), barium chloride (BaCI2), calcium fluoride (CaF2), magnesium fluoride (MgF2), strontium fluoride (SrF2), barium fluoride (BaF2), beryllium chloride (BeCI2), and beryllium fluoride (BeF2), sodium chloride (NaCI), potassium chloride (KCI), lithium chloride (LICI), sodium fluoride (NaF), potassium fluoride (KF), lithium fluoride (LIF), sodium bromide (NaBr), potassium bromide (KBr), lithium bromide (LIBr), sodium iodide (Nal), potassium iodide (KI), lithium iodide (Lil), sodium nitrate (NaNO3), potassium nitrate (KNO3), lithium nitrate (LINO3), rubidium nitrate (RbNO3), cesium nitrate (CsNO3), calcium nitrate (Ca(N03)2), magnesium nitrate (Mg(N03)2), barium nitrate (Ba(N03)2), or strontium nitrate (Sr(N03)2).

[0435] Preferably, the inorganic salt functions in one or more of the following manners:

[0436] (a) Particles of inorganic salt may remain solid while the thermoplastic polymer is in a molten state, thereby becoming incorporated into both the polymer melt and the subsequent glassy carbon obtained after the carbonisation of the polymer melt. Under these conditions, the inorganic salt creates porosity and / or textured surfaces in the glassy carbon product. The inorganic salt can then be easily removed by washing the glassy carbon product with water or an appropriate solvent, leaving behind glassy carbon particles with a porous or textured surface. In some embodiments, the porosity and textured surfaces of the glassy carbon are advantageous for various applications. For instance, in glassy carbon composites, these features allow better integration of a secondary phase (such as a ceramic, polymer or metallic / alloy binder) with the glassy carbon. Additional applications of the glassy carbon materials include their use in energy storage devices, such as metal-ion batteries, where the textured or porous surfaces of the glassy carbon materials provide significant advantages. Specifically, the porosity and textured surfaces facilitate enhanced incorporation of the electrolyte into the glassy carbon material, thereby reducing ionic and electronic diffusion pathways and improving the overall performance of the glassy carbon as an electrode material, for example as the anode material of Na-ion batteries. Furthermore, the glassy carbon material is also applicable as a catalyst support. In this context, the textured surface and porosity enable a high deposition density of catalyst particles, which is advantageous for applications in fuel cells, water-splitting electrolysers, lithium-air cathodes, and other similar applications.

[0437] (b) During the thermal treatment of the feedstock comprising the thermoplastic polymer, particles of the inorganic salt may undergo melting. In this case, the molten salt serves to protect the glassy carbon product from severe oxidation, particularly at temperatures exceeding 600°C, when the process is conducted in an oxidative atmosphere, such as one containing oxygen.

[0438] In some embodiments, the inorganic salt comprises sodium chloride (NaCI), potassium chloride (KCI), or combinations thereof. A person skilled in the art can adjust the melting point of the inorganic salt mixtures within the range of 200°C to 1600°C. For example, a mixture containing NaCI and KCI in specific proportions can achieve a melting point of approximately 658°C, near the eutectic point of the NaCI-KCI binary system.

[0439] In some embodiments, the presence of inorganic salts during synthesis enhances the textured surfaces of the glassy carbon particles, thereby significantly increasing the efficiency of the subsequent ball milling process in augmenting the surface area of the glassy carbon particles by approximately 200-300%, for instance for 244%. This enhancement is remarkable, considering the high hardness of glassy carbon particles, making the ball milling of certain other glassy carbon particles a challenge.P / 91817

[0440] (c) The present invention discloses that the inclusion of an appropriate inorganic salt can induce the formation of a secondary phase during the thermal treatment of the thermoplastic polymer. In certain embodiments, the inorganic salt comprises a calcium halide, such as calcium chloride, and the secondary phase formed is calcium carbonate. In some embodiments, the secondary phase develops on the surface of the glassy carbon product obtained by the carbonisation of the polymer, rendering the surface porous with features such as circular or semi-circular holes. The porous glassy carbon material produced through this process offers significant advantages across a range of applications, including its use in composites, hybrid structures, and as a support material for catalysts for various industrial and scientific applications. Even though CaCl2 may offer advantages in terms of physical properties and cost, other calcium-containing inorganic salts can also be applicable in these embodiments.

[0441] For instance, while CaF2and CaCI2have melting points of 1418°C and 772°C, respectively, a person skilled in the art can adjust the melting point of the inorganic salt to a desired value. For example, a mixture of CaCl2 and NaCI can provide a melting point of approximately 504°C, near the eutectic composition of the CaCl2-NaCI binary system. Examples of alternative salts include CaCl2-NaCI-MgCl2, which has a melting temperature of around 420°C; CaCl2-NaCI-KCI-MgCl2, with a melting point of 385°C; CaCh-NaCI-KCI, with a melting point of around 481°C; and CaCI2-LICI-KCI, with a melting point of 332°C.

[0442] In these embodiments, the presence of the calcium-containing inorganic salt during the thermal treatment of the polymer feedstock results in synergistic effects, including the formation of the glassy carbon as the primary phase, and sodium carbonate crystals as the secondary phase. In some embodiments, this process can be explained by at least two effects: (1) the nucleation and growth of the secondary phase from the primary phase or an intermediate phase driven from the polymer feedstock, and (2) imparting porosity to the glassy carbon.

[0443] In certain embodiment, the inorganic salt contains calcium cations, such as CaCl2 and the porous glassy carbon contains circular and / or semi-circular holes. In these embodiments, the secondary phase comprises calcium carbonate, where the calcium and carbon of the calcium carbonate originate from CaCl2 and the polymer, respectively.

[0444] Certain aspects of the invention relate to calcium carbonate particles with rod-like, interconnected rod-like, or hook-like morphologies, with calcite crystalline structure. These calcium carbonate morphologies are beneficial for various applications, for instance in composite materials, as they provide enhanced grip to the substrate and improve the mechanical properties of the resulting composite. Examples of the applications include composites with polymeric, ceramic or metallic substrate and rod-like, interconnected rod-like, or hook-like calcium carbonate particles as the reinforcing component. The composite materials include concrete.

[0445] Aspects of the current invention relate to combination of synthetic calcium carbonate crystals and porous glassy carbon particles. The synthetic calcium carbonate crystals and porous glassy carbon particles can be physically mixed, or can be connected at certain locations. Calcium carbonate component of the combination can have rod-like, interconnected rod-like, or hook-like morphologies, with a calcite crystalline structure. This combination provides advantages in various applications including ceramic-, polymeric- and metal-based composites, where the penetration of the substrate around calcium carbonate crystals, and through the holes of the porous glassy carbon particles improves the properties of the composite, including the mechanical and / or physical properties of the composite. The composite materials include concrete.

[0446] In some embodiments, the porous carbon particles (with mostly through holes) and connected CaC03rod-like and hook-like crystals can be used for the preparation of composite materials. In some specific embodiments, the combination of porous glassy carbon particles and rod-like (and hook-like) CaCOa crystals can be used for theP / 91817

[0447] preparation of composite materials, in which the penetration of an additional phase into the holes of the porous carbon and around rod-like and hook-like CaCOa crystals can promote physical and / or mechanical properties of the resulting composites. The additional phase involved in the resulting composite can be a polymer like polypropylene (PP), polyethylene (PE), polyvinyl chloride (PVC), rubbers or biodegradable polymers such as polylactic acid (PLA) or polybutylene succinate (PBS) to be used in various applications including automotive parts, packaging, tires, seals, and gaskets, household items, plastic films, pipes, profiles, and flooring materials containers. In some embodiments of this invention, the additional phase involved in the resulting composite can be concrete. In this case, the porous carbon / rod-like and hook-like CaCOa crystals act as fillers in the concrete, improving one or more of properties including the compressive strength of the concrete, and / or its durability and resistance against crack formation and propagation. In some embodiments, the additional phase involved in the resulting composite can be a metal, a metallic alloy, or an intermetallic alloy, containing metallic materials such as aluminium and magnesium. The resulting composites with enhanced properties like strength, wear resistance, or thermal stability, and can be used in the preparation of lightweight components for aerospace and automotive industries, where the porous glassy carbon and rod-like or hooklike CaCOa crystals act as reinforcing agents, enhancing the composite's mechanical properties and / or physical properties. In some embodiments, the additional phase involved in the resulting composite can be a ceramic, a polymer, a metal or an alloy, and resulting composite can be used as structural component with enhanced physical and mechanical properties. In some embodiments, the additional phase involved in the resulting composite can be a ceramic, a polymer, a metal or an alloy, and resulting composite can be used as coating applied to other objects to enhance their surface properties such as corrosion-resistance. The resulting coated objects can be used in various applications such as marine structures, pipelines, and infrastructures exposed to aggressive environments. According to this aspect of the invention, the porous glassy carbon and CaCOa crystals provide a passive layer that slows down the corrosion of the substrate.

[0448] In some embodiments of the current invention, a combination of porous glassy carbon particles (with mostly through holes) and CaCOa crystals is formed, and then the CaCOa content of the combination is removed partially or totally to form porous carbon particles as the only component or the major component with mass fraction in the range 60-100%, 70-100%, 80-100%, 90-100%, 95-100% or 97-100%. In some embodiments of the invention, the porous glassy carbon made is used for the fabrication of a composite structure, containing the glassy porous carbon and an additional phase. In some embodiments, the additional phase is a polymer, a ceramic, a metal, and intermetallic material or a metallic or ceramic alloy. In some embodiments of the invention, the second phase is a high entropy alloy (HEA). In some specific embodiments, the second phase is a high entropy oxide (HEO).

[0449] In some embodiments, treating the glassy carbon-calcite hybrid material with an acidic solution having a pH of less than 7 and greater than 1, for a sufficiently prolonged time in the range of 1 second to 5 hours, and at a temperature in the range of 0-100°C, reduces the calcite content of the hybrid material or completely removes it. The acid washing process can produce pure or nearly pure porous glassy carbon particles. In certain embodiments, these pure or nearly pure porous glassy carbon particles are advantageous for enhancing the physical and / or chemical properties of various composite materials, such as concrete and asphalt, and for improving electrochemical performances in applications like electrodes for metal-ion batteries, including Na-ion batteries.

[0450] In some embodiments, the porous glassy carbon material can be used as a support to accommodate catalysts for applications in electrochemical cells such as fuel cells, hydrogen production electrolysers, metal-air batteries, or metal-sulphur batteries, such as Li-sulphur batteries.P / 91817

[0451] In some embodiments, the porous glassy carbon can be used for the preparation of monolithic objects using conventional and advanced powder metallurgical processes. In some embodiments, the monolithic consolidated objects can be used as inert or semi-inert anodes in molten oxide electrolysis and / or molten salt electrolysis processes for metal and alloy production.

[0452] This invention encompasses both the materials described above and the methods for their preparation.

[0453] (C) Consolidation of Glassy Carbon Powders

[0454] Aspects of the current invention relate to the preparation of glassy carbon particles using the disclosed methods. These particles possess specific features, including smooth surfaces, textured surfaces, porous structures, and / or crystalline shapes. Certain aspects of the current invention relates to the consolidation of the glassy carbon particles to obtain consolidated or monolithic glassy carbon objects, with no or minimal voids, cracks and other defects.

[0455] In some embodiments, the consolidation process involves pressing of the glassy carbon particles. In some embodiments, a mixture of glassy carbon particles and a sintering aid is pressed into a green body with specific dimensions in the range 1 mm to 10 m. In some embodiments, the sintering aid is a metal or alloy comprising Fe, Ni, Cr, Mn, Co, Zr, Nb, Ta, Au, Si, Cu, Al, Ti, Mo, W, Ir and Pt. In some embodiments, the sintering aid is an oxide phase or ceramic containing the above mentioned elements. In certain specific embodiments, the pressing is performed at room temperature, typically between 0 and 50°C. In other specific embodiments, the pressing is conducted at elevated temperatures in the range of 50-2500°C, preferably between 100-2500°C, 500-2500°C, 700-2500°C, 900-2500°C, 1100-2500°C, 1300-2500°C, 1500-2500°C, or 1700-2500°C, and more preferably between 1000-2000°C. In certain specific embodiments, the pressing is performed unidirectionally at a pressure in the range of 5-700 MPa. Alternatively, the pressing may be performed isostatically, including methods such as cold pressing and hot pressing. The pressed compact body formed under any of the aforementioned conditions may then be thermally treated at temperatures within the range of 500-2000°C, with specific ranges including 500-2000°C, 500-2000°C, 600-2000°C, 700-2000°C, 800- 2000°C, 900-2000°C, 1000-2000°C, 1200-2000°C, and 1300-2000°C. In some embodiments, the pressing and / or subsequent thermal treatment is carried out in air. In other embodiments, these processes are conducted in an inert atmosphere comprising gases such as Ar, He, or Xe. Additionally, pressing and / or thermal treatment may be performed in a reducing atmosphere containing hydrogen, with the hydrogen concentration ranging from 0.1 to 100.0 vol%, including narrower ranges such as 0.2-90.0 vol%, 0.3-80.0 vol%, 0.4-70.0 vol%, 0.5-60.0 vol%, 0.6-50.0 vol%, 0.7- 40.0 vol%, 0.8-30.0 vol%, 0.9-20.0 vol%, 1.0-10.0 vol%, and 1.1-5.0 vol%.

[0456] While it is preferred that the pressing and / or subsequent thermal treatment be conducted using the glassy carbon particles produced by the methods specified in this invention, certain aspects of the invention also encompass glassy carbon bodies consolidated by the methods disclosed herein, utilising any type of glassy carbon particles, including glassy carbon particles prepared by alternative methods.

[0457] In some specific embodiments, the pressing and / or subsequent thermal treatment is conducted using glassy carbon particles in combination with the sintering aid that supports the consolidation of the glassy carbon body. The amount of sintering aid used ranges from 0.1 to 90 wt%, with specific ranges including 0.1 to 80 wt%, 0.1 to 70 wt%, 0.1 to 60 wt%, 0.1 to 50 wt%, 0.1 to 40 wt%, 0.1 to 30 wt%, and 5 to 30 wt%.

[0458] In some specific embodiments, the glassy carbon particles used to prepare the consolidated glassy carbon body have both smooth and textured surfaces, and the consolidated body contains the sintering aid component. In these embodiments, the textured surfaces of the glassy carbon particles support the consolidation process more effectively than certain other surfaces, such as smooth surfaces. Without being bound by any particular mechanism, the texturedP / 91817

[0459] surfaces of glassy carbon particles provide better adhesion to the secondary phase (such as the binder or the sintering aid) used in the preparation of the consolidated glassy carbon body, thereby enhancing certain mechanical, physical, and chemical properties of the consolidated body.

[0460] In some specific embodiments, the glassy carbon particles used in the preparation of the consolidated glassy carbon body have porous surfaces or structures containing open circular or semi-circular holes. In these embodiments, the consolidated glassy carbon body contains a sintering aid component, and the porous surfaces or structures of the glassy carbon support the consolidation process to be more effective than certain other surfaces, such as smooth and textured surfaces.

[0461] Without being restricted to any specific microstructure or morphology, Figure 1 illustrates an example of the microstructure or morphology obtained by consolidating glassy carbon particles, preferentially the glassy carbon particles prepared using the methods of this invention. In this figure, (1) represents the glassy carbon particles, and (2) represents the sintering or binding aid material. In some embodiments, (2) may also represent a substrate or a continuous, semi-continuous, or non-continuous network of the sintering aid formed during the pressing and / or sintering steps. Additionally, the glassy carbon particles may be further bound to the substrate through the formation of an interfacial layer or an interlayer between the glassy carbon particles and the substrate. In some embodiments, the interfacial layer or the interlayer comprises a carbide material.

[0462] (D) Glassy Carbon Coating

[0463] Aspects of the invention relate to materials comprising glassy carbon combined with another component. This additional component may be ceramic, polymer, carbon (such as graphite), metal, or metallic alloy, with the glassy carbon forming a continuous coating primarily on the surface of the component. The methods for producing the glassy carbon coating disclosed in this invention offer advantages over certain alternative approaches.

[0464] For example, the current processes for making glassy carbon coatings (such as the method presented in JP2000272987A) are similar to those used for making bulk glassy carbon materials. Both types of these processes typically involve the use of a precursor solution prepared by dissolving a thermosetting resin, such as phenolic resins, furan resins, or epoxy resins in an appropriate solvent such as methanol, dimethyl sulfoxide, N-Methy l-2-py rrol idinone (NMP) or tetrahydrofuran (THF) to create a uniform solution. This solution may include additional components, including catalysts such as 4-toluenesulfony I chloride to control the curing and pyrolysis process. Moreover, additives such as silicon compounds can be used to enhance the properties of the final glassy carbon product, reducing the risk of cracks during the carbonisation process by providing diffusing channels for pyrolysis gases. For coating purpose, the solution is applied on the surface, and then dried to remove the solvent, and cured typically for several hours, such as 3-20 hours, followed by heating in a non-oxidising atmosphere to achieve carbonisation. Such methods are inevitably multi-step, time-consuming, and often result in defective coatings.

[0465] Aspects of the current invention offer advantages over certain other methods. For example, unlike the prior art, this invention employs a thermoplastic polymer as the carbon source. The thermoplastic polymer melts at a specific temperature, allowing the molten polymer to wet the surface of the object to be coated. This can be achieved by simply immersing the object in the molten polymer for a soaking time ranging from 1 second to 1 hour. After soaking, the object is removed from the melt and heated to a sufficiently high temperature to carbonise the polymer. This innovative process eliminates the need for solvents, solvent drying, and curing, resulting in significant environmental, technical and economic benefits. This innovative approach can used to coat various materials, including ceramic materials, metallic materials and carbon materials, such as graphite, with glassy carbon having a thickness of 1 nm to 100 pm.P / 91817

[0466] In some embodiments, the glassy carbon and the component (the substrate) are bonded through an interlayer material. In certain embodiments, the interlayer material is a carbide that contains one or more elements derived from the substrate.

[0467] In some embodiments, the carbide layer exhibits excellent electrical conductivity, ranging from 10 S / m to 107S / m. Without being limited to a specific type of carbide, the material can include transition metal carbides, for instance, refractory carbides such as titanium carbide, tungsten carbide, zirconium carbide, molybdenum carbide, niobium carbide, tantalum carbide, vanadium carbide, hafnium carbide and a high-entropy carbide, with electrical conductivity values in the range of 105to 107S / m. In some embodiments, the refractory carbide exhibits metallic bonding, which contributes to its high electrical conductivity. In other embodiments, the carbide material may include iron carbide. Some aspects of the embodiments mentioned above are illustrated in Figure 2, where (1) represents a solid substrate made of a polymeric material, a ceramic material, a carbon material (such as graphite), or a metallic material such as a metallic alloy.

[0468] In some embodiments, the metal or metallic alloy substrate contains of a transition metal from the group comprising iron (Fe), titanium (Ti), manganese (Mn), zirconium (Zr), vanadium (V), chromium (Cr), copper (Cu), zinc (Zn), cobalt (Co), nickel (Ni), molybdenum (Mo), silver (Ag), tungsten (W), ruthenium (Ru), rhodium (Rh), iridium (Ir), platinum (Pt), gold (Au), hafnium (Hf), tantalum (Ta), yttrium (Y), scandium (Sc) and cadmium (Cd); and (2) is the glassy carbon; and (3) is an interlayer phase containing a metal of the substrate (1).

[0469] In some embodiments, the interlayer phase can be a carbide containing a transition metal element derived from (1). In some embodiments, this carbide interlayer has a thickness of 1 nm to 10 nm. Without being limited to specific performance characteristics, this interlayer carbide phase can enhance the integrity of the coating-substrate interface and improve certain mechanical and / or physical properties of the coated material, such as mechanical properties and / or the electrical and thermal conductivity.

[0470] The glassy carbon coated material (presented in Figure 2) can be beneficial for various applications. In some applications, the glassy carbon coated object is exposed to a corrosive, oxidising and / or abrasive environment, and the glassy carbon coating protects the substrate against the environment. These features can be attractive for various applications including the electrodes in electrochemical processes such as molten oxide or molten salt electrolysis, where the glassy carbon protect the substrate from corrosion, erosion and oxidation. Other applications include protecting materials used in nuclear reactors from nuclear irradiation and high-temperature oxidising gases.

[0471] Specific aspects of the present invention relate to glassy carbon-coated objects, wherein the coating comprises a layer of glassy carbon applied to a substrate. The substrate may consist of various materials, including ceramics, polymeric materials, carbon materials such as graphite, metals, or metallic alloys. In some embodiments, the glassy carbon coating has a thickness ranging from 1 nm to 1 mm. The coating thickness can be tailored to specific applications, offering properties such as mechanical protection, thermal / electrical conductivity, or surface modification. In certain embodiments, the glassy carbon-coated object may take on various sizes and shapes, with dimensions ranging from 1 mm to 10 m, enabling their use in a wide array of applications. The objects may include, but are not limited to, wires, rods, sheets, foils, spheres, cylindrical or rectangular blocks, or objects with complex geometrical structures. Specific aspects of the invention also relate to methods for preparing glassy carbon-coated objects.

[0472] In some embodiments, the glassy carbon materials, and the carbon coated metals and alloys disclosed in this invention can be used for the nucleation and growth of diamond using high pressure high temperature method at pressures in the rage 3-100 GPa and temperatures 1000-3000 °C.P / 91817

[0473] FURTHER SUMMARY OF THE INVENTION

[0474] (A) Glassy Carbon Materials

[0475] Some aspects of the current invention relate to the carbonisation of thermoplastic plastics, such as polyethylene terephthalate (PET) to form glassy carbon particles, with greater metal-ion storage performance than certain other materials. The resulting glassy carbon particles may be referred to as plastic-derived carbon (PDC) materials in this invention. The PDC material can be used, for instance, as the anode of Na-ion batteries. The effective conversion of plastics, particularly waste plastics, into advanced functional materials with enhanced metal-ion storage properties, along with enhanced thermal and chemical stability, comparing to certain other alternatives, provides a sustainable approach to energy storage technologies.

[0476] Certain aspects of the invention relate to techniques for increasing the degree of carbonisation of plastics and enhancing the properties of PDCs, offering economic advantages. Efficiently utilising waste plastics as a carbon precursor for energy storage also provides environmental benefits by mitigating the adverse environmental impacts of such waste.

[0477] Some specific embodiments of the invention relate to glassy carbon particles ranging in size from 10 nm to 300 pm, characterized by sharp edges, trihedral corners and smooth surfaces. In some embodiments, the glassy carbon particles have regular or semi-regular shapes. In some embodiments, the glassy carbon particles contains rhombuslike structures. These particles may have diagonals in the range 10 nm to 300 pm, such as 888 nm and 546 nm. These particles may have acute and obtuse angles of around 31.59° and 116.83°, respectively. In some embodiments, the glassy carbon particles have randomly oriented crystalline planes, confirming the semi-crystalline nature of the glassy carbon, with nano-crystallites with dimensions of around 1-3 nm, such as 2.09 nm, 2.47 nm and 2.75 nm. The invention further encompasses methods for producing these glassy carbon particles.

[0478] Some specific embodiments of the invention relate to glassy carbon particles with volcanic-like textured surfaces, with the surface fraction of the volcanic-like textured areas being less than 50%, 40%, 30%, 20%, or 10%. The invention further encompasses methods for producing these glassy carbon particles.

[0479] Some specific embodiments of the invention relate to glassy carbon particles exhibiting a Type IV N2adsorptiondesorption isotherm with H4 hysteresis, indicative of slit-shaped mesopores or cylindrical pores and capillary condensation within the porosity. Some embodiments feature glassy carbon particles with a BET specific surface area ranging from 400 to 700 m2 / g (e.g., 515.2 m2 / g) and an average pore diameter of 1-10 nm (e.g., 1.97 nm). The invention further encompasses methods for producing these glassy carbon particles.

[0480] Some specific embodiments of the invention relate to curved and sliced glassy carbon particles measuring 1 to 550 pm, typically featuring both smooth and textured surfaces.

[0481] Some specific embodiments of the invention relates to glassy carbon particles with smooth and textured surfaces, where the textured surfaces have porosity characterized by slit-like cuts with rectangular areas, in the range 1- 10 pm x 0.1- 1 pm, such as 8.2 x 0.4 pm and 4.1 x 0.3 pm. The invention further encompasses methods for producing these glassy carbon particles. For example, in some embodiments, the slit-like cuts with rectangular areas on the textured glassy carbon surface is created by the carbonisation of plastics, such as PET, in the presence of an inorganic salt or mixture of two or more inorganic salts. In some embodiments, the salt mixture comprises NaCI and KCI, and the dimensions of the surface slit-like cuts can be influenced by varying the carbonisation temperature in the presence of the salt mixture. For instance, when a NaCI-KCI salt mixture is used, the dimensions of the slit-like cuts are approximately 1-10 pm x 0.1-1 pm at 700 °C, 20-30 pm x 3-7 pm at 800 °C (e.g., about 28 x 5 pm or 25 x 4 pm),P / 91817

[0482] and 15-22 m x 3-7 pm at 900 °C. In these embodiments, the areas of surface slit-like cuts are larger at specific processing temperatures (for example at 800 °C), and this promotes the metal-ion storage performances of the glassy carbon.

[0483] In some embodiments, the glassy carbon materials comprise or consist of carbon and oxygen. The following embodiments are provided by way of example and not limitation. The surface of the glassy carbon formed by the carbonisation of PET at 800 °C in air in the presence of KCI-NaCI salt mixture, characterised by XPS, can contain only carbon (C, 88.09 wt%) and oxygen (O, 11.91 wt%). The BET specific surface area of this sample can be 534.5 m2 / g, with an average pore dimeter of 2.29 nm. In some embodiments, the carbonisation of thermoplastic polymers in the presence of inorganic salts increases the porosity of the sample. For instance, the pore diameter in the glassy carbon prepared in the presence of NaCI-KCI in comparison with that of produced without the presence of salt can be larger. Without being restricted by mechanism, this observation can be related to the penetration of the molten salt into the plastic-derived carbon during the thermal carbonisation of the polymer.

[0484] In some specific embodiments of the invention, PET materials are thermally treated in the presence of an inorganic salt mixture with an appropriate melting temperature and thermal stability. For example, a mixture of NaCI (7.5 g) and KCI (7.5 g) provides a melting point of 658°C. Heating PET with this salt mixture to an appropriate temperature (such as 800 °C) in air with a short dwell time at the maximum temperature (for example, only 10 min) leads to the formation of glassy carbon particles with smooth and textured surfaces. In these embodiments, the glassy carbon obtained demonstrates a suitable Na-ion storage capacity, for example, 144.9 mAh / g after 120 cycles in a coin cell using Na as the counter / reference electrode and 1 M NaCFaSOa in diglyme as the electrolyte. In some embodiments, ball milling of the glassy carbon particles enhances the Na-ion storage capacity; for example, increasing it to 217.8 mAh / g after 100 cycles at a current density of 100 mA / g, resulting in an energy density of 218 Wh / kg.

[0485] Some specific embodiments relate to a glass carbon product comprising particles with sizes ranging from 1 to 500 pm that feature a textured surface. This surface texture is characterised by the presence of cuts with dimensions ranging from 500 nm to 20 pm and thicknesses between 100 nm and 5 pm. Such a microstructure offers significant advantages for various applications, including metal-ion storage and composite material development. For applications as electrodes of metal-ion batteries, the textured surface facilitates enhanced penetration of electrolytes, thereby improving the electrochemical performance of the electrode compared to certain other materials. Without being restricted to a specific mechanism, the enhanced electrolyte penetration into the glassy carbon reduces ionic and electronic transport distances across the electrode, which are critical for energy storage systems such as batteries. For applications as fillers in composites, the penetration of other materials, such as polymers and metals, into the textured surface increases the integrity of the two phases, thereby enhancing certain physical and / or mechanical properties of the composite material. The incorporation of these textured glassy carbon particles into composite materials contributes to improved mechanical, thermal, and electrical properties. The structural features enable stronger interfacial bonding within the composite, leading to greater durability, thermal stability, and overall performance, comparing to certain other composite materials. These benefits make textured glassy carbon an attractive material for advanced technological applications.

[0486] One such application is molten oxide and molten salt electrolysis processes, in which the use of graphite anodes is challenging due to their consumable nature. Graphite anodes degrade primarily through oxidation reactions, leading to the formation of carbon oxides and erosion. The degradation is influenced by the high temperatures and the presence of reactive oxygen species, which accelerate the oxidation process and chemical attack. Therefore, the lifespan ofP / 91817

[0487] graphite anodes in high-temperature electrolysis (above 500°C to 2000°C) is relatively short, typically lasting only an hour to a few days, depending on the specific conditions. The glassy carbon particles, produced based on the methods of this invention, including the glassy carbon particles containing textured surfaces exhibit high resistance against thermal oxidation and chemical corrosion and erosion comparing to certain other carbon materials, including graphite, making them an attractive alternative material for such applications.

[0488] In certain embodiments, waste PET is converted into glassy carbon particles that exhibit significant resistance to chemical and electrochemical oxidation. Under an air atmosphere, at least 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, or 50% of the glassy carbon particles remain stable when heated to 1000 °C at a rate of 20°C / min. In some embodiments, at least 80%, 85%, 90%, 95%, or 98% of the glass remains stable after heating to 1000 °C in the presence of an inorganic salt or salt mixture with an evaporation temperature exceeding 1000 °C, such as NaCI. In some other embodiments, at least 50%, 60%, 70%, 80%, 85%, 90%, 95%, or 98% of the glassy carbon remains stable when exposed to molten oxides at temperatures greater than 1500 °C but less than 2000 °C. This stability is maintained under oxidation polarisation for durations of at least 1 hour, 5 hours, 10 hours, 20 hours, 1 day, 5 days, 10 days, 20 days, 1 month, 2 months, 3 months, 4 months, 5 months, 6 months, 7 months, 8 months, 9 months, 10 months, 11 months, or up to I year.

[0489] Aspects of this invention relates to crystalline-shaped glassy carbon particles, and the method of making them. In some embodiments, the glassy carbon particles have amorphous or semi-crystalline structure. In some embodiments, the glassy carbon material comprises faceted particles with dimensions ranging from 10 to 500 pm. In some embodiments, these particles may have angles of 90° or 90° ± 2°. In some embodiments, the particles may be plate-like with parallel sides, having sizes ranging from 100 to 500 pm, for example, 120, 150, 200, 225, and 300 pm, and a thickness of less than 1 to 100 pm, such as 5, 10, 20, 30, 41, and 50 pm. In some embodiments, the glassy carbon material comprises particles with perfect or semi-perfect rectangular faces. In certain embodiments, these crystalline-shaped glassy carbon particles exhibit X-ray diffraction (XRD) patterns characterised by a decrease in intensity between two-theta values of approximately 5-10°, along with two broad diffraction peaks at two-theta ranges of 15-32° and 37-49°. In some embodiments, the XRD pattern of the crystalline-shaped glassy carbon particles may also include peaks corresponding to an organic crystalline compound. In some specific embodiments, the organic compound comprises of CsHeC . In some embodiments, the CsHeC^ can be terephthalic acid, exhibiting an anorthic (triclinic) crystalline structure. In some specific embodiments, the peaks related to the CsHeC^ phase can be found at two-theta values of around 17.244°, 25.087°, 27.752°, 35.152°, 42.485°, 54.006°, and 60.568°, corresponding to the (110), (0-11), (200), (220), (300), (-140), and (141) planes of terephthalic acid.

[0490] In some embodiments of the current invention, the crystalline-shaped glassy carbon particles are formed by the thermal treatment of a polymer in an atmosphere containing hydrogen (H2). In some embodiments, the polymer is a thermoplastic polymer, and in some other embodiments, the polymer is a plastic material, such as polyethylene terephthalate (PET). In some embodiments, the thermal treatment is conducted at temperatures between 500-2000°C, and preferentially between 550-1950°C, 600-1900°C, 600-1850°C, 600-1800°C, 600-1700°C, 600-1600°C and 600-1500°C, 600-1400°C, 600-1500°C, 600-1400°C, 600-1300°C, 600-1200°C, 600-1100°C and 600-1000°C. In some embodiments, the heating atmosphere contains H2in a range of 0.1-100 vol%, preferably 0.1-90%, 0.1-80%, 0.1— 70%, 0.1-60%, 0.1-50%, 0.1-40%, 0.1-30%, 0.1-20%, 0.1-10%, 0.1-5%, or 1-4 vol%.

[0491] In some embodiments, the atmosphere, in addition to hydrogen, includes a non-oxidising gas such as N2, Ar, or He. In specific embodiments, the crystalline-shaped glassy carbon particles are formed by the thermal treatment ofP / 91817

[0492] polyethylene terephthalate in an atmosphere containing hydrogen at temperatures ranging from 500 to 1500°C. In specific embodiments, PET can be sourced from waste PET objects, such as discarded liquid bottles. In other embodiments, the starting PET material can consist of commercially available virgin PET granulates commonly used in the industrial production of PET objects. In certain embodiments of the invention, crystalline-shaped glassy carbon particles are formed by the thermal treatment of the waste PET in an atmosphere of Ar containing H2at temperatures ranging from 500°C to 2000°C. In some embodiments, the utilisation of waste PET offers advantages over virgin PET newly manufactured from raw petrochemical feedstocks. Without being bound by reasoning, waste PET is advantageous over virgin PET due to its uniform thickness (for example, between 0.1 - 0.3 mm for disposable water bottles, and 0.5 - 2 mm for reusable water bottles), which can be thinner than virgin PET particles, which typically range from 2 mm to 5 mm. Moreover, waste PET may be melted easier than the virgin PET, due to relative degradation of its molecular structure. These characteristics support more uniform melting of the waste PET and more consistent carbonisation of the melt. In particles with larger diameters, the surface may melt and undergo carbonisation while the core reacts later, owing to the limited thermal conductivity of PET.

[0493] In some embodiments, the surface and bulk of the glassy carbon particles comprise of oxygen and carbon. In some embodiments, the surface and bulk of the glassy carbon particles consist solely of oxygen and carbon. The surface chemical composition of the glassy carbon particles can be measured by X-ray photoelectron spectroscopy (XPS) probing the outermost layer less than 10 nanometres deep, while the bulk chemical composition can be measured by energy-dispersive X-ray spectroscopy (EDS), probing depths ranging from 1 to several micrometres. In some specific embodiments, the XPS spectra of the glassy carbon particles consist of carbon and oxygen, with the carbon content ranging from 80.0 to 95.0 at% or 82.0 to 90.0 at%, and the oxygen content ranging from 5.0 to 20.0 at% or 10.0 to 18.0 at%. In some specific embodiments, the EDS analysis of the glassy carbon particles consists solely of carbon and oxygen. In some specific embodiments, the EDS analysis of the glassy carbon particles consists solely of carbon and oxygen, with the oxygen content being less than 7 mass%, less than 6 mass%, less than 5 mass%, less than 4 mass%, or less than 3 mass%. In some specific embodiments, the EDS analysis of the glassy carbon particles consists solely of carbon and oxygen, with the carbon content being greater than 92 mass%, greater than 93 mass%, greater than 94 mass%, greater than 95 mass%, greater than 96 mass%, greater than 97 mass%, or greater than 98 mass%.

[0494] In certain embodiments of the invention, crystalline-shaped glassy carbon particles are formed by thermally treating waste PET in an atmosphere of Ar containing 4 vol% H2at 1000 °C for a short dwell time of up to 10 minutes at the maximum temperature. The glassy carbon particles consist solely of carbon (C) and oxygen (O), with the bulk chemical composition determined to be 93.38 mass% (94.04 at%) C and 6.62 mass% (5.06 at%) O. In some embodiments, the crystalline-shaped glassy particles exhibit a bulk chemical composition of 97.80 mass% (98.34 at%) C and 2.20 mass% (1.66 at%) O. In certain embodiments, extending the thermal process at the maximum temperature, for example, to durations of 30, 60, 90, or 120 minutes, under a reducing atmosphere can decrease the oxygen content in the crystalline-shaped glassy carbon particles. Additionally, in certain embodiments, increasing the treatment temperature beyond 1000 °C can further reduce the oxygen content in crystalline-shaped glass particles.

[0495] Some specific embodiments of the invention relate to a product comprising glassy carbon with a portion of porous glassy carbon particles featuring circular or semi-circular holes with diameters ranging from 20 to 200 nm, including examples such as 30 nm, 80 nm, 140 nm, 160 nm, and 170 nm. These circular holes may merge to form larger pores with diameters of up to 350 nm. In certain embodiments, the product also comprises calcium carbonate (CaCOa) crystals, primarily exhibiting a rod-like morphology with a length-to-diameter ratio ranging from 30 to1.5. ExamplesP / 91817

[0496] include ratios such as 28, 26, 22, 21 , 20, 18, 16, 14, 12, 10, 8, 7, 6, 5, 4, 3, 2, and 1.5. In some embodiments, the rodlike CaCOa crystals are interconnected, forming structures with hook-like shapes. In some embodiments, the CaCOa rod-like crystals have a calcite structure.

[0497] Some embodiments of the invention relate to porous glassy carbon particles with little (less than 5 wt%) to no presence of a second phase, such as CaCOa. In certain embodiments, a combination of porous glassy carbon particles and CaCOa crystals is initially formed, and the CaCOa content is then partially or completely removed to produce porous glassy carbon particles as the sole or primary component. The mass fraction of the porous glassy carbon particles ranges from 60-100%, 70-100%, 80-100%, 90-100%, 95-100%, or 97-100%. In some embodiments, the removal of CaCOa crystals is achieved by washing the combination of porous glassy carbon particles and CaCOa crystals with an acidic solution, with pH value in the range 1.0-6.5, preferentially 1.0 to 3.0, followed by filtration and drying.

[0498] In certain embodiments of the present invention, a thermoplastic polymer is thermally treated at temperatures in the range of 300°C to 2000°C to form a glassy carbon phase and a gas phase. In some embodiments, the gas phase is subsequently cooled to a desirable temperature, for instance in the range 25°C to 300°C, causing the deposition of a solid phase comprising monomers of the said polymer. In particular embodiments, the polymer comprises PET, and the monomer comprises terephthalic acid.

[0499] In some embodiments, the proportion of the glassy carbon phase relative to the polymer feedstock is in the range of 10-60 mass%, 12-48 mass%, or 13-45 mass%. In further embodiments, the proportion of the monomer obtained is in the range of 10-40 mass%, 12-38 mass%, or 13-35 mass% of the feedstock. In specific embodiments, the addition of inorganic salts to the polymer feedstock, prior or during the heating process, enhances the proportion of the glassy carbon product and / or the monomer product by a maximum of 1%, 5%, 10%, 15%, 20%, 25%, or 30%, further optimizing the yield of the desired phases in the process.

[0500] In some embodiments, the mixture of porous glassy carbon and CaCOa rod-like crystals, or the porous glassy carbon with minimal (less than 5 wt%) to no calcite presence, are used to fabricate consolidated or monolithic materials. In some embodiments, the monolithic material is fabricated using the said materials in combination with a second phase comprising a metal, polymer, or ceramic material. In these embodiments, the porosity of the porous glassy carbon and the rod-like features of the CaCOa crystals enhance specific physical and / or mechanical properties of the resulting composite, comparing to certain other composite materials.

[0501] In some embodiments of this invention, the second phase involved in the resulting monolithic material is a polymer, like polypropylene (PP), polyethylene (PE), polyvinyl chloride (PVC), polyethylene terephthalate (PET), rubbers or biodegradable polymers such as polylactic acid (PLA) or polybutylene succinate (PBS). In some embodiments, the prepared polymers enhanced with hard and light glassy carbon particles can be utilised in a variety of applications across multiple industries due to their improved mechanical, thermal, and physical properties. These composites can be used to manufacture lightweight yet strong automotive components, such as dashboards, bumpers, and other parts that require high impact resistance and durability, also improving fuel efficiency and reducing emissions. Certain monolithic materials (composites) prepared by the said approach can be used to manufacture lightweight structures for the aerospace sector benefiting from the high strength-to-weight ratio of the polymer composites filled with glassy carbon particles, which enhance fracture toughness and impact strength of the components. The glassy carbon fillers may improve the thermal stability and resistance of polymers, making them suitable for components exposed to extreme temperatures. Certain such monolithic materials (composites) can be used to manufacture biomedical materials such as scaffolds that mimic the mechanical properties of bone, promoting cell growth and integration intoP / 91817

[0502] body tissues, and implants. Certain such monolithic materials (composites) can be used to manufacture rigid and durable packaging materials, with enhanced barrier properties against moisture and gases. Other possible applications include lightweight, durable, and weather-resistant building materials such as panels, pipes, and insulation.

[0503] In some embodiments, the glassy carbon can be used in additive manufacturing to produce parts with customized mechanical, thermal, electrical and thermal properties for advanced electronic applications. These composites can be used to manufacture sports and leisure equipment, such as helmets, rackets, and protective gear. These composites can be used to manufacture biodegradable and sustainable materials for various applications, reducing environmental impact. Polymers with addition of glassy carbon materials can be used for electromagnetic interference (EMI) shielding applications. This combination leverages the lightweight, flexible, and corrosion-resistant properties of polymers with the enhanced electrical conductivity and shielding effectiveness of the carbon material. Other possible applications include tires, seals, gaskets, household items, plastic films, pipes, profiles, flooring materials, and containers.

[0504] In some embodiments of this invention, the second phase in the resulting monolithic material (composite) is a ceramic material. In these embodiments, the porous glassy carbon particles and the rod-like and hook-like CaCOa crystals serve as fillers, enhancing one or more properties of the ceramic material, including the compressive strength, durability, and resistance of the ceramic against crack formation and propagation. In certain embodiments, the glassy carbon particles and the CaCOa crystals can be used as additives in the manufacturing of ceramic composites, including concrete and asphalt, as well as alumina-, zirconia-, silica-, silicon carbide-, boron carbide-, silicon nitride-, aluminium nitride-, titanium diboride-, mullite-, and cordierite-based composites. In some embodiments of this invention, the second phase in the resulting composite is a high entropy oxide (HEO) ceramic material.

[0505] In some embodiments of this invention, the second phase in the resulting composite can be a metal, metallic alloy, or intermetallic alloy. The metal include light metals such as aluminium (Al), magnesium (Mg), and titanium (Ti); transition metals such as iron (Fe), copper (Cu), nickel (Ni), cobalt (Co), and zinc (Zn); refractory metals such as tungsten (W), molybdenum (Mo), tantalum (Ta), and niobium (Nb); or precious metals such as gold (Au), silver (Ag), platinum (Pt), and palladium (Pd). In certain embodiments, the metallic alloy may include ferrous alloys such as stainless steel, nickel-based superalloys, cobalt-based superalloys, and aluminium alloys. Other metals such as beryllium (Be), lithium (Li), and lead (Pb) may also be used. In some embodiments of the invention, the second phase is a high entropy alloy (HEA). The appropriate metal or alloy can be selected based on various factors, including mechanical properties, thermal and electrical properties, working temperature limits, radiation shielding capabilities, chemical or electrochemical corrosion resistance, surface properties such as wear, scratch, and erosion resistance, hardness, density, cost, availability, and abundance.

[0506] In some embodiments, the resulting composite may contain varying proportions of glassy carbon particles or a mixture of glassy carbon particles and calcite, ranging from 1-99 wt%. Examples include 1-95 wt%, 1-90 wt%, 1-85 wt%, 1-80 wt%, 1-75 wt%, 1-70 wt%, 1-65 wt%, 1-60 wt%, 1-55 wt%, 1-50 wt%, 1-45 wt%, 1-40 wt%, 1-35 wt%, 1-30 wt%, 1-25 wt%, 1-20 wt%, 1-15 wt%, 1-10 wt%, or 1-5 wt%. Alternatively, their proportion in the composite may range from 10-90 wt%, 20-90 wt%, 30-90 wt%, 40-90 wt%, 50-90 wt%, or 60-90 wt%.

[0507] In some embodiments, the resulting composite may be utilised in various applications, such as the production of lightweight, high-performance components for the aerospace and automotive industries. In these applications, the glassy carbon particles or the mixture of glassy carbon particles and rod-like or hook-like CaCOa crystals serve as reinforcements, enhancing the mechanical properties of the metal or alloy, including specific strength, radiation resistance, corrosion resistance, and wear resistance.P / 91817

[0508] In certain embodiments, the composite material is configured for use in radiation protection applications. These embodiments may incorporate a combination of heavy metals, such as lead, and glassy carbon particles. The incorporation of glassy carbon particles is designed to minimize the required quantity of heavy metals, thereby reducing associated toxicological risks.

[0509] In some embodiments of this invention, the second phase involved in the resulting composite can be a ceramic, a polymer, a metal or an alloy, and resulting composite can be used in various applications, including structural and / or functional components with enhanced physical properties, mechanical properties, surface properties, chemical properties or electrochemical properties. One application of the composite material is inert anodes used for high-temperature electrolysis. In these embodiments, the composite material, in addition to the glassy carbon, contains a metallic material or a ceramic material comprising chromium, iron, silicon, nickel, cobalt, titanium, molybdenum, tungsten, niobium, magnesium, calcium, sodium, potassium, copper and zinc.

[0510] In some embodiments of this invention, the glassy carbon serves as a coating for a second phase, which may be a ceramic, a polymer, a metal or an alloy. In these embodiments, the glassy carbon coating may enhance one or more properties of the second phase, such as increasing its corrosion resistance, hardness, electrochemical oxidation resistance, or electromagnetic shielding performance. In some embodiments, the resulting glassy carbon coated material can be used in a variety of applications, where the glassy carbon serves as a passive or protective layer that enhances the substrate's resistance to corrosion, wear, and / or electrochemical oxidation. In some embodiments, the protective glassy carbon layer effectively shields the underlying material from environmental factors, thereby extending its lifespan and maintaining its structural integrity. The glassy carbon layer can improve the chemical, mechanical, electrical, and / or thermal stability of the substrate. Additionally, the glassy carbon layer can improve the overall durability and performance of the substrate in harsh or chemically reactive environments.

[0511] In certain embodiments, the second phase comprises of nuclear waste, wherein the glassy carbon coating is applied to serve as a barrier for encapsulation to contain radioactive gases and radiation, such as tritium, thereby enhancing the containment, isolation, and management of radioactive waste and facilitating its cleanup.

[0512] Examples of applications for glassy carbon-coated materials include biomedical applications, such as scaffolds for tissue engineering, due to their biocompatibility and stability; medical devices, including heart valves, prosthetic devices, and biomaterials for neural engineering and acupuncture needles; electrochemical sensors for molecular detection, such as the detection of fentanyl citrate and nitrite; energy and environmental applications, such as energy storage systems; water treatment, for example, as adsorbents in water treatment systems; precision moulding, particularly in high-temperature applications; and the encapsulation of nuclear waste, where the chemical stability of glassy carbon coatings makes them suitable for this purpose. Additionally, the glassy carbon-coated materials can be used in high-temperature manufacturing, electrochemical applications (including the fabrication of sensors and electrodes), electrochemiluminescent platforms, aerospace applications (due to their resistance to harsh environments, including high temperatures and ionizing radiation), and antistatic packaging. Glassy carbon-coated materials also serve as protective coatings, offering protection against corrosion and wear in various industrial applications.

[0513] In some embodiments, the glassy carbon coating disclosed in this invention can be used for the production of dry cask storage systems, or as protective layers on the surface of graphite cores in molten salt breeder nuclear reactors. Without being restricted to a specific mechanism, this performance is primarily attributed to the desirable properties of the glassy carbon layer, including its excellent thermal resistance, high impermeability to molten salts and fission product gases, and superior mechanical strength. In certain embodiments, the glassy carbon-coated materials canP / 91817

[0514] replace conventional materials used in nuclear storage systems, such as copper, stainless steel, and titanium alloys. The glassy carbon layer may also function as a diffusion barrier against fission products and protect substrates under nuclear and ionic radiation, including exposure to xenon, indium, strontium, cadmium, and selenium.

[0515] In some embodiments, the glassy carbon coating disclosed in this invention can be applied to electrodes used in molten oxide or molten salt electrolysis. In some embodiments, the glassy carbon coating can be used to coat electrodes and containers utilised in acidic or alkaline water-splitting reactions. In these embodiments, the electrodes coated with glassy carbon can be made of a metal, a metallic alloy, an intermetallic alloy, a high-entropy alloy, a ceramic material, or a high-entropy oxide material. In some embodiments, the coated electrodes can also be carbon-based electrode, such as graphite electrodes.

[0516] (B) Some Preferred Methods of Making Glassy Carbon

[0517] Glassy carbon particles and objects: Certain embodiments of the present invention are illustrated in Figure 3. In this figure, (1) represents a polymer, preferably a thermoplastic polymer, or a mixture of various polymers comprising at least one thermoplastic polymer, served as the feedstock for the preparation of the glassy carbon. The polymer of the feedstock may consist of waste or virgin plastic species. In some embodiments, the polymer may comprises of waste PET. (2) is an optional additive to the feedstock, comprising an inorganic salt or a mixture of two or more inorganic salts. These salts perform one or more functions during the thermal processing of the feedstock, such as texturing the glassy carbon product's surfaces, creating porosity within the glassy carbon particles, and forming additional phases like calcite. The salts may also provide protective effects against severe oxidation of the glassy carbon in oxidising environments. (3) is an optional additive to the feedstock, comprising a ceramic, a metal, or an alloy powder, preferably with particle sizes ranging from 1 nm to 10 pm. The function of this powder is to facilitate the formation of glassy carbon- encapsulated particles. Additionally, this powder can promote the formation of crystalline graphitic domains within the glassy carbon material, such as enhancing the crystalline domain size from the range of 0.5-5.0 nm to 1.0-100.0 nm. A mixture comprising components (1), (2), and (3) is prepared and loaded into a container (5), which can be made of ceramic, metal, or carbon. The container containing the feedstock (6) is placed into a tube furnace (6A) and directed to the heating zone (7). A gas flow (8) is introduced into the tube, which may include inert gases such as argon (Ar) or helium (He), nitrogen, oxygen, or a reducing gas such as hydrogen (H2). (8) may also represent a natural flow of air. During the process, the mixture container (5) is positioned in the heating zone, and the temperature is increased to a desired value, typically in the range of 300°C-2000°C, with a heating rate ranging from TC / min to 200°C / min, preferentially between 20°C / min and 100°C / min. During this thermal treatment, the thermoplastic polymer of the feedstock melts, facilitating the removal of the gas phase from the melt, which leads to carbonisation. Additionally, at least one portion of inorganic salt included in the feedstock may melt during the thermal process. The gas phase is then cooled to temperatures below 350°C, typically between 100°C and 350°C, using the cooling device (11), resulting in the deposition of a monomer (12) of the polymer feedstock. The remaining gas phase (9), comprising water and other hydrocarbons, exits the reactor and may undergo further processing.

[0518] The glassy carbon product may include one or more types of materials, such as particles with smooth and textured surfaces, crystalline-shaped glassy carbon particles, porous glassy carbon particles, and porous glassy carbon particles mixed with rod-like calcite crystals. Its characteristics can be tailored by adjusting the reaction parameters. The recovered glassy carbon product, represented by (6), may optionally be washed with water or acidic solutions to remove inorganic salts or to reduce or eliminate other phases, such as calcite.P / 91817

[0519] The glassy carbon particles obtained through the described process may be utilised to fabricate bulk consolidated monolithic glassy carbon objects by employing traditional or advanced powder metallurgical techniques. Such techniques may include, but are not limited to, pressing, sintering, hot isostatic pressing, or cold isostatic pressing methods. The sintering process may be facilitated by incorporating sintering aids or binders, which can include polymeric, ceramic, or metallic materials, depending on the desired final properties of the monolithic carbon object. Alternatively, the glassy carbon particles may be processed using additive manufacturing techniques, such as direct ink writing, binder jetting, or selective laser sintering, to produce complex geometries and custom-designed structures. The resulting bulk consolidated monolithic glassy carbon objects are suitable for a wide range of applications. For instance, they may serve as electrodes in high-temperature electrolysis applications, including but not limited to hydrogen production, molten salt electrolysis, molten oxide electrolysis and other electrochemical processes. Furthermore, these monolithic glassy carbon objects may be employed in structural components, high-temperature application, or as functional materials in various industrial, aerospace, and energy-related technologies, where their exceptional properties are advantageous.

[0520] Glassy Carbon Coating: Specific aspects of the invention relate to the preparation of glassy carbon-coated objects. These aspects can be achieved through the interaction of a thermoplastic polymer, such as a polyester, with an object such as a ceramic, a polymeric material, a carbon material such as graphite, a metallic material or a metallic alloy. In certain embodiments, the polymer is physically brought into contact with the object, and then thermally treated at temperatures exceeding the melting point of the polymer. During this process, the polymer melts and wets the surface of the object, forming a polymer-coated object. By further raising the temperature to a level sufficiently above the melting point of the polymer, but preferably below the melting point or the degradation point or softening point of the object, the polymer undergoes carbonisation, leading to the formation of a glassy carbon coating on the object. In certain embodiments, the thermoplastic polymer comprises of polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polycyclohexylene dimethylene terephthalate (PCT), polyethylene naphthalate (PEN), polytrimethylene terephthalate (PTT), polyetheretherketone (PEEK), polycaprolactone (PCL), polylactic acid (PLA), polyhydroxyalkanoates (PHA), and isotactic polypropylene terephthalate (I PT).

[0521] In some embodiments, the first step of the carbon coating process disclosed in this invention involves preparing a bath of molten polymer. The temperature of the bath is maintained above the melting point of the polymer but below its decomposition temperature. The bath temperature can range from 55°C to 600°C, and more specially, 240°C to 350°C (for PET), 220°C to 370°C for (PBT), 280°C to 375°C (for PCT), 260°C to 400°C (for PEN), 220°C to 370°C (for PTT), 340°C to 600°C (for PEEK), 55°C to 220°C (for PCL), 170°C to 250°C (for PLA), 140°C to 300°C (for PHA) and 240°C-350°C (for IPT). The bath may include additional additives intended for incorporation into the carbon coating, such as metallic or ceramic particles, or precursors of ceramic or metallic particles.

[0522] In some embodiments, the second step of the carbon coating process disclosed in this invention involves immersing the object to be coated into the molten bath prepared in the first step. The exposure time may range from 1 second to 10 hours, preferably from 10 minutes to 30 minutes. After immersion, the object is extracted from the melt, forming a polymer coating on its surface.

[0523] In some embodiments, the third step of the carbon coating process disclosed in this invention involves the thermal treatment of the polymer-coated object to facilitate the carbonisation of the polymer coating. In certain embodiments, the maximum temperature of the treatment is determined by the physicochemical properties of the object being coated,P / 91817

[0524] which may be a ceramic, a polymer or a metallic material. Typically, the maximum temperature can be less than 2500°C, 2000°C, 1900°C, 1800°C, 1700°C, 1600°C, 1500°C, 1400°C, 1300°C, 1200°C, 1100°C, 1000°C, 900°C, 800°C, 700°C, 600°C, or less than 500°C; and greater than 100°C, 200°C, or 300°C. In certain embodiments, the heating atmosphere comprises air. Alternatively, the heating atmosphere may consist entirely of nitrogen or include nitrogen. In other embodiments, the atmosphere may contain an inert gas such as argon or helium. Additionally, the heating atmosphere may include hydrogen or a mixture of hydrogen with another gas, such as argon, helium, or nitrogen. In some embodiments, the heating process is conducted in the presence of a salt, which may include an alkali or alkaline earth halide.

[0525] In certain embodiments, the second step for forming a glassy carbon coating comprises a dip-coating process, wherein the object is submerged into a molten polymer bath and subsequently withdrawn at a controlled rate to achieve a uniform polymer coating layer. In alternative embodiments, the process involves submerging the object into a liquid suspension containing glassy carbon particles, followed by a controlled withdrawal to produce a uniform glassy carbon coating layer. In further aspects of the invention, the glassy carbon coating may be applied through spray-coating techniques. In this approach, glassy carbon particles are dispersed and deposited onto the surface of the object using a spraying mechanism. This is followed by a thermal treatment step, which carbonises the polymer and adheres the glassy carbon particles to form a durable coating layer.

[0526] The carbon-coated objects produced by the disclosed methods exhibit utility in a variety of applications, including, but not limited to, serving as protective layers in high-temperature environments, corrosive conditions, or any setting requiring enhanced thermal and chemical resistance.

[0527] Aspects and embodiments of this disclosure, which may be combined with other features set out in this disclosure, are set out in the following numbered clauses Ex1 A to Ex16F.

[0528] Ex1A. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, the method comprising the steps of:

[0529] heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor;

[0530] further heating the meltable organic precursor to a predetermined treatment temperature to form a treated organic precursor, the predetermined treatment temperature being at least 200°C in excess of the melting point of the meltable organic precursor;

[0531] optionally maintaining the treated organic precursor at, or above, the predetermined treatment temperature for a predetermined period of time; and

[0532] cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material.

[0533] Ex1B. A method of producing carbon, preferably glassy carbon, material according to example Ex1A, in which the predetermined treatment temperature is in excess of 400°C, for example in excess of 450°C, for example in excess of 500°C, or in excess of 550°C, or in excess of 600°C, preferably in which the predetermined treatment temperature is between 500°C and 1500°C, for example between 550°C and 1200°C, for example between 600°C and 1000°C, for example between 700°C and 900°C, for example between 750°C and 850°C or between 700°C and 800°C.

[0534] Ex1Ci. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor is heated to a maximum predetermined treatment temperature of 3000°C or lower, forP / 91817

[0535] example 2000°C or lower, or 1500°C or lower, preferably in which the maximum predetermined treatment temperature is 1300°C or lower, for example 1200°C or lower, or 1100°C or lower, or 1000°C or lower.

[0536] ExICii. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor is heated to a maximum predetermined treatment temperature of between 500°C and 2000°C.

[0537] ExICiii. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the predetermined period of time that the meltable organic precursor is maintained at, or above, the predetermined treatment temperature is between 0.1 seconds and 48 hours, for example between 1 second and 12 hours, preferably between 30 seconds and 6 hours, for example between 60 seconds and 2 hours, or between 2 minutes and 1 hour, for example between 5 minutes and 45 minutes.

[0538] Ex1 D. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which thermal treatment of the meltable organic precursor, such as one or both of the steps of heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor and further heating the meltable organic precursor to a predetermined treatment temperature, includes the step of heating the meltable organic precursor at a heating rate of between 1°C per minute and 100°C per minute, for example between 2°C per minute and 75°C per minute, for example between 5°C per minute and 50°C per minute.

[0539] Ex1 E. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which thermal treatment of the meltable organic precursor, such as the step of cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material, includes the step of cooling the treated organic precursor at a cooling rate of between 1°C per minute and 100°C per minute, for example between 2°C per minute and 75°C per minute, for example between 5°C per minute and 50°C per minute.

[0540] Ex1F. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the carbon, preferably glassy carbon, material is in the form of carbon, preferably glassy carbon, particles having an average particle size of between 1 micron and 1000 microns, for example between 2 microns and 800 microns, for example between 4 microns and 500 microns, or between 5 microns and 400 microns, or in which the carbon, preferably glassy carbon, material is in the form of a carbon, preferably glassy carbon, coating formed on an object.

[0541] Ex1G. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the carbon, preferably glassy carbon, material comprises graphitic nano-crystallites having maximum dimensions in the range of 0.5 nm to 5 nm, for example 1 nm to 3 nm.

[0542] Ex1 H. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the carbon, preferably glassy carbon, material has a d002 plane spacing, measured for example by XRD, of between 0.35 nm and 0.45 nm, for example between 0.36 nm and 0.44 nm, for example between 0.37 nm and 0.42 nm. Ex11. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the carbon, preferably glassy carbon, material has a Raman ID / IG value of between 0.9-1.3, for example between 1.0 and 1.2.

[0543] Ex1 J. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the method comprises the further step of loading the meltable organic precursor into a crucible.

[0544] Ex1 K. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor comprises, or is entirely formed from, one or more thermoplastic materials, for example in which the meltable organic precursor comprises, or is entirely formed from, one or more thermoplastic materialsP / 91817

[0545] selected from the list consisting of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polycarbonate, and polyethylene terephthalate, for example in which the meltable organic precursor comprises, or is entirely formed from, polyethylene terephthalate.

[0546] Ex1 Ki. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor comprises one or more organic acids, for example, in which the meltable organic precursor comprises one or more of: citric acid, tartaric acid, malic acid, succinic acid, glutaric acid, and malonic acid.

[0547] Ex1 Kii. A method of producing carbon, preferably glassy carbon, material according to example Ex1 Ki, in which the organic acid, or each of the organic acids, has a molecular weight less than 300 grams per mole, more preferably less than 200 grams per mole.

[0548] ExlKiii. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor comprises one or more polyols such as sorbitol.

[0549] Ex1L. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor has a melting point of between 75°C and 300°C, for example between 100°C and 280°C, for example between 200°C and 260°C.

[0550] Ex1M. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which carbonisation yield of the meltable organic precursor is between 25% and 50%, for example between 30% and 45%.

[0551] Ex1 N. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor comprises, or consists of, reclaimed thermoplastic material, for example from treated thermoplastic waste.

[0552] Ex1O. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor is in the form of precursor elements or precursor particles having a minimum dimension of less than 1 mm, for example less than 0.75 mm, for example less than 0.5 mm.

[0553] Ex1 P. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the meltable organic precursor is in the form of precursor elements or precursor particles formed by cutting thermoplastic waste, for example formed by cutting thermoplastic products such as sheets or bottles into precursor elements having length and width dimensions of between 0.5 cm and 3 cm, for example between 0.75 cm and 2 cm, for example about 1 cm, for example in which the precursor elements have a length of between 0.5 cm and 3 cm, a width of between 0.5 cm and 3 cm, and a thickness of less than 1 mm.

[0554] Ex1Q. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the method comprises the further step of milling the carbon, preferably glassy carbon, particles to produce milled carbon, preferably glassy carbon, particles, for example ball milling the carbon, preferably glassy carbon, particles.

[0555] Ex1 R. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which a total thermal treatment time includes a time for increasing the temperature of the meltable organic precursor to the predetermined treatment temperature, a time that the meltable organic precursor is maintained at, or above, the predetermined thermal treatment temperature, and a time for cooling the treated organic precursor from the predetermined treatment temperature, preferably in which the total thermal treatment time and the predetermined treatment temperature are controlled to produce carbon, preferably glassy carbon, material with desired d002 spacings, for example d002 spacings greater than 0.36 nm, preferably greater than 0.37 nm, or 0.38 nm, or 0.39 nm, or 0.40 nm.

[0556] Ex1S. A method of producing carbon, preferably glassy carbon, material according to any preceding example, in which the thermal treatment is conducted under a selected atmosphere, the selected atmosphere being one of an oxidisingP / 91817

[0557] atmosphere, a reducing atmosphere and an inert atmosphere, preferably in which selection of the atmosphere depends on the desired surface area of the carbon, preferably glassy carbon, product.

[0558] Ex1 Si. A method of producing carbon, preferably glassy carbon, material according to example Ex1 S, in which the selected atmosphere is the reducing atmosphere or the inert atmosphere and the meltable organic precursor is heated to a maximum predetermined treatment temperature of between 900°C and 2000°C.

[0559] Ex1T. A method of producing carbon, preferably glassy carbon, material according to any of examples 1A to 1 Si, in which the thermal treatment is conducted in an oxidising atmosphere, and the carbon, preferably glassy carbon, particles have a BET surface area greater than 500 m2 / g, preferably comprising a further step of milling the carbon, preferably glassy carbon, particles to produced milled carbon, preferably glassy carbon, particles having a BET surface area greater than 600 m2 / g.

[0560] Ex1U. A method of producing carbon, preferably glassy carbon, material according to any of examples 1A to 1 Si, in which the thermal treatment is conducted in a reducing atmosphere and the carbon, preferably glassy carbon, particles have a BET surface area less than 50 m2 / g.

[0561] Ex1V. A method of producing carbon, preferably glassy carbon, material according to any of examples 1A to 1 U, in which, after the step of cooling the treated organic precursor to produce the carbon, preferably glassy carbon, material, the method comprises a step of heating the carbon, preferable glassy carbon, material.

[0562] Ex1W. A method of producing carbon, preferably glassy carbon, material according to example 1 V, in which the step of heating the carbon, preferable glassy carbon, material comprises heating the carbon, preferable glassy carbon, material to a temperature greater, for example at least 50, 100 or 200 °C greater, than the predetermined treatment temperature.

[0563] Ex1X. A method of producing carbon, preferably glassy carbon, material according to example 1V or 1 W, in which the step of heating the carbon, preferable glassy carbon, material may comprise heating the carbon, preferable glassy carbon, material to a temperature in the range of 510 °C to 2000 °C.

[0564] Ex1Y. A method of producing carbon, preferably glassy carbon, material according to example 1 V, 1W, or 1X, in which the step of heating the carbon, preferable glassy carbon, material is conducted in an inert or reducing atmosphere.

[0565] Ex2A. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to any preceding example except 1T, in which the carbon, preferably glassy carbon, material is carbon, preferably glassy carbon, particles having low specific surface area, the method comprising the steps of:

[0566] heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor;

[0567] further heating the meltable organic precursor to a predetermined treatment temperature to form a treated organic precursor, the predetermined treatment temperature being at least 200°C in excess of the melting point of the meltable organic precursor;

[0568] optionally maintaining the treated organic precursor at, or above, the predetermined treatment temperature for a predetermined period of time; and

[0569] cooling the treated organic precursor to produce the carbon, preferably glassy carbon, particles, in which the thermal treatment is conducted in a reducing atmosphere and the BET surface area of the resulting carbon, preferably glassy carbon, particles is lower than 50 m2 / g.P / 91817

[0570] Ex2B. A method of producing carbon, preferably glassy carbon, material according to Ex2A, in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is lower than 30 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g.

[0571] Ex2C. A method of producing carbon, preferably glassy carbon, material according to example Ex2A or Ex2B, in which the predetermined treatment temperature is between 400°C and 3000°C, for example between 600°C and 2000°C, for example between 700°C and 1500°C, for example between 800°C and 1200°C, for example between 850°C and 1100°C, for example between 900°C and 1000°C.

[0572] Ex2Ci. A method of producing carbon, preferably glassy carbon, material according to any examples Ex2A to Ex2C, in which the meltable organic precursor is heated to a maximum predetermined treatment temperature of between 500°C and 2000°C.Ex2Cii. A method of producing carbon, preferably glassy carbon, material according to any examples Ex2A to Ex2Ci, in which the meltable organic precursor is heated to a maximum predetermined treatment temperature of between 900°C and 2000°C.

[0573] Ex2D. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2Cii, in which the thermal treatment is conducted in a reducing atmosphere containing hydrogen, for example gaseous hydrogen in the form of H2, for example in which the hydrogen concentration of the reducing atmosphere is between 0.1 vol% and 100 vol%, for example between 1 vol% and 90 vol%, or between 1 vol% and 5 vol%, or between 2.5 vol% and 80 vol%, or between 5 vol% and 70 vol%, or between 7.5 vol% and 60 vol%, or between 10 vol% and 50 vol%, or between 15 vol% and 40 vol%, or between 20 vol% and 30 vol%.

[0574] Ex2E. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2D, in which the thermal treatment is conducted in a reducing atmosphere containing hydrogen and an inert gas, for example hydrogen and one or more inert gas selected from the list consisting of nitrogen, argon, helium, neon, and xenon, particularly preferably wherein the reducing atmosphere contains hydrogen and nitrogen.

[0575] Ex2F. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2E, in which the predetermined period of time that the meltable organic precursor is maintained at, or above, the predetermined treatment temperature is between 0.1 second and 1 month, for example between 1 second and 12 hours, preferably between 30 seconds and 6 hours, for example between 60 seconds and 5 hours, or between 2 minutes and 1 hour, for example between 5 minutes and 45 minutes.

[0576] Ex2G. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2F, in which the thermal treatment is conducted for sufficient time and / or at sufficient temperature for the carbon, preferably glassy carbon, particles have a bulk carbon concentration of greater than 90 mass%, for example between 95 mass % and 99 mass %, for example in which the predetermined treatment temperature is in excess of 1000°C and the bulk carbon concentration is greater than 90 mass%, and / or in which the predetermined treatment time is greater than 10 minutes and the bulk carbon concentration is greater than 90 mass%.

[0577] Ex2H. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2G, in which the thermal treatment is conducted for sufficient time and / or at sufficient temperature for the carbon, preferably glassy carbon, particles have a surface carbon concentration of greater than 80 mass%, for example between 80 mass % and 90 mass %, for example in which the predetermined treatment temperature is in excess of 1000°C and the surface carbon concentration is greater than 80 mass%, and / or in which the predetermined treatment time is greater than 5 minutes and the surface carbon concentration is greater than 80 mass%.P / 91817

[0578] Ex2L A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2H, in which the carbon, preferably glassy carbon, particles have a crystalline-like morphology, for example an angular or cubic morphology, or a morphology having substantially parallel sides, for example a plate-like morphology.

[0579] Ex2J. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2l, in which the carbon, preferably glassy carbon, material has a single-point adsorption total pore volume of between 0.010 and 0.001 cm3 / g.

[0580] Ex2K. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2 J, in which the carbon, preferably glassy carbon, material has adsorption average pore diameter (4V / A by BET) of between 2 nm and 5 nm.

[0581] Ex2L. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex2A to Ex2K, in which the thermal treatment is conducted for a short enough time and / or at low enough temperature for the carbon, preferably glassy carbon, particles have a d002 spacing of between 0.36 nm and 0.45 nm, preferably between 0.37 nm and 0.43 nm, for example in which the predetermined treatment temperature is lower than 1200°C, for example lower than 1000°C, and the d002 spacing of between 0.36 nm and 0.45 nm, and / or in which the predetermined treatment time is lower than 5 hours, for example lower than 1 hour, and the d002 spacing of between 0.36 nm and 0.45 nm.

[0582] Ex3A. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to any of examples Ex1A to Ex1T, in which the carbon, preferably glassy carbon, material is carbon, preferably glassy carbon, particles having high specific surface area, the method comprising the steps of:

[0583] heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor;

[0584] further heating the meltable organic precursor to a predetermined treatment temperature to form a treated organic precursor, the predetermined treatment temperature being at least 200°C in excess of the melting point of the meltable organic precursor;

[0585] optionally maintaining the treated organic precursor at, or above, the predetermined treatment temperature for a predetermined period of time; and

[0586] cooling the treated organic precursor to produce the carbon, preferably glassy carbon, particles, in which the thermal treatment is conducted in an oxidising atmosphere and the BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 400 m2 / g.

[0587] Ex3B. A method of producing carbon, preferably glassy carbon, material according to Ex3A, in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g, for example greater than 550 m2 / g, or greater than 600 m2 / g, for example greater than 650 m2 / g, or greater than 700 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 700 m2 / g, for example between 500 m2 / g and 600 m2 / g.

[0588] Ex3C. A method of producing carbon, preferably glassy carbon, material according to example Ex3A or Ex3B, in which the maximum predetermined treatment temperature is 1500°C or lower, for example in which the predetermined treatment temperature is between 400°C and 1000°C, for example between 500°C and 900°C, for example between 600°C and 800°C, for example between 650°C and 750°C.P / 91817

[0589] Ex3D. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex3A to Ex3C, in which the thermal treatment is conducted in an oxidising atmosphere containing oxygen, for example gaseous oxygen in the form of O2, for example in which the oxygen concentration of the reducing atmosphere is between 0.1 vol% and 100 vol%, for example between 1 vol% and 40 vol%, or between 2.5 vol% and 30 vol%, or between 5 vol% and 25 vol%, or between 7.5 vol% and 22 vol%, preferably in which the oxidising atmosphere is air or oxygen-enriched air.

[0590] Ex3E. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex3A to Ex3D, in which the predetermined period of time that the meltable organic precursor is maintained at, or above, the predetermined treatment temperature is between 0.1 second and 6 hours, for example between 1 second and 2 hours, preferably between 10 seconds and 1 hour, for example between 20 seconds and 30 minutes, or between 30 seconds and 20 minutes, for example between 1 minute and 10 minutes.

[0591] Ex3F. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex3A to Ex3E, in which the carbon, preferably glassy carbon, particles comprise a number of surfaces, optionally in which the number of surfaces is all of the surfaces of the carbon particles, a proportion of the number of surfaces being smooth surfaces and a proportion of the number of surfaces being highly textured surfaces, for example in which between 10% and 70% of the number of surfaces are highly textured surfaces, for example in which between 20% and 60% of the number of surfaces are highly textured surfaces, for example between 30% and 50% of the number of surfaces are highly textured surfaces.

[0592] Ex3G. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex3A to Ex3F, comprising the further step of milling the carbon, preferably glassy carbon, particles to increase the surface area, for example ball milling the carbon, preferably glassy carbon, particles, preferably milling until the BET specific surface area is increased by between 10% and 300%, for example between 20% and 200%, for example between 30% and 100%, preferably in which milled carbon, preferably glassy carbon, particles have a BET surface area greater than 600 m2 / g, for example greater than 700 m2 / g, or greater than 750 m2 / g, for example greater than 800 m2 / g, or greater than 850 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 600 m2 / g and 900 m2 / g, for example between 700 m2 / g and 800 m2 / g.

[0593] Ex4A. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to any preceding example except 1 U, in which the carbon, preferably glassy carbon, material is carbon, preferably glassy carbon, particles having high specific surface area, the method comprising the steps of:

[0594] arranging the meltable organic precursor in contact with at least one inorganic salt having a melting point greater than 300°C;

[0595] controlling temperature of the meltable organic precursor and the at least one inorganic salt to a predetermined treatment temperature in excess of the melting point of the inorganic salt to form a treated precursor;

[0596] optionally maintaining the treated organic precursor and at least one inorganic salt at, or above, the predetermined treatment temperature for a predetermined period of time;

[0597] cooling the treated precursor; and

[0598] washing the at least one inorganic salt from the treated precursor to produce the carbon, preferably glassy carbon, particles, in which BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 400 m2 / g.P / 91817

[0599] Ex4B. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to Ex4A, in which the carbon, preferably glassy carbon, material is carbon, preferably glassy carbon, particles having high specific surface area, the method comprising the steps of:

[0600] combining the meltable organic precursor with at least one inorganic salt to form a precursor mixture, the at least one inorganic salt having a melting point greater than 300°C;

[0601] heating the precursor mixture to a temperature above the melting point of the meltable organic precursor; further heating the precursor mixture to a predetermined treatment temperature in excess of the melting point of the inorganic salt to form a treated precursor;

[0602] optionally maintaining the treated precursor at or above the predetermined treatment temperature for a predetermined period of time;

[0603] cooling the treated precursor; and

[0604] washing the at least one inorganic salt from the treated precursor to produce the carbon, preferably glassy carbon, particles, in which BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 400 m2 / g.

[0605] Ex4C. A method of producing carbon, preferably glassy carbon, material according to Ex4A or Ex4B, in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g, for example greater than 550 m2 / g, or greater than 600 m2 / g, for example greater than 650 m2 / g, or greater than 700 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 700 m2 / g, for example between 500 m2 / g and 600 m2 / g.

[0606] Ex4D. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex4A to Ex4C, in which the at least one inorganic salt is one or more of: an alkali metal halide, an alkaline earth metal halide, an alkali metal nitrate and an alkaline earth metal nitrate,

[0607] for example in which the at least one inorganic salt is at least one salt from the list consisting of calcium chloride (CaCI2), magnesium chloride (MgCI2), strontium chloride (SrCI2), barium chloride (BaCI2), calcium fluoride (CaF2), magnesium fluoride (MgF2), strontium fluoride (SrF2), barium fluoride (BaF2), beryllium chloride (BeCI2), and beryllium fluoride (BeF2), sodium chloride (NaCI), potassium chloride (KCI), lithium chloride (LICI), sodium fluoride (NaF), potassium fluoride (KF), lithium fluoride (LIF), sodium bromide (NaBr), potassium bromide (KBr), lithium bromide (LIBr), sodium iodide (Nal), potassium iodide (KI), lithium iodide (Lil), sodium nitrate (NaNO3), potassium nitrate (KNO3), lithium nitrate (LINO3), rubidium nitrate (RbNO3), cesium nitrate (CsNO3), calcium nitrate (Ca(N03)2), magnesium nitrate (Mg(N03)2), barium nitrate (Ba(N03)2), and strontium nitrate (Sr(N03)2),

[0608] optionally in which the at least one salt does not include a calcium based salt, for example in which the at least one inorganic salt is at least one salt from the list consisting of magnesium chloride (MgCI2), strontium chloride (SrCI2), barium chloride (BaCI2), magnesium fluoride (MgF2), strontium fluoride (SrF2), barium fluoride (BaF2), beryllium chloride (BeCI2), and beryllium fluoride (BeF2), sodium chloride (NaCI), potassium chloride (KCI), lithium chloride (LICI), sodium fluoride (NaF), potassium fluoride (KF), lithium fluoride (LIF), sodium bromide (NaBr), potassium bromide (KBr), lithium bromide (LIBr), sodium iodide (Nal), potassium iodide (KI), lithium iodide (Lil), sodium nitrate (NaNO3), potassium nitrate (KNO3), lithium nitrate (LINO3), rubidium nitrate (RbNO3), cesium nitrate (CsNO3), magnesium nitrate (Mg(N03)2), barium nitrate (Ba(N03)2), and strontium nitrate (Sr(N03)2),

[0609] particularly preferably in which the at least one inorganic salt is at least one salt from the list consisting of magnesium chloride (MgCI2), sodium chloride (NaCI), potassium chloride (KCI), and lithium chloride (LICI).P / 91817

[0610] Ex4E. A method of producing carbon, preferably glassy carbon, material according to Ex4D, in which the at least one inorganic salt is a salt mixture of two or more inorganic salts, preferably in which the composition of the salt mixture is selected to control the melting point of the salt mixture, for example in which the at least one inorganic salt is a salt mixture of NaCI and KCI, for example a eutectic or near-eutectic mixture of NaCI and KCI.

[0611] Ex4F. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex4A to Ex4E, in which the predetermined treatment temperature is at least 100°C in excess of the melting point of the at least one inorganic salt, for example at least 150°C in excess of the melting point of the at least one inorganic salt, or at least 200°C in excess of the melting point of the at least one inorganic salt.

[0612] Ex4G. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex4A to Ex4F, in which the predetermined treatment temperature is no more than 500°C in excess of the melting point of the at least one inorganic salt, for example no more than 400°C in excess of the melting point of the at least one inorganic salt, preferably no more than 300°C in excess of the melting point of the at least one inorganic salt.

[0613] Ex4H. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex4A to Ex4G, in which the predetermined treatment temperature is between 400°C and 1200°C, preferably between 500°C and 1000°C, for example between 600°C and 900°C.

[0614] Ex4L A method of producing carbon, preferably glassy carbon, material according to any of examples Ex4A to Ex4H, comprising the further step of milling the carbon, preferably glassy carbon, particles to increase the surface area, for example ball milling the carbon, preferably glassy carbon, particles, preferably milling until the BET specific surface area is increased by between 10% and 300%, for example between 20% and 200%, for example between 30% and 100%, preferably in which milled carbon, preferably glassy carbon, particles have a BET surface area greater than 600 m2 / g, for example greater than 700 m2 / g, or greater than 750 m2 / g, for example greater than 800 m2 / g, or greater than 850 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 600 m2 / g and 900 m2 / g, for example between 700 m2 / g and 800 m2 / g.

[0615] Ex5A. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to any preceding example, in which the carbon, preferably glassy carbon, material is a particulate carbon, preferably glassy carbon, composite comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix, the method comprising the steps of:

[0616] heating the meltable organic precursor in contact with at least one inorganic salt to a predetermined treatment temperature to form a treated precursor, the at least one inorganic salt containing calcium and having a melting point greater than 300°C;

[0617] optionally maintaining the treated precursor and salt mixture at, or above, the predetermined treatment temperature for a predetermined period of time;

[0618] cooling the treated precursor; and

[0619] washing the at least one inorganic salt from the treated precursor to produce an initial particulate product, the particles of the initial particulate product comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix.

[0620] Ex5B. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to Ex5A, in which the carbon, preferably glassy carbon, material is a particulate carbon, preferably glassy carbon, composite comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix, the method comprising the steps of:P / 91817

[0621] combining the meltable organic precursor with at least one inorganic salt to form a precursor mixture, the at least one inorganic salt comprising calcium and having a melting point greater than 300°C;

[0622] heating the precursor mixture to a temperature above the melting point of the meltable organic precursor; further heating the precursor mixture to a predetermined treatment temperature in excess of the melting point of the inorganic salt to form a treated precursor;

[0623] optionally maintaining the treated precursor at, or above, the predetermined treatment temperature for a predetermined period of time;

[0624] cooling the treated precursor; and

[0625] washing the at least one inorganic salt from the treated precursor to produce an initial particulate product, the particles of the particulate product comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix.

[0626] Ex5C. A method of producing carbon, preferably glassy carbon, material according to Ex5A or Ex5B, in which the at least one inorganic salt comprises a calcium halide salt, for example calcium chloride, preferably in which the at least one inorganic salt is a mixture of a calcium halide salt and at least one other inorganic salt, for example in which the at least one inorganic salt is a mixture of sodium chloride and calcium chloride.

[0627] Ex5D. A method of producing carbon, preferably glassy carbon, material according to any of Ex5A to Ex5C, in which the at least one inorganic salt is a mixture of two or more inorganic salts, preferably in which the composition of the mixture of two or more inorganic salts is selected to control the melting point of the salt mixture, for example in which the at least one inorganic salt is a mixture of NaCI and CaCl2, for example a eutectic or near-eutectic mixture of NaCI and CaCl2, optionally in which the at least one inorganic salt is a CaCl2-NaCI-MgCl2 mixture, or a CaC -NaCI-KCl-MgCl2 mixture, or a CaCI2-NaCI-KCI mixture, or a CaCI2-LiCI-KCI mixture.

[0628] Ex5E. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5D, in which the predetermined treatment temperature is at least 100°C in excess of the melting point of the at least one inorganic salt, for example at least 150°C in excess of the melting point of the at least one inorganic salt, or at least 200°C in excess of the melting point of the at least one inorganic salt.

[0629] Ex5F. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5E, in which the predetermined treatment temperature is no more than 500°C in excess of the melting point of the at least one inorganic salt, for example no more than 400°C in excess of the melting point of the at least one inorganic salt, preferably no more than 300°C in excess of the melting point of the at least one inorganic salt.

[0630] Ex5G. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5F, in which the predetermined treatment temperature is between 400°C and 1200°C, preferably between 500°C and 1000°C, for example between 600°C and 900°C.

[0631] Ex5H. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5G, in which the particulate product comprises particles having an average particle size of between 1 micron and 1000 microns, for example between 2 microns and 800 microns, for example between 4 microns and 500 microns, or between 5 microns and 400 microns.

[0632] Ex5L A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5H, in which the calcium carbonate crystals have a rod-like morphology with a length to diameter ratio of between 30:1 and 1.5:1.

[0633] Ex5J. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5l, in which the calcium carbonate crystals have a rod-like morphology with a diameter of between 20 and 500 nm, forP / 91817

[0634] example between 40 and 400 nm, for example in which the calcium carbonate crystals have a calcite-rhombohedral crystalline structure.

[0635] Ex5K. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5l, in which the calcium carbonate crystals have a rod-like morphology with a length of between 30 nm and 15 micron, for example between 60 nm and 12 micron.

[0636] Ex5L. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5K, in which the calcium carbonate crystals have a crystal size, measured perpendicular to the (104) planes of the crystals, of between 10 nm and 200 nm, for example between 20 nm and 100 nm.

[0637] Ex5M. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5L, in which XRD analysis of the calcium carbonate crystals shows a sharp peak at a two-theta value of 29.399° ±0.2.

[0638] Ex5N. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5M, in which the thermal treatment is conducted in an oxidising atmosphere, for example in air, and the BET surface area of the resulting particulate product is greater than 300 m2 / g, for example greater than 350 m2 / g, or greater than 400 m2 / g, for example greater than 450 m2 / g, or greater than 500 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 350 m2 / g and 600 m2 / g, for example between 400 m2 / g and 550 m2 / g.

[0639] Ex5O. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5M, in which the thermal treatment is conducted in a reducing atmosphere, for example a hydrogen containing atmosphere, and the BET surface area of the resulting carbon, preferably glassy carbon, particles is lower than 50 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g.

[0640] Ex5P. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5O, in which the carbon, preferably glassy carbon, matrix is porous.

[0641] Ex5Q. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex5A to Ex5P, in which the carbon, preferably glassy carbon, matrix comprises holes, for example one or both of blind holes and through-holes, optionally wherein an average diameter of the holes is between 2 nm and 500 nm, or 5 nm and 200 nm, optionally wherein the holes have a substantially circular or semi-circular cross-sectional shape.

[0642] Ex5R. A method of producing carbon, preferably glassy carbon, material according to example Ex5Q, in which, in the initial particulate product, at least some of the calcium carbonate crystals are at least partially located in at least some of the holes of the carbon, preferably glassy carbon, matrix.

[0643] Ex6A. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to any preceding example, in which the carbon, preferably glassy carbon, material is carbon, preferably glassy carbon, particles having high specific surface area, the method comprising the steps of:

[0644] heating the meltable organic precursor in contact with at least one inorganic salt to a predetermined treatment temperature to form a treated precursor, the at least one inorganic salt containing calcium and having a melting point greater than 300°C;

[0645] optionally maintaining the treated precursor and salt mixture at, or above, the predetermined treatment temperature for a predetermined period of time;

[0646] cooling the treated precursor;P / 91817

[0647] washing the at least one organic salt from the treated precursor to produce an initial particulate product, the particles of the particulate product comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix: and

[0648] washing the initial particulate product in an acidic solution to remove at least a portion of the calcium carbonate crystals, in which BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g.

[0649] Ex6B. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to Ex6A, in which the carbon, preferably glassy carbon, material is a particulate carbon, preferably glassy carbon, composite comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix, the method comprising the steps of:

[0650] combining the meltable organic precursor with at least one inorganic salt to form a precursor mixture, the at least one inorganic salt comprising calcium and having a melting point greater than 300°C;

[0651] heating the precursor mixture to a temperature above the melting point of the meltable organic precursor; further heating the precursor mixture to a predetermined treatment temperature in excess of the melting point of the inorganic salt to form a treated precursor;

[0652] optionally maintaining the treated precursor mixture at, or above, the predetermined treatment temperature for a predetermined period of time;

[0653] cooling the treated precursor; and

[0654] washing the at least one organic salt from the treated precursor to produce an initial particulate product, the particles of the particulate product comprising calcium carbonate crystals in a carbon, preferably glassy carbon, matrix: and

[0655] removing at least a portion of the calcium carbonate crystals, for example by washing the initial particulate product in an acidic solution to remove at least a portion of the calcium carbonate crystals or by heating the initial particulate product to melt or evaporate and thereby remove at least a portion of the calcium carbonate crystals, in which BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g.

[0656] Ex6C. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6B, in which the steps of washing the at least one organic salt from the treated precursor and washing the initial particulate product in an acidic solution to remove at least a portion of the calcium carbonate crystals are conducted simultaneously by washing the treated precursor in an acidic solution to remove the salt and at least a portion of the calcium carbonate crystals.

[0657] Ex6D. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6C, in which the step of washing in acidic solution is conducted until at least 50% of the calcium carbonate crystals are removed, preferably at least 60%, preferably at least 70%, or at least 80%, or at least 90%, particularly preferably until substantially all of the calcium carbonate crystals are removed.

[0658] Ex6E. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6D, in which the resulting carbon, preferably glassy carbon, particles are highly porous particles, preferably in which the particles comprise rounded, semi-circular and / or through holes that extend through individual carbon, preferably glassy carbon, particles.P / 91817

[0659] Ex6F. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6E, in which the carbon, preferably glassy carbon, particles comprise a plurality of holes, and the holes have a diameter or cross-sectional dimension of between 5 nm and 500 nm, for example between 10 nm and 400 nm.

[0660] Ex6G. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6F, in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 750 m2 / g, or greater than 800 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 500 m2 / g and 900 m2 / g, for example between 600 m2 / g and 800 m2 / g.

[0661] Ex6H. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6G, in which the at least one inorganic salt comprises a calcium halide salt, for example calcium chloride, preferably in which the at least one inorganic salt is a mixture of a calcium halide salt and at least one other inorganic salt, for example in which the at least one inorganic salt is a mixture of sodium chloride and calcium chloride.

[0662] Ex6L A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6H, in which the at least one inorganic salt is a mixture of two or more inorganic salts, preferably in which the composition of the mixture of two or more inorganic salts is selected to control the melting point of the salt mixture, for example in which the at least one inorganic salt is a mixture of NaCI and CaCl2, for example a eutectic or near-eutectic mixture of NaCI and CaCl2, optionally in which the at least one inorganic salt is a CaCl2-NaCI-MgCl2 mixture, or a CaCl2-NaCI-KCI-MgCl2 mixture, or a CaCI2-NaCI-KCI mixture, or a CaCI2-LiCI-KCI mixture.

[0663] Ex6J. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6l, in which the predetermined treatment temperature is at least 100°C in excess of the melting point of the at least one inorganic salt, for example at least 150°C in excess of the melting point of the at least one inorganic salt, or at least 200°C in excess of the melting point of the at least one inorganic salt.

[0664] Ex6K. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6 J, in which the predetermined treatment temperature is no more than 500°C in excess of the melting point of the at least one inorganic salt, for example no more than 400°C in excess of the melting point of the at least one inorganic salt, preferably no more than 300°C in excess of the melting point of the at least one inorganic salt.

[0665] Ex6L. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6K, in which the predetermined treatment temperature is between 400°C and 1200°C, preferably between 500°C and 1000°C, for example between 600°C and 900°C.

[0666] Ex6M. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6L, in which the particulate product comprises particles having an average particle size of between 1 micron and 1000 microns, for example between 2 microns and 800 microns, for example between 4 microns and 500 microns, or between 5 microns and 400 microns.

[0667] Ex6N. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6M, in which the acidic solution has a pH value of between 0.5 and 7, for example between 1 and 4.

[0668] Ex6O. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6N, in which a salt recovery step is conducted after the washing step to recover the at least one inorganic salt from the wash and / or in which a calcium carbonate recovery step is conducted to recover calcium carbonate from the acidic solution.P / 91817

[0669] Ex6P. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex60, in which the thermal treatment is conducted in an oxidising atmosphere, for example in air.

[0670] Ex6Q. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex6A to Ex6P, comprising the further step of milling the carbon, preferably glassy carbon, particles to increase the surface area, for example ball milling the carbon, preferably glassy carbon, particles, preferably milling until the BET specific surface area is increased by between 10% and 300%, for example between 20% and 200%, for example between 30% and 100%, preferably in which milled carbon, preferably glassy carbon, particles have a BET surface area greater than 600 m2 / g, for example greater than 700 m2 / g, or greater than 800 m2 / g, for example greater than 850 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 600 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g, or between 800 m2 / g and 900 m2 / g.

[0671] Ex7A. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to any of examples Ex1 A to Ex1 U, in which the carbon, preferably glassy carbon, material is a coating on a carbon, preferably glassy carbon, coated object, the method comprising the steps of:

[0672] coating a meltable organic precursor onto a surface of an object thereby forming a meltable organic coating; heating the meltable organic coating to a temperature above the melting point of the meltable organic coating; further heating the meltable organic coating to a predetermined treatment temperature in excess of 300°C; optionally maintaining the meltable organic coating at or above the predetermined treatment temperature for a predetermined period of time thereby forming a treated organic coating; and

[0673] cooling the treated organic coating to produce the carbon, preferably glassy carbon, coated object.

[0674] Ex7B. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to any of examples Ex1 A to Ex1 U, in which the carbon, preferably glassy carbon, material is a coating on a carbon, preferably glassy carbon, coated object the method comprising the steps of:

[0675] heating a meltable organic precursor thereby forming a molten organic precursor; arranging for the object to contact the molten organic precursor thereby forming a molten organic coating on at least one surface of the object;

[0676] further heating the molten organic coating to a predetermined treatment temperature in excess of 300°C; optionally maintaining the molten organic coating at or above the predetermined treatment temperature for a predetermined period of time thereby forming a treated organic coating; and

[0677] cooling the treated organic coating to produce the carbon, preferably glassy carbon, coated object.

[0678] Ex7C. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex7A to Ex7B, in which in which the thermal treatment is conducted in an oxidising atmosphere and the carbon, preferably glassy carbon, coating has a BET surface area greater than 200 m2 / g, for example greater than 300 m2 / g.

[0679] Ex7D. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex7A to Ex7B, in which the thermal treatment is conducted in an reducing atmosphere and the carbon, preferably glassy carbon, coating has a BET surface area less than 50 m2 / g, for example less than 20 m2 / g, or less than 10 m2 / g, or less than 5 m2 / g.

[0680] Ex7E. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex7A to Ex7D, in which the object is an electrode and the resulting product is a carbon, preferably glassy carbon, coated electrode,P / 91817

[0681] for example in which the object is a graphite electrode and the resulting product is a carbon, preferably glassy carbon, coated graphite electrode.

[0682] Ex7F. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex7A to Ex7D, in which the object is a fuel rod and the resulting product is a carbon, preferably glassy carbon, coated fuel rod. Ex7G. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex7A to Ex7D, in which the object is a medical implant and the resulting product is a carbon, preferably glassy carbon, coated medical implant.

[0683] Ex7H. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex7A to Ex7D, in which the object is plurality of particles and the resulting product is a plurality of carbon, preferably glassy carbon, coated particles, for example in which each of the plurality of particles is coated with carbon, preferably glassy carbon,.

[0684] Ex7l. A method of producing carbon, preferably glassy carbon, material according to Ex7H, in which the plurality of particles are a plurality of metallic particles, or a plurality of ceramic particles, or a plurality of alloy particles, or a plurality of intermetallic particles.

[0685] Ex7J. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex7A to Ex7D, in which the object is a container such as a waste container and the resulting product is a container such as a waste container coated with carbon, preferably glassy carbon,, for example coated on the inside and / or outside with carbon, preferably glassy carbon,.

[0686] Ex7K. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex7A to Ex7D, in which the object is a nuclear material, for example a nuclear waste container, or nuclear waste material.

[0687] Ex8A. A method of producing carbon, preferably glassy carbon, material by thermal treatment of a meltable organic precursor, for example a method according to any preceding example, in which the carbon, preferably glassy carbon, material is upcycled carbon, preferably glassy carbon, material formed from thermoplastic waste, the method comprising the steps of:

[0688] comminuting thermoplastic waste to form a recycled thermoplastic precursor, heating the recycled thermoplastic precursor to a temperature above the melting point of the recycled thermoplastic precursor;

[0689] further heating the recycled thermoplastic precursor to a predetermined treatment temperature in excess of 300°C;

[0690] optionally maintaining the recycled thermoplastic precursor at, or above, the predetermined treatment temperature for a predetermined period of time thereby forming a treated precursor; and

[0691] cooling the treated precursor to produce the upcycled carbon, preferably glassy carbon, material.

[0692] Ex8B. A method of producing carbon, preferably glassy carbon, material according to example Ex8A, in which the recycled thermoplastic precursor is formed by comminuting, for example by cutting, waste thermoplastic products, such as sheets or bottles, into precursor elements having length and width dimensions of between 0.5 cm and 3 cm, for example between 0.75 cm and 2 cm, for example about 1 cm, for example in which the precursor elements have a length of between 0.5 cm and 3 cm, a width of between 0.5 cm and 3 cm, and a thickness of less than 1 mm.

[0693] Ex8C. A method of producing carbon, preferably glassy carbon, material according to example Ex8A or Ex8B, in which the thermoplastic waste is washed before and / or after the comminution step.

[0694] Ex8D. A method of producing carbon, preferably glassy carbon, material according to any of examples Ex8A to Ex8C, in which the thermoplastic waste comprises, or is, used drinks bottles, for example used PET bottles.P / 91817

[0695] Ex9A. A method of forming a product comprising carbon, preferably glassy carbon, particles, the method comprising the steps of:

[0696] forming carbon, preferably glassy carbon, particles by a method of producing carbon, preferably glassy carbon, material according to any preceding example; and

[0697] consolidating the carbon, preferably glassy carbon, particles to form the product.

[0698] Ex9B. A method of forming a product comprising carbon, preferably glassy carbon, particles according to Ex9A, comprising the step of:

[0699] mixing the carbon, preferably glassy carbon, particles with at least one consolidation agent, for example at least one of a lubricant, a binder, and a sintering aid, to form a product precursor mixture; and

[0700] consolidating the product precursor mixture.

[0701] Ex9C. A method of forming a product comprising carbon, preferably glassy carbon, particles according to Ex9A or Ex9B, in which consolidation is effected by traditional or advanced powder metallurgical techniques, for example in which consolidation is effected by a process selected from the list consisting of pressing, sintering, selective laser sintering, printing, hot isostatic pressing, or cold isostatic pressing.

[0702] Ex9D. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9B to Ex9C, in which the product precursor mixture comprises a sintering aid or a binder, in which the sintering aid or the binder is a polymeric material, a ceramic material, or a metallic material, preferably in which the sintering aid or the binder is a metal, for example a refractory metal.

[0703] Ex9E. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9B to Ex9D, in which the product precursor mixture comprises a metallic object or metallic particles, in which the product precursor mixture is consolidated at a sufficient temperature to form a metal carbide interface between the carbon, preferably glassy carbon, particles and the metallic object or metallic particles.

[0704] Ex9F. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9B to Ex9E, in which the product precursor mixture comprises further filler particles, for example further carbonaceous particles, for example particles of carbon, or particles of graphite, or particles of carbon nanostructures such as graphene or nanotubes.

[0705] Ex9G. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9A to Ex9F, in which the step of consolidating the carbon, preferably glassy carbon, particles, for example the product precursor mixture that comprises the carbon, preferably glassy carbon, particles, is conducted at a temperature of greater than 300°C, for example greater than 500°C, for example greater than 1000°C.

[0706] Ex9H. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9A to Ex9G, in which the step of consolidating the carbon, preferably glassy carbon, particles, for example the product precursor mixture that comprises the carbon, preferably glassy carbon, particles, is conducted in a reducing atmosphere or an inert atmosphere.

[0707] Ex9L A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9B to Ex9H, in which the product precursor mixture comprises metallic particles, in which the product precursor mixture comprises between 1 vol% and 25 vol % metallic particles, for example between 2.5 vol% and 20 vol % metallic particles, for example between 5 vol% and 15 vol % metallic particles

[0708] Ex9J. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9B to Ex9l, in which the product precursor mixture comprises at least one organic binder.P / 91817

[0709] Ex9K. A method of forming a product comprising carbon, preferably glassy carbon, particles according to Ex9 J, in which consolidation of the product precursor mixture comprising the at least one organic binder involves a step of forming the product precursor mixture into a shape, or coating the product precursor mixture onto a substrate, and drying the product precursor mixture.

[0710] Ex9L. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9A to Ex9K, comprising the steps of:

[0711] forming carbon, preferably glassy carbon, particles by a method of producing carbon, preferably glassy carbon, material according to any preceding example;

[0712] mixing the carbon, preferably glassy carbon, particles with a binder and conductive carbon particles, forming a product precursor mixture; and

[0713] consolidating the product precursor mixture to form the product.

[0714] Ex9M. A method of forming a product comprising carbon, preferably glassy carbon, particles according to Ex9L, in which the product precursor mixture comprises between 50 mass% and 90 mass% of the carbon, preferably glassy carbon, particles, between 25 mass % and 5 mass% of binder and between 25 mass% and 5 mass % conductive carbon particles.

[0715] Ex9N. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9A to Ex9M, in which the carbon, preferably glassy carbon, particles, or the product precursor mixture that comprises the carbon, preferably glassy carbon, particles, is consolidated onto, or in contact with, an electrically conductive substrate to form an electrode.

[0716] Ex90. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9A to Ex9N, comprising a further step of grading the carbon, preferably glassy carbon, particles, for example by sieving, for example in order to obtain a preferred particle size and / or particle size distribution.

[0717] Ex9P. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex9A to Ex9O, comprising a further step of milling the carbon, preferably glassy carbon, particles, for example to obtain a desired particle size and / or a desired surface area.

[0718] Ex10A. A method of forming a product comprising carbon, preferably glassy carbon, particles, for example a method according to any of examples 9A to 9P, the method being a method of forming an electrode, for example for a metal ion battery, the method comprising the steps of:

[0719] forming carbon, preferably glassy carbon, particles by a method of producing carbon, preferably glassy carbon, material according to any preceding example;

[0720] forming an electrode precursor mixture comprising or consisting of the carbon, preferably glassy carbon, particles;

[0721] arranging the electrode precursor mixture in contact with a conductive substrate; and

[0722] consolidating the electrode precursor mixture to the conductive substrate to form the electrode.

[0723] Ex10B. A method of forming a product comprising carbon, preferably glassy carbon, particles according to Ex10A, in which the conductive substrate is a current collector, for example a foil or mesh, optionally comprises or formed of a conductive metal or alloy, for example Al, Cu, Ni, Ti, or stainless steel.

[0724] Ex10C. A method of forming a product comprising carbon, preferably glassy carbon, particles according to Ex10A or Ex1 OB, in which the electrode precursor mixture is formed into a slurry, applied to the conductive substrate, and dried to consolidate the electrode precursor mixture to the conductive substrate.P / 91817

[0725] Ex10D. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10A to Ex10C, in which the electrode precursor mixture comprises the carbon, preferably glassy carbon, particles and an organic binder, for example carboxymethyl cellulose (CMC) and / or Polyvinylidene Fluoride (PVDF).

[0726] Ex10E. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10A to Ex10D, in which the electrode precursor mixture comprises the carbon, preferably glassy carbon, particles and conductive carbon particles.

[0727] Ex10F. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10A to Ex10E, in which the electrode precursor mixture comprises between 50 mass% and 95 mass% of the carbon, preferably glassy carbon, particles, between 25 mass % and 2.5 mass% of an organic binder and between 25 mass% and 2.5 mass % conductive carbon particles, preferably between 50 mass% and 90 mass% of the carbon, preferably glassy carbon, particles, between 25 mass % and 5 mass% of an organic binder and between 25 mass% and 5 mass % conductive carbon particles.

[0728] Ex10G. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10A to Ex1 OF, in which the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a d002 plane spacing, measured for example by XRD, of between 0.36 nm and 0.45 nm, for example between 0.37 nm and 0.44 nm, for example between 0.38 nm and 0.42 nm, for example in which the product is an electrode for a lithium ion battery or a sodium ion battery or a potassium ion battery or a zinc ion battery.

[0729] Ex10H. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10A to Ex1 OF, in which the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a BET surface area of lower than 50 m2 / g, for example lower than 30 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g, for example in which the product is an electrode for a lithium ion battery or a sodium ion battery.

[0730] Ex10L A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10A to Ex1 OF, in which the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g, for example in which the product is an electrode for a lithium ion battery or a sodium ion battery or a potassium ion battery or a zinc ion battery.

[0731] Ex10J. A method of forming a product comprising carbon, preferably glassy carbon, particles, for example a method according to any of examples 9A to 9P, the method being a method of forming an electrode, for example for an electrolytic cell.

[0732] Ex10K. A method of forming a product comprising carbon, preferably glassy carbon, particles according to example Ex10J, in which the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a d002 plane spacing, measured for example by XRD, of between 0.36 nm and 0.45 nm, for example between 0.37 nm and 0.44 nm, for example between 0.38 nm and 0.42 nm.

[0733] Ex10L. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10J to Ex1 OK, in which the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a BET surface area of lower than 50 m2 / g, for example lower than 30 m2 / g, for exampleP / 91817

[0734] lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g.

[0735] Ex10M. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10 J to Ex10L, in which the carbon, preferably glassy carbon, particles are formed from carbon, preferably glassy carbon, material having a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for example greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g.

[0736] Ex10N. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10J to Ex10M, in which the electrode is for use as an anode of a Hall-Heroult cell for aluminium production, or an anode of a molten oxide cell, or an anode of a molten salt electrolysis cell.

[0737] Ex10O. A method of forming a product comprising carbon, preferably glassy carbon, particles according to any of examples Ex10J to Ex1 ON, in which the electrode is for use as an anode of a molten oxide cell used for metal production such as iron or steel production, or an anode of a molten salt electrolysis cell used for the preparation of metals and alloys, or an anode of a molten salt electrolysis cell containing hydrogen cations used for the preparation of metals, alloys and hydrogen.

[0738] Ex11A. A particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles, each carbon, preferably glassy carbon, particle comprising, or consisting of, carbon, preferably glassy carbon, material, in which the carbon, preferably glassy carbon, material is formed according to any preceding example defining a method of forming carbon, preferably glassy carbon, material.

[0739] Ex11B. A particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles, for example a particulate carbon, preferably glassy carbon, product according to Ex11A, each carbon, preferably glassy carbon, particle comprising, or consisting of, carbon, preferably glassy carbon, material, in which the carbon, preferably glassy carbon, material is characterised by a d002 plane spacing, measured for example by XRD, of between 0.35 nm and 0.45 nm, for example between 0.36 nm and 0.44 nm, for example between 0.37 nm and 0.42 nm.

[0740] Ex11C. A particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles according to any of Ex11A to Ex11B, in which the carbon, preferably glassy carbon, material comprises graphitic nano-crystallites having maximum dimensions in the range of 0.5 nm to 5 nm, for example 1 nm to 3 nm.

[0741] Ex11D. A particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles according to any of Ex11A to Ex11C, in which the carbon, preferably glassy carbon, material has a Raman / l G value of between 0.9-1.3, for example between 1.0 and 1.2.

[0742] Ex11E. A particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles according to any of Ex11A to Ex11 D, in which the carbon, preferably glassy carbon, particles have an average particle size of between 1 micron and 1000 microns, for example between 2 microns and 800 microns, for example between 4 microns and 500 microns, or between 5 microns and 400 microns.

[0743] Ex11F. A particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles according to any of Ex11 A to Ex11 E, in which the carbon, preferably glassy carbon, particles have a BET surface area of greater than 500 m2 / g, for example greater than 600 m2 / g, or greater than 700 m2 / g, for exampleP / 91817

[0744] greater than 800 m2 / g, or greater than 900 m2 / g, preferably in which the BET surface area of the carbon, preferably glassy carbon, particles is between 400 m2 / g and 1200 m2 / g, for example between 700 m2 / g and 1000 m2 / g.

[0745] Ex11G. A particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles according to any of Ex11 A to Ex11 E, in which the carbon, preferably glassy carbon, particles have a BET surface area of lower than 50 m2 / g, for example lower than 30 m2 / g, for example lower than 20 m2 / g, or lower than 10 m2 / g, preferably in which the BET surface area of the resulting carbon, preferably glassy carbon, particles is between 1 m2 / g and 5 m2 / g, for example between 2 m2 / g and 3 m2 / g.

[0746] Ex11H. A particulate carbon, preferably glassy carbon, product comprising a plurality of carbon, preferably glassy carbon, particles acc...

Claims

1. P / 91817CLAIMS1. A method of producing glassy carbon material by thermal treatment of a meltable organic precursor, the method comprising the steps of:heating the meltable organic precursor to a temperature above the melting point of the meltable organic precursor;further heating the meltable organic precursor to a predetermined treatment temperature to form a treated organic precursor, the predetermined treatment temperature being at least 200°C in excess of the melting point of the meltable organic precursor; andcooling the treated organic precursor to produce the glassy carbon material.

2. A method according to claim 1 , wherein the predetermined treatment temperature is between 500°C and 2000°C, or between 700°C and 900°C.

3. A method according to claim 1 or 2, wherein the glassy carbon material comprises glassy carbon particles, and wherein the thermal treatment is conducted in a reducing atmosphere, and the BET surface area of the resulting glassy carbon particles is lower than 50 m2 / g.

4. A method according to claim 1 or 2, wherein the glassy carbon material comprises glassy carbon particles, and wherein the thermal treatment is conducted in an oxidising atmosphere and the BET surface area of the resulting glassy carbon particles is greater than 400 m2 / g.

5. A method according to claim 4, wherein the glassy carbon particles comprise a number of surfaces, in which the number of surfaces are all of the surfaces of the glassy carbon particles, a proportion of the surfaces being smooth surfaces and a proportion of the surfaces being highly textured surfaces, in which between 10% and 70% of the number of surfaces are highly textured surfaces.

6. A method according to any preceding claim, wherein:the glassy carbon material comprises glassy carbon particles;the method comprises arranging the meltable organic precursor in contact with at least one inorganic salt having a melting point greater than 300°C;the step of heating comprises controlling temperature of the meltable organic precursor and the at least one inorganic salt to a predetermined treatment temperature in excess of the melting point of the inorganic salt to form a treated precursor; andthe method comprises washing the at least one inorganic salt from the treated precursor to produce the glassy carbon particles,in which BET surface area of the glassy carbon particles is greater than 400 m2 / g.

7. A method according to claim 6, wherein the at least one inorganic salt is a eutectic or near-eutectic mixture of NaCI and KCI.

8. A method according to claim 6, wherein:the glassy carbon particles are glassy carbon composite particles comprising calcium carbonate crystals in a glassy carbon matrix; andthe at least one inorganic salt contains calcium.P / 918179. A method according to claim 8, wherein the glassy carbon matrix comprises one or both of blind holes and through- holes, wherein an average diameter of each the holes is between 2 nm and 500 nm, and at least some of the calcium carbonate crystals are at least partially located in at least some of the holes of the glassy carbon matrix.

10. A method according to claim 8 or 9, wherein the step of washing the at least one inorganic salt from the treated precursor comprises washing in an acidic solution to simultaneously remove at least a portion of the calcium carbonate crystals and the at least one inorganic salt from the treated precursor.

11. A method according to any preceding claim, wherein:the glassy carbon material is a coating on a glassy carbon coated object;the method comprises coating a meltable organic precursor onto a surface of an object thereby forming a meltable organic coating;the step of heating comprises heating the meltable organic coating to a temperature above the melting point of the meltable organic coating;the step of further heating is a step of further heating the meltable organic coating to the predetermined treatment temperature in excess of 300°C thereby forming a treated organic coating; andthe step of cooling is a step of cooling the treated organic coating to produce the glassy carbon coated object.

12. A method according to any of claims 1 to 10, wherein:the glassy carbon material is a coating on a glassy carbon coated object;the method comprises, between the steps of heating and further heating, arranging for an object to contact the molten organic precursor thereby forming a molten organic coating on at least one surface of the object; the step of further heating is a step of further heating the molten organic coating to the predetermined treatment temperature in excess of 300°C thereby forming a treated organic coating; andthe step of cooling is a step of cooling the treated organic coating to produce the glassy carbon coated object.

13. A method according to claim 11 or 12, in which the thermal treatment is conducted in an oxidising atmosphere and the glassy carbon coating has a BET surface area greater than 200 m2 / g.

14. A method according to claim 11 or 12, in which the thermal treatment is conducted in a reducing atmosphere and the glassy carbon coating has a BET surface area less than 50 m2 / g.

15. A method according to any of claims 11 to 14, in which the object is one of: an electrode, a fuel rod, a medical implant, a container, or nuclear material.

16. A method according to any preceding claim, wherein the carbon, preferably glassy carbon, material is upcycled glassy carbon material formed from thermoplastic waste.

17. A method of forming a product precursor mixture comprising glassy carbon particles, the method comprising the steps of:producing glassy carbon material by a method according to any of claims 1 to 10; andmixing the glassy carbon particles with at least one consolidation agent to form the product precursor mixture.

18. A method of forming a product comprising glassy carbon particles, the method comprising the steps of:producing glassy carbon material by a method according to any of claims 1 to 10; andmixing the glassy carbon particles with at least one consolidation agent to form a product precursor mixture; andconsolidating the product precursor mixture.

19. A method of forming a product comprising glassy carbon particles, the method comprising the steps of:P / 91817producing glassy carbon material by a method according to any of claims 1 to 10; andconsolidating the glassy carbon particles to form the product.

20. A method according to claim 18, wherein the product precursor mixture comprises a metallic object or metallic particles, and the step of consolidating the product precursor forms a metal carbide interface between the glassy carbon particles and the metallic object or metallic particles.

21. A method according to any of claims 18 to 20, wherein the step of consolidating is conducted in a reducing atmosphere.

22. A method according to claim 19, wherein:the product is an electrode;the method comprises forming an electrode precursor mixture comprising or consisting of the glassy carbon particles;the method comprises arranging the electrode precursor mixture in contact with a conductive substrate; and the step of consolidating comprises consolidating the electrode precursor mixture to the conductive substrate to form the electrode.

23. A glassy carbon material, wherein: carbon, oxygen, if present, and hydrogen, if present, make up at least 99 wt% of the material; carbon makes up at least 90 wt% of the material; the material has only two peaks in an XRD pattern, a first peak appearing in the range of 20-27 degrees and a second peak appearing in the range 40-48 degrees; the material has a d002 spacing between 0.36 and 0.45 nanometres; and the material has a Raman ID / IG value of between 0.9 and 1.3.

24. A particulate glassy carbon product comprising a plurality of glassy carbon particles, each glassy carbon particle comprising a plurality of through-holes, each of the plurality of holes having a diameter or cross-sectional dimension of between 5 nm and 500 nm.

25. A composite comprising the particulate carbon product of claim 24 and at least one further material.

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