Porous carbon scaffold material processing

Abstract

A method and system for performing dual fine particle removal. The system includes a particle size reduction device (grinding mill), a separator, and a fan. The grinding mill is configured to reduce the particle size of a porous carbon scaffold material to produce porous carbon scaffold particles and fine carbon particles with a desired particle size distribution, and to separate the desired porous carbon scaffold particle size from the fine carbon particles. The fan is configured to entrain porous carbon scaffold particles from the grinding mill. The separator is configured to receive the entrained porous carbon scaffold particles and further separate the desired porous carbon scaffold particles from the remaining fine carbon particles.

Description

Background Technology

[0001] Controlling particle size distribution is a crucial factor in powder processing. In particular, fine carbon particles (i.e., fine carbon grains) are undesirable in many particle processing techniques, such as chemical vapor infiltration (CVI) for porous carbon particles.

[0002] Current technologies for removing fine carbon particles include spiral jet mills, which sometimes have a collector tip positioned below the mill. The collector tip allows some of the coarse product stream to separate from the mill's grinding air and the excessively fine particles suspended in the grinding air. However, unwanted fine carbon particles may still remain in the coarse output produced by the spiral jet mill. Summary of the Invention

[0003] Various disclosed embodiments include illustrative systems and methods for generating carbon particles and carbon particles permeated by an electrochemical modifier. In some embodiments, the electrochemical modifier comprises at least one group 14 element (e.g., carbon or silicon).

[0004] In an illustrative embodiment, the system includes a grinder (e.g., a jet mill, ball mill, water jet mill, and other methods known in the art), a separator, and a fan. The grinder is configured to reduce the particle size of the porous carbon scaffold material to produce porous carbon scaffold particles and fine carbon particles having a desired particle size distribution, and to separate the desired porous carbon scaffold particle size from the fine carbon particles. The fan is configured to entrain the porous carbon scaffold particles from the grinder. The separator is configured to receive the entrained porous carbon scaffold particles and further separate the desired porous carbon scaffold particles from the remaining fine carbon particles.

[0005] In another illustrative embodiment, the method includes grinding the porous carbon scaffold material using a dual-emission jet mill to produce porous carbon scaffold particles and carbon fines, separating the carbon fines from the porous carbon scaffold particles, entraining the porous carbon scaffold particles from the dual-emission jet mill to a separator, and using the separator to separate the remaining carbon fines from the entrained porous carbon scaffold particles.

[0006] In yet another illustrative embodiment, the system includes a porous carbon generation system, a dual fine particle removal system, and a chemical vapor infiltration system. The porous carbon generation system is configured to generate porous carbon scaffold material, and the chemical vapor infiltration system is configured to permeate the pores of the porous carbon scaffold particles with an electrochemical modifier (e.g., silicon). The dual fine particle removal system includes a grinder, a fan, and a separator. The grinder is configured to grind the porous carbon scaffold material to generate porous carbon scaffold particles and carbon fine particles, and to separate the porous carbon scaffold particles from the carbon fine particles. The fan is configured to carry the porous carbon scaffold particles from the grinder, and the separator is configured to further separate the porous carbon scaffold particles from the remaining carbon fine particles. Attached Figure Description

[0007] Figure 1 This is a block diagram of a material processing system formed according to an embodiment of the present invention.

[0008] Figure 2 This is a schematic block diagram of a dual fine particle removal system formed according to an embodiment of the present invention.

[0009] Figure 3 This is a flowchart of a dual fine particle removal method according to an embodiment of the present invention. Detailed Implementation

[0010] In the following description, certain specific details are set forth to provide a full understanding of various embodiments. However, those skilled in the art will understand that this disclosure may be practiced without these details. In other instances, well-known structures have not been shown or described in detail to avoid unnecessarily obscuring the description of the embodiments. Unless the context otherwise requires, throughout the specification and the following claims, the word “comprise” and its variations, such as “comprises” and “comprising”, shall be interpreted in an open-ended, inclusive sense, meaning “including, but not limited to”. Furthermore, the headings provided herein are merely for convenience and do not constitute an explanation of the scope or meaning of the claimed disclosure.

[0011] Throughout this specification, references to "an embodiment" or "an embodiment" mean that a specific feature, structure, or characteristic described in connection with that embodiment is included in at least one embodiment. Therefore, the phrases "in an embodiment" or "in an embodiment" appearing throughout the specification do not necessarily refer to the same embodiment. Furthermore, in one or more embodiments, specific features, structures, or characteristics may be combined in any suitable manner. Additionally, as used in this specification and the appended claims, the singular forms "a / an" and "the" include plural indicators unless otherwise expressly stated. It should also be noted that the term "or" is generally used in its meaning encompassing "and / or" unless otherwise expressly stated.

[0012] In various implementation schemes, such as Figure 1 As shown, a system 20 for producing carbon materials with electrochemical modifiers is illustrated. System 20 includes a porous carbon production system 22, a dual fine particle removal system 24, and a chemical vapor infiltration system 26.

[0013] A. Porous support material

[0014] For the purposes of embodiments of this disclosure, a porous scaffold can be used, into which one or more electrochemical modifiers (e.g., lithium or silicon) can be impregnated. Throughout this document, the porous scaffold can comprise a variety of materials. In some embodiments, the porous scaffold material primarily comprises carbon, such as hard carbon. In other embodiments, other allotropes of carbon are also contemplated, such as graphite, amorphous carbon, diamond, C60, carbon nanotubes (e.g., single-walled and / or multi-walled), graphene, and / or carbon fibers. Porosity can be introduced into carbon materials in various ways. For example, porosity in a carbon material can be achieved by adjusting the polymer precursor and / or processing conditions to produce the porous carbon material, as described in detail in subsequent sections.

[0015] In other embodiments, the porous scaffold comprises a polymeric material. Therefore, a variety of polymers are contemplated as practical in various embodiments, including but not limited to inorganic polymers, organic polymers, and other polymers. Examples of organic polymers include, but are not limited to, sulfur-containing polymers (e.g., polysulfides and polysulfones), low-density polyethylene (LDPE), high-density polyethylene (HDPE), polypropylene (PP), polyvinyl chloride (PVC), polystyrene (PS), nylon, nylon 6, nylon 6,6, Teflon (polytetrafluoroethylene), thermoplastic polyurethane (TPU), polyurea, poly(lactide), poly(glycolic acid) and combinations thereof, phenolic resins, polyamides, polyarylamides, polyethylene terephthalate, polychloroprene, polyacrylonitrile, polyaniline, polyimide, poly(3,4-ethylenedioxythiophene)polystyrene sulfonate (PDOT:PSS), polymerized polydivinylbenzene, and other organic polymers known in the art. Organic polymers may be synthetic or of natural origin. In some embodiments, the polymer is a polysaccharide, such as sucrose, starch, cellulose, cellobiose, amylose, amylopectin, gum arabic, lignin, etc. In some embodiments, the polysaccharide is derived from the caramelization of monosaccharides or oligosaccharides (e.g., fructose, glucose, sucrose, maltose, raffinose, etc.).

[0016] In some embodiments, the porous scaffold polymer material comprises a coordination polymer. Coordination polymers as used herein include, but are not limited to, metal-organic frameworks (MOFs). Techniques for generating MOFs and exemplary types of MOFs are known and described in the art. "The Chemistry and Applications of Metal-Organic Frameworks, Hiroyasu Furukawa et al. Science 341, (2013); DOI: 10.1126 / science.1230444 Examples of MOFs in this article include, but are not limited to, Basolite. TM Materials and zeolite imidazole ester skeleton (ZIF).

[0017] In various embodiments, while considering the potential of the various polymers envisioned to provide porous substrates, various processing methods are contemplated to achieve said porosity. Throughout this document, as is known in the art, numerous general methods for imparting porosity to various materials are available, including, but not limited to, methods involving: emulsification, micelle generation, vaporization, dissolution followed by solvent removal (e.g., lyophilization), axial pressing and sintering, gravity sintering, powder rolling and sintering, isostatic pressing and sintering, metal spraying, metal coating and sintering, metal injection molding and sintering, etc. Other methods for producing porous polymer materials are also contemplated, including the production of porous gels, such as lyophilized gels, aerogels, etc.

[0018] In some embodiments, the porous scaffold material comprises a porous ceramic material. In some embodiments, the porous scaffold material comprises a porous ceramic foam. Throughout this document, as is known in the art, a variety of general methods for imparting porosity to ceramic materials are available, including, but not limited to, generating porosity. Throughout this document, general methods and materials suitable for constituting porous ceramics include, but are not limited to, porous alumina, porous zirconia-toughened alumina, porous partially stabilized zirconia, porous alumina, porous sintered silicon carbide, sintered silicon nitride, porous cordierite, porous zirconium oxide, clay-bonded silicon carbide, etc.

[0019] In some embodiments, the porous material comprises a porous metal. Suitable metals in this regard include, but are not limited to, porous aluminum, porous steel, porous nickel, porous inconcelite, porous hastelloy, porous titanium, porous copper, porous brass, porous gold, porous silver, porous germanium, and other metals capable of forming a porous structure, as known in the art. In some embodiments, the porous support material comprises a porous metal foam. The types of metals and associated manufacturing methods are known in the art. Such methods include, but are not limited to, casting (including foaming, infiltration, and lost foam casting), deposition (chemical and physical), gas eutectic formation, and powder metallurgy techniques (e.g., powder sintering, compaction in the presence of a foaming agent, and fiber metallurgy techniques).

[0020] B. Porous carbon scaffold materials

[0021] Methods for preparing porous carbon materials from polymer precursors are known in the art. For example, methods for preparing carbon materials are described in U.S. Patents Nos. 7,723,262, 8,293,818, 8,404,384, 8,654,507, 8,916,296, 9,269,502, 10,590,277, and 10,711,140, ​​the entire disclosure of which is incorporated herein by reference for all purposes.

[0022] Therefore, in one embodiment, this disclosure provides a method for preparing any of the above-described carbon materials or polymer gels. This method can be carried out using a porous carbon generation system 22. The carbon material can be synthesized by the pyrolysis of a single precursor and a combination thereof, said single precursor being, for example, a carbohydrate material, such as sucrose, fructose, glucose, dextrin, maltodextrin, starch, amylopectin, amylose, lignin, gum arabic, and other carbohydrates known in the art. Alternatively, the carbon material can be synthesized by the pyrolysis of a composite resin, for example using a sol-gel method with a polymer precursor (e.g., phenol, resorcinol, bisphenol A, urea, melamine, and other suitable compounds and combinations thereof) in a suitable solvent (e.g., water, ethanol, methanol, and other solvents and combinations thereof) and a crosslinking agent (e.g., formaldehyde, hexamethylenetetramine, furfural, and other crosslinking agents and combinations thereof known in the art). The resin can be acidic or basic and can contain a catalyst. The catalyst can be volatile or non-volatile. As known in the art, the pyrolysis temperature and residence time can be varied.

[0023] In some embodiments, the method includes preparing a polymer gel via a sol-gel process, a condensation process, or a crosslinking process (involving a monomer precursor and a crosslinking agent, two existing polymers and a crosslinking agent, or a single polymer and a crosslinking agent), followed by pyrolysis of the polymer gel. The polymer gel may be dried (e.g., freeze-dried) prior to pyrolysis; however, drying is not necessarily required.

[0024] The target carbon property can be derived from various polymer chemistry properties, as long as the polymerization reaction produces a resin / polymer with the necessary carbon backbone. Different polymer families include Novolacs, Resoles, acrylates, styrene, urethane, rubbers (chloroprene, styrene-butadiene, etc.), nylon, etc. The preparation of any of these polymer resins can be carried out by many different methods, including sol-gel, emulsion / suspension, solid, solution, and molten states for polymerization and crosslinking methods.

[0025] In some embodiments, the reactant includes phosphorus. In some other embodiments, the phosphorus is in the form of phosphoric acid. In some other embodiments, the phosphorus may be in the form of a salt, wherein the anion of said salt includes one or more phosphate ions, phosphite ions, phosphide ions, hydrogen phosphate ions, dihydrogen phosphate ions, hexafluorophosphate ions, hypophosphite ions, polyphosphate ions, or pyrophosphate ions, or combinations thereof. In some other embodiments, the phosphorus may be in the form of a salt, wherein the cation of said salt includes one or more phosphonium ions. The phosphate-free anion or cation pair used in any of the above embodiments may be selected from those known and described in the art. Exemplary cations paired with phosphate-containing anions include, but are not limited to, ammonium ions, tetraethylammonium ions, and tetramethylammonium ions. Exemplary anions paired with phosphate-containing cations include, but are not limited to, carbonate ions, bicarbonate ions, and acetate ions.

[0026] In some embodiments, the reactants include sulfur. In some other embodiments, the sulfur is in the form of sulfuric acid. In some other embodiments, the sulfur may be in the form of a salt, wherein the anion of said salt includes one or more sulfate, sulfite, bisulfite, bisulfite, hypothiocyanate, sulfonium, S-methylmethionine, thiocarbonate, thiocyanate, thiophosphate, thiosilicate, or trimethylsulfonium, or combinations thereof.

[0027] In some embodiments, the catalyst comprises a basic volatile catalyst. For example, in one embodiment, the basic volatile catalyst comprises ammonium carbonate, ammonium bicarbonate, ammonium acetate, ammonium hydroxide, or combinations thereof. In a further embodiment, the basic volatile catalyst is ammonium carbonate. In yet another further embodiment, the basic volatile catalyst is ammonium acetate.

[0028] In other embodiments, the method includes blending with an acid. In some embodiments, the acid is a solid at room temperature and pressure. In some embodiments, the acid is a liquid at room temperature and pressure. In some embodiments, the acid is a liquid at room temperature and pressure that does not provide solubility for one or more other polymer precursors.

[0029] In one embodiment, spherical polydivinylbenzene spheres are produced by precipitation polymerization, pyrolysis, and activation using the methods described herein.

[0030] In one embodiment, porous carbon can be prepared by pyrolyzing a fluoropolymer (e.g., polyvinylidene fluoride) by heating the material to 600°C in a horizontal tube furnace under a flow of inert gas (e.g., nitrogen). The material is allowed to cool for 30 minutes before being removed from the furnace, and then cooled to room temperature. The resulting carbonized material is attrified to a particle size distribution of less than 25 micrometers and used to prepare electrodes. The porous carbon prepared by this method is fluorine-rich, which facilitates the formation of lithium fluoride in the initial stages of the electrochemical plating of lithium metal in lithium-ion batteries, thereby increasing lithiophilicity and reducing harmful dendrite growth in the battery.

[0031] In some embodiments, the polymer precursor components are blended together and subsequently held at a time and temperature sufficient to achieve polymerization. One or more of the polymer precursor components may have a particle size of less than about 20 mm, for example less than 10 mm, less than 7 mm, less than 5 mm, less than 2 mm, less than 1 mm, less than 100 micrometers, or less than 10 micrometers. In some embodiments, the particle size of one or more of the polymer precursor components is reduced during the blending process.

[0032] The blending of one or more polymer precursor components in the absence of a solvent can be achieved by methods described in the art, such as ball milling, jet milling, Fritsch milling, planetary stirring, and other blending methods for mixing or blending solid particles while controlling process conditions (e.g., temperature). The mixing or blending process can be carried out before, during, and / or after incubation at the reaction temperature (or a combination thereof).

[0033] The reaction parameters include aging the blended mixture at temperatures and times sufficient to cause the one or more polymer precursors to react with each other and form a polymer. In this regard, suitable aging temperatures are from about room temperature to temperatures at or near the melting points of one or more of the polymer precursors. In some embodiments, suitable aging temperatures are from about room temperature to temperatures at or near the glass transition temperatures of one or more of the polymer precursors. For example, in some embodiments, the solvent-free mixture is aged at temperatures from about 20°C to about 600°C, for example, from about 20°C to about 500°C, for example, from about 20°C to about 400°C, for example, from about 20°C to about 300°C, for example, from about 20°C to about 200°C. In some embodiments, the solvent-free mixture is aged at temperatures from about 50°C to about 250°C.

[0034] The reaction duration is typically sufficient to allow the polymer precursors to react and form a polymer; for example, depending on the desired outcome, the mixture may be aged from 1 hour to 48 hours or longer or shorter. Typical embodiments include aging periods of approximately 2 hours to approximately 48 hours; for example, in some embodiments, aging includes approximately 12 hours, and in other embodiments, aging includes approximately 4 hours to 8 hours (e.g., approximately 6 hours).

[0035] In some embodiments, for example, an electrochemical modifier is added during the polymerization process described above via the chemical vapor infiltration system 26. For example, in some embodiments, the electrochemical modifier in the form of metal particles, metal paste, metal salt, metal oxide, or molten metal may be dissolved or suspended in the mixture, from which a gel resin is produced.

[0036] Exemplary electrochemical modifiers used to generate composite materials may fall into one or more chemical classifications. In some embodiments, the electrochemical modifier is a lithium salt, such as, but not limited to, lithium fluoride, lithium chloride, lithium carbonate, lithium hydroxide, lithium benzoate, lithium bromide, lithium formate, lithium hexafluorophosphate, lithium iodate, lithium iodide, lithium perchlorate, lithium phosphate, lithium sulfate, lithium tetraborate, lithium tetrafluoroborate, and combinations thereof.

[0037] In some embodiments, the electrochemical modifier comprises a metal, and exemplary substances include, but are not limited to, aluminum isopropoxide, manganese acetate, nickel acetate, ferric acetate, tin chloride, silicon chloride, and combinations thereof. In some embodiments, the electrochemical modifier is a phosphate compound, including but not limited to phytic acid, phosphoric acid, ammonium dihydrogen phosphate, and combinations thereof. In some embodiments, the electrochemical modifier comprises silicon, and exemplary substances include, but are not limited to, silicon powder, silicon nanotubes, polycrystalline silicon, nanocrystalline silicon, amorphous silicon, porous silicon, nanoscale silicon, nanocharacterized silicon, nanoscale and nanocharacterized silicon, silylene, and black silicon, and combinations thereof.

[0038] Electrochemical modifiers can be combined with various polymer systems through physical stirring or chemical reactions with potential (or secondary) polymer functional groups. Examples of potential polymer functional groups include, but are not limited to, epoxide groups, unsaturated bonds (double and triple bonds), acid groups, alcohol groups, amine groups, and basic groups. Crosslinking with potential functional groups can occur via: heteroatoms (e.g., sulfidation with sulfur, acid / base / ring-opening reactions with phosphoric acid), reactions with organic acids or bases (as described above), coordination with transition metals (including but not limited to Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Zr, Nb, Mo, Ag, Au), ring-opening or ring-closing reactions (rotaxanes, spirocyclic compounds, etc.).

[0039] Electrochemical modifiers can also be added to polymer systems through physical blending. Physical blending can include, but is not limited to, melt blending of polymers and / or copolymers, including discrete particles, chemical vapor deposition electrochemical modifiers, and co-precipitation of electrochemical modifiers and main polymer materials.

[0040] In some cases, the electrochemical modifier can be added via a metal salt solid, solution, or suspension. The metal salt solid, solution, or suspension may contain acids and / or alcohols to improve the solubility of the metal salt. In yet another variation, the polymer gel (before or after an optional drying step) is contacted with a paste containing the electrochemical modifier. In yet another variation, the polymer gel (before or after an optional drying step) is contacted with a metal or metal oxide sol containing the desired electrochemical modifier.

[0041] In addition to the electrochemical modifiers exemplified above, the composite material may contain one or more other forms of carbon (i.e., allotropes). In this regard, it has been found effective to incorporate different allotropes of carbon (e.g., graphite, amorphous carbon, conductive carbon, carbon black, diamond, C60, carbon nanotubes (e.g., single-walled and / or multi-walled), graphene, and / or carbon fibers) into the composite material for optimizing its electrochemical properties. Various allotropes of carbon may be incorporated into the carbon material during any stage of the preparation methods described herein. For example, during the solution stage, during the gelation stage, during the curing stage, during the pyrolysis stage, during the milling stage, or after milling. In some embodiments, a second carbon form is incorporated into the composite material by adding a second carbon form before or during the polymerization of the polymer gel as described in more detail herein. The polymer gel containing the second carbon form is then treated according to the general techniques described herein to obtain a carbon material containing a second allotrope of carbon.

[0042] In some embodiments, the polymer precursor is polyethylene benzene spheres produced by precipitation polymerization. In other embodiments, the polymer precursor in the low-solvent or substantially solvent-free reaction mixture is a urea- or amine-containing compound. For example, in some embodiments, the polymer precursor is urea, melamine, hexamethylenetetramine (HMT), or combinations thereof. Other embodiments include polymer precursors selected from isocyanates or other activated carbonyl compounds (e.g., acyl halides).

[0043] Some embodiments of the disclosed method involve preparing low-solvent or solvent-free polymer gels (and carbon materials) containing an electrochemical modifier. Such electrochemical modifiers include, but are not limited to, nitrogen, silicon, and sulfur. In other embodiments, the electrochemical modifier includes fluorine, iron, tin, silicon, nickel, aluminum, zinc, or manganese. The electrochemical modifier may be included at any step of the preparation process. For example, in some cases, the electrochemical modifier is mixed with a mixture, a polymer phase, or a continuous phase.

[0044] As described above, porous carbon materials can be achieved through the pyrolysis of polymers generated from precursor materials. In some embodiments, the porous carbon material comprises amorphous activated carbon produced by pyrolysis, physical or chemical activation, or a combination thereof, in a single process step or a sequence of process steps.

[0045] The pyrolysis temperature and residence time can be varied; for example, the residence time can be 1 minute to 10 minutes, 10 minutes to 30 minutes, 30 minutes to 1 hour, 1 hour to 2 hours, 2 hours to 4 hours, or 4 hours to 24 hours. The temperature can also be varied; for example, the pyrolysis temperature can be 200°C to 300°C, 250°C to 350°C, 350°C to 450°C, 450°C to 550°C, 540°C to 650°C, 650°C to 750°C, 750°C to 850°C, 850°C to 950°C, 950°C to 1050°C, 1050°C to 1150°C, or 1150°C to 1250°C. In some embodiments, the pyrolysis temperature is 650°C to 1100°C. Pyrolysis can be carried out in an inert gas (e.g., nitrogen or argon).

[0046] In some embodiments, alternative gases are used to further activate the carbon. In some embodiments, pyrolysis is combined with activation. Suitable gases for achieving carbon activation include, but are not limited to, carbon dioxide, carbon monoxide, water (steam), air, oxygen, and further combinations thereof. The activation temperature and residence time can vary; for example, the residence time can be 1 minute to 10 minutes, 10 minutes to 30 minutes, 30 minutes to 1 hour, 1 hour to 2 hours, 2 hours to 4 hours, or 4 hours to 24 hours. The temperature can vary; for example, the pyrolysis temperature can be 200°C to 300°C, 250°C to 350°C, 350°C to 450°C, 450°C to 550°C, 540°C to 650°C, 650°C to 750°C, 750°C to 850°C, 850°C to 950°C, 950°C to 1050°C, 1050°C to 1150°C, or 1150°C to 1250°C. In some implementations, the temperature for pyrolysis and activation of the combination is 650°C to 1100°C.

[0047] In some embodiments, combined pyrolysis and activation are performed to prepare porous carbon scaffolds. In such embodiments, the process gas can remain the same during processing, or the composition of the process gas can vary during processing. In some embodiments, after sufficient temperature and time have allowed for the pyrolysis of the solid carbon precursor, an activation gas such as CO2, steam, or a combination thereof is added to the process gas.

[0048] Suitable gases for carbon activation include, but are not limited to, carbon dioxide, carbon monoxide, water (steam), air, oxygen, and further combinations thereof. The activation temperature and residence time can vary; for example, the residence time can be 1 to 10 minutes, 10 to 30 minutes, 30 minutes to 1 hour, 1 hour to 2 hours, 2 hours to 4 hours, or 4 hours to 24 hours. The temperature can vary; for example, the pyrolysis temperature can be 200°C to 300°C, 250°C to 350°C, 350°C to 450°C, 450°C to 550°C, 540°C to 650°C, 650°C to 750°C, 750°C to 850°C, 850°C to 950°C, 950°C to 1050°C, 1050°C to 1150°C, or 1150°C to 1250°C. In some embodiments, the activation temperature is 650°C to 1100°C.

[0049] Carbon particle size reduction can be performed before pyrolysis and / or after pyrolysis and / or after activation. Particle size reduction can be achieved by various techniques known in the art, such as jet milling in the presence of various gases, including air, nitrogen, argon, helium, supercritical steam, and other gases known in the art. Other particle size reduction methods are also envisioned, such as grinding, ball milling, jet milling, water jet milling, and other methods known in the art.

[0050] Porous carbon scaffolds can be in the form of particles. Particle size and particle size distribution can be measured using various techniques known in the art and can be described based on fractional volume. In this respect, the Dv,50 of the carbon scaffold can be 10 nm to 10 mm, for example 100 nm to 1 mm, for example 1 μm to 100 μm, for example 2 μm to 50 μm, for example 3 μm to 30 μm, for example 4 μm to 20 μm, for example 5 μm to 10 μm. In some embodiments, Dv,50 is less than 1 mm, for example less than 100 μm, for example less than 50 μm, for example less than 30 μm, for example less than 20 μm, for example less than 10 μm, for example less than 8 μm, for example less than 5 μm, for example less than 3 μm, for example less than 1 μm. In some embodiments, Dv,100 is less than 1 mm, for example, less than 100 μm, for example, less than 50 μm, for example, less than 30 μm, for example, less than 20 μm, for example, less than 10 μm, for example, less than 8 μm, for example, less than 5 μm, for example, less than 3 μm, for example, less than 1 μm. In some embodiments, Dv,99 is less than 1 mm, for example, less than 100 μm, for example, less than 50 μm, for example, less than 30 μm, for example, less than 20 μm, for example, less than 10 μm, for example, less than 8 μm, for example, less than 5 μm, for example, less than 3 μm, for example, less than 1 μm. In some embodiments, Dv,90 is less than 1 mm, for example, less than 100 μm, for example, less than 50 μm, for example, less than 30 μm, for example, less than 20 μm, for example, less than 10 μm, for example, less than 8 μm, for example, less than 5 μm, for example, less than 3 μm, for example, less than 1 μm. In some embodiments, Dv,0 is greater than 10 nm, for example, greater than 100 nm, for example, greater than 500 nm, for example, greater than 1 μm, for example, greater than 2 μm, for example, greater than 5 μm, for example, greater than 10 μm. In some embodiments, Dv,1 is greater than 10 nm, for example, greater than 100 nm, for example, greater than 500 nm, for example, greater than 1 μm, for example, greater than 2 μm, for example, greater than 5 μm, for example, greater than 10 μm. In some embodiments, Dv,10 is greater than 10 nm, for example, greater than 100 nm, for example, greater than 500 nm, for example, greater than 1 μm, for example, greater than 2 μm, for example, greater than 5 μm, for example, greater than 10 μm.

[0051] In some implementations, the surface area of ​​the porous carbon scaffold may include greater than 400 m². 2 / g surface area, for example, greater than 500 m 2 / g, for example, greater than 750 m 2 / g, for example, greater than 1000 m 2 / g, for example, greater than 1250 m2 / g, for example, greater than 1500m 2 / g, for example, greater than 1750 m 2 / g, for example, greater than 2000 m 2 / g, for example, greater than 2500 m 2 / g, for example, greater than 3000 m 2 / g. In other embodiments, the surface area of ​​the porous carbon scaffold can be less than 500 m². 2 / g. In some embodiments, the surface area of ​​the porous carbon scaffold is 200 m². 2 / g to 500 m 2 / g. In some embodiments, the surface area of ​​the porous carbon scaffold is 100 m². 2 / g to 200 m 2 / g. In some embodiments, the surface area of ​​the porous carbon scaffold is 50 m². 2 / g to 100 m 2 / g. In some embodiments, the surface area of ​​the porous carbon scaffold is 10 m². 2 / g to 50 m 2 / g. In some embodiments, the surface area of ​​the porous carbon scaffold can be less than 10 m². 2 / g.

[0052] In some implementations, the pore volume of the porous carbon scaffold is greater than 0.4 cm³. 3 / g, for example, greater than 0.5 cm 3 / g, for example, greater than 0.6 cm 3 / g, for example, greater than 0.7 cm 3 / g, for example, greater than 0.8 cm 3 / g, for example, greater than 0.9 cm 3 / g, for example, greater than 1.0 cm 3 / g, for example, greater than 1.1 cm 3 / g, for example, greater than 1.2 cm 3 / g, for example, greater than 1.4 cm 3 / g, for example, greater than 1.6cm 3 / g, for example, greater than 1.8 cm 3 / g. For example, greater than 2.0 cm 3 / g. In other embodiments, the pore volume of the porous carbon scaffold is less than 0.5 cm³. 3 For example, 0.1 cm 3 / g to 0.5 cm 3 / g. In some other embodiments, the pore volume of the porous carbon scaffold is 0.01 cm³. 3 / g to 0.1 cm 3 / g.

[0053] In some other embodiments, the porous carbon scaffold has a diameter of 0.2 cm. 3 / g to 2.0 cm 3 Amorphous activated carbon with a pore volume of / g. In some embodiments, the carbon is 0.4 cm². 3 / g to 1.5 cm 3 Amorphous activated carbon with a pore volume of / g. In some embodiments, the carbon is 0.5 cm². 3 / g to 1.2 cm 3 Amorphous activated carbon with a pore volume of / g. In some embodiments, the carbon is 0.6 cm⁻¹. 3 / g to 1.0 cm 3 Amorphous activated carbon with a pore volume of / g.

[0054] In some other embodiments, the porous carbon scaffold comprises less than 1.0 g / cm³. 3 The tap density, for example, is less than 0.8 g / cm³. 3 For example, less than 0.6 g / cm³ 3 For example, less than 0.5 g / cm³ 3 For example, less than 0.4 g / cm³ 3 For example, less than 0.3 g / cm³ 3 For example, less than 0.2 g / cm³ 3 For example, less than 0.1 g / cm³ 3 .

[0055] The surface functional groups of porous carbon scaffolds can vary. One property that can be predicted for surface functional groups is the pH of the porous carbon scaffold. Currently disclosed porous carbon scaffolds include pH values ​​from less than 1 to about 14, for example, less than 5, 5 to 8, or greater than 8. In some embodiments, the pH of the porous carbon is less than 4, less than 3, less than 2, or even less than 1. In other embodiments, the pH of the porous carbon is about 5 to 6, about 6 to 7, about 7 to 8, or 8 to 9, or 9 to 10. In other embodiments, the pH is high, and the pH of the porous carbon is greater than 8, greater than 9, greater than 10, greater than 11, greater than 12, or even greater than 13.

[0056] The pore volume distribution of the porous carbon scaffold can vary. For example, the percentage of micropores can include less than 30%, such as less than 20%, such as less than 10%, such as less than 5%, such as less than 4%, such as less than 3%, such as less than 2%, such as less than 1%, such as less than 0.5%, such as less than 0.2%, such as less than 0.1%. In some embodiments, there is no detectable micropore volume in the porous carbon scaffold.

[0057] The mesopores constituting the porous carbon scaffold can vary. For example, the percentage of mesopores can include less than 30%, such as less than 20%, such as less than 10%, such as less than 5%, such as less than 4%, such as less than 3%, such as less than 2%, such as less than 1%, such as less than 0.5%, such as less than 0.2%, such as less than 0.1%. In some embodiments, there is no detectable mesopore volume in the porous carbon scaffold.

[0058] In some embodiments, the pore volume distribution of the porous carbon scaffold includes more than 50% macropores, such as more than 60% macropores, such as more than 70% macropores, such as more than 80% macropores, such as more than 90% macropores, such as more than 95% macropores, such as more than 98% macropores, such as more than 99% macropores, such as more than 99.5% macropores, such as more than 99.9% macropores.

[0059] In some preferred embodiments, the pore volume of the porous carbon scaffold comprises a mixture of micropores, mesopores, and macropores. Therefore, in some embodiments, the porous carbon scaffold comprises 0% to 20% micropores, 30% to 70% mesopores, and less than 10% macropores. In some other embodiments, the porous carbon scaffold comprises 0% to 20% micropores, 0% to 20% mesopores, and 70% to 95% macropores. In some other embodiments, the porous carbon scaffold comprises 20% to 50% micropores, 50% to 80% mesopores, and 0% to 10% macropores. In some other embodiments, the porous carbon scaffold comprises 40% to 60% micropores, 40% to 60% mesopores, and 0% to 10% macropores. In some other embodiments, the porous carbon scaffold comprises 80% to 95% micropores, 0% to 10% mesopores, and 0% to 10% macropores. In some other embodiments, the porous carbon scaffold comprises 0% to 10% micropores, 30% to 50% mesopores, and 50% to 70% macropores. In some other embodiments, the porous carbon scaffold comprises 0% to 10% micropores, 70% to 80% mesopores, and 0% to 20% macropores. In some other embodiments, the porous carbon scaffold comprises 0% to 20% micropores, 70% to 95% mesopores, and 0% to 10% macropores. In some other embodiments, the porous carbon scaffold comprises 0% to 10% micropores, 70% to 95% mesopores, and 0% to 20% macropores.

[0060] In some embodiments, the percentage of pore volume representing pores from 100 Å to 1000 Å (10 nm to 100 nm) in the porous carbon scaffold includes greater than 30% of the total pore volume, for example, greater than 40% of the total pore volume, for example, greater than 50% of the total pore volume, for example, greater than 60% of the total pore volume, for example, greater than 70% of the total pore volume, for example, greater than 80% of the total pore volume, for example, greater than 90% of the total pore volume, for example, greater than 95% of the total pore volume, for example, greater than 98% of the total pore volume, for example, greater than 99% of the total pore volume, for example, greater than 99.5% of the total pore volume, for example, greater than 99.9% of the total pore volume.

[0061] In some embodiments, the pycnometry density of the porous carbon scaffold is from about 1 g / cc to about 3 g / cc, for example, from about 1.5 g / cc to about 2.3 g / cc. In other embodiments, the framework density is from about 1.5 cc / g to about 1.6 cc / g, from about 1.6 cc / g to about 1.7 cc / g, from about 1.7 cc / g to about 1.8 cc / g, from about 1.8 cc / g to about 1.9 cc / g, from about 1.9 cc / g to about 2.0 cc / g, from about 2.0 cc / g to about 2.1 cc / g, from about 2.1 cc / g to about 2.2 cc / g, or from about 2.2 cc / g to about 2.3 cc / g, from about 2.3 cc / g to about 2.4 cc / g, for example, from about 2.4 cc / g to about 2.5 cc / g.

[0062] In some embodiments, the pore volume distribution of the carbon support can be described as the number or volume distribution of pores as determined by gas adsorption analysis (e.g., nitrogen adsorption analysis) as known in the art. In some embodiments, the pore size distribution can be represented by the pore size at or below a certain percentage of the total pore volume. For example, 10% of the pores at or below a certain pore size can be represented as DPv10.

[0063] The DPv10 used for porous carbon scaffolds can vary, for example, DPv10 can be 0.01 nm to 100 nm, for example 0.1 nm to 100 nm, for example 1 nm to 100 nm, for example 1 nm to 50 nm, for example 1 nm to 40 nm, for example 1 nm to 30 nm, for example 1 nm to 10 nm, for example 1 nm to 5 nm.

[0064] The DPv50 of the porous carbon scaffold can vary; for example, DPv50 can be 0.01 nm to 100 nm, such as 0.1 nm to 100 nm, such as 1 nm to 100 nm, such as 1 nm to 50 nm, such as 1 nm to 40 nm, such as 1 nm to 30 nm, such as 1 nm to 10 nm, such as 1 nm to 5 nm. In other embodiments, DPv50 is 2 to 100, such as 2 to 50, such as 2 to 30, such as 2 to 20, such as 2 to 15, such as 2 to 10.

[0065] The DPv90 of the porous carbon scaffold can vary; for example, DPv90 can be between 0.01 nm and 100 nm, such as 0.1 nm to 100 nm, 1 nm to 100 nm, 1 nm to 50 nm, 1 nm to 50 nm, 1 nm to 40 nm, 1 nm to 30 nm, 1 nm to 10 nm, or 1 nm to 5 nm. In other embodiments, DPv50 is 2 nm to 100 nm, such as 2 nm to 50 nm, 2 nm to 30 nm, 2 nm to 20 nm, 2 nm to 15 nm, or 2 nm to 10 nm.

[0066] In some embodiments, DPv90 is less than 100 nm, for example less than 50 nm, for example less than 40 nm, for example less than 30 nm, for example less than 20 nm, for example less than 15 nm, for example less than 10 nm. In some embodiments, the carbon scaffold includes a pore volume having greater than 70% micropores and DPv90 less than 100 nm, for example less than 50 nm, for example less than 40 nm, for example less than 30 nm, for example less than 20 nm, for example less than 15 nm, for example less than 10 nm, for example less than 5 nm, for example less than 4 nm, for example less than 3 nm. In other embodiments, the carbon scaffold includes a pore volume having a micropore content greater than 80% and a DPv90 less than 100 nm, for example, DPv90 less than 50 nm, for example, DPv90 less than 40 nm, for example, DPv90 less than 30 nm, for example, DPv90 less than 20 nm, for example, DPv90 less than 15 nm, for example, DPv90 less than 10 nm, for example, DPv90 less than 5 nm, for example, DPv90 less than 4 nm, for example, DPv90 less than 3 nm.

[0067] The DPv99 of the porous carbon scaffold can vary; for example, DPv99 can be 0.01 nm to 1000 nm, such as 0.1 nm to 1000 nm, such as 1 nm to 500 nm, such as 1 nm to 200 nm, such as 1 nm to 150 nm, such as 1 nm to 100 nm, such as 1 nm to 50 nm, such as 1 nm to 20 nm. In other embodiments, DPv99 is 2 nm to 500 nm, such as 2 nm to 200 nm, such as 2 nm to 150 nm, such as 2 nm to 100 nm, such as 2 nm to 50 nm, such as 2 nm to 20 nm, such as 2 nm to 15 nm, such as 2 nm to 10 nm.

[0068] In some embodiments, the carbon scaffold is modified prior to lithium impregnation. For example, in some embodiments, the carbon pores are surface-functionalized to create a more lithium-friendly surface, i.e., a surface that preferentially interacts with lithium or lithium-containing precursor materials, wherein the preferential interaction can manifest as preferential diffusion, deposition, adsorption, etc.

[0069] In some embodiments, metal oxides are used to functionalize porous carbon and improve its lithiophilicity, thereby improving the SEI stability of the lithium metal anode. In this embodiment, the porous carbon scaffold is modified with zinc oxide via a hydrothermal sol-gel synthesis reaction. Zinc acetate dihydrate is dissolved in water and stirred together with micronized porous carbon powder. A strong oxidizing agent such as NaOH is then added dropwise to the reaction solution and the reaction is allowed to proceed for up to 2 hours, followed by separation by filtration and drying. In some embodiments, the metal oxide may be aluminum oxide, nickel oxide, manganese oxide, cobalt oxide, tin oxide, or titanium oxide.

[0070] In a further embodiment, the metal oxide is deposited onto the porous carbon surface via atomic layer deposition or physical vapor deposition, and then converted into a metal oxide through a chemical or thermal oxidation reaction. In a further embodiment, the porous carbon can be coated with a lithium-containing polymer.

[0071] C. Introducing silicon into scaffold materials to create composite materials

[0072] In conventional electrodes, nanoscale silicon is difficult to handle and process. Due to its high surface area and tendency to agglomerate, uniform dispersion and coating require special procedures and / or binder systems. To truly become a direct replacement for existing graphite anode materials, next-generation Si-C materials need to be micrometer-sized. In a preferred embodiment, the size distribution of the composite is relatively uniform, with upper and lower limits within preferred ranges, such as Dv,10 not less than 5 nm, Dv,50 from 500 nm to 5 μm, and Dv,90 not greater than 50 μm. In some embodiments, the composite particles comprise the following size distribution: Dv,10 not less than 50 nm, Dv,50 from 1 μm to 10 μm, and Dv,90 not greater than 30 μm. In some other embodiments, the composite particles comprise the following size distribution: Dv,10 not less than 100 nm, Dv,50 from 2 μm to 8 μm, and Dv,90 not greater than 20 μm. In some further embodiments, the composite particles comprise the following size distributions: DV,10 of not less than 250 nm, Dv,50 of 4 μm to 6 μm, and Dv,90 of not more than 15 μm.

[0073] Unlike existing composite materials that embed silicon within a large amount of inactive material, it should be understood that silicon requires space to expand and contract for optimal performance. In some embodiments, high-pore-volume carbon is used as a porous scaffold in which silicon is embedded or deposited, engineered to fill the desired range of pore volumes to produce impregnated carbon materials of the desired size range. Therefore, the scaffold (e.g., porous carbon material) plays a crucial role as a framework and in-situ control for the expansion and contraction of the material, as well as for promoting the overall electronic and ionic conductivity of the composite particles. This scaffold structure allows for the movement of electrons and ions. The primary function of the scaffold is to act as a framework that holds silicon to a single location and volume, allowing silicon to expand and contract outward while remaining within the pores of the carbon scaffold material.

[0074] In some implementations, by Figure 1The chemical vapor infiltration system 26 introduces silicon into porous carbon via nanoparticle impregnation. Thus, nano-sized or nano-sized and nano-characterized silicon is first produced. In a preferred embodiment, the nano-sized and nano-characterized silicon (alone or collectively, "nanosilicon") is produced according to the methods described in U.S. Patent No. 10,147,950, "Materials With Extremely Durable Intercalation Of Lithium And Manufacturing Methods Thereof," and / or U.S. Patent No. 11,611,073, "Composites of Porous Nano-Featured Silicon Materials and Carbon Materials," the entire disclosure of which is incorporated herein by reference for all purposes.

[0075] Porous carbon can be mixed with nano-silicon, for example, in a stirred reactor vessel, where carbon particles, such as micron-sized porous carbon particles, are co-suspended with nano-silicon of the desired particle size. As is known in the art, the suspension environment can vary, for example, it can be aqueous or non-aqueous. In some embodiments, the suspension fluid can be multi-component, containing miscible or immiscible co-solvents. Suitable co-solvents for aqueous (water) environments include, but are not limited to, acetone, ethanol, methanol, and other co-solvents known in the art. A variety of non-aqueous environments are also known in the art, including, but not limited to, heptane, hexane, cyclohexane, oils such as mineral oils, vegetable oils, etc. Without being bound by theory, mixing within the reactor vessel allows silicon nanoparticles to diffuse within the porous carbon particles. The resulting nano-silicon-impregnated carbon particles can then be collected, for example, by centrifugation, filtration, and subsequent drying, all as is known in the art.

[0076] For this purpose, porous carbon particles with a desired degree and type of pores are processed, resulting in the formation of silicon within the pores. For this processing, the porous carbon particles can first be reduced in size, for example to provide a Dv,50 of 1 micrometer to 1000 micrometers, for example 1 micrometer to 100 micrometers, for example 1 micrometer to 50 micrometers, for example 1 micrometer to 20 micrometers, for example 1 micrometer to 15 micrometers, for example 2 micrometers to 12 micrometers, for example 5 micrometers to 10 micrometers. Particle size reduction can be carried out as is known in the art and as described elsewhere herein, for example by jet milling.

[0077] In a preferred embodiment, silicon is deposited within the pores of porous carbon by subjecting porous carbon particles to a silane gas at an elevated temperature in the presence of the gas, thereby achieving silicon deposition via chemical vapor deposition (CVD). The silane gas can be mixed with other inert gases (e.g., nitrogen). The processing temperature and time can vary, for example, the temperature can be 300°C to 400°C, 400°C to 500°C, 500°C to 600°C, 600°C to 700°C, 700°C to 800°C, or 800°C to 900°C. The gas mixture can contain 0.1% to 1% silane and the remainder inert gas. Alternatively, the gas mixture can contain 1% to 10% silane and the remainder inert gas. Alternatively, the gas mixture can contain 10% to 20% silane and the remainder inert gas. Alternatively, the gas mixture can contain 20% to 50% silane and the remainder inert gas. Alternatively, the gas mixture may contain more than 50% silane and the remainder inert gas. Alternatively, the gas may be substantially 100% silane gas. The reactor for the CVD process is based on various designs known in the art, such as fluidized bed reactors, static bed reactors, lift kilns, rotary kilns, box kilns, or other suitable reactor types. As known in the art, the reactor materials are suitable for this task. In a preferred embodiment, the porous carbon particles are processed under conditions that provide uniform contact with the gas phase, for example, in a reactor where the porous carbon particles are fluidized or otherwise agitated to provide said uniform gas contact.

[0078] In some embodiments, the CVD process is a plasma-enhanced chemical vapor deposition (PECVD) process. This process is known in the art for its use in depositing thin films from a gaseous (vapor) state to a solid state on a substrate. The process involves a chemical reaction that occurs after the generation of a plasma of reactive gases. The plasma is typically generated by an RF (AC) frequency or DC discharge between two electrodes, the space between which is filled with reactive gases. In some embodiments, the PECVD process is used to coat porous carbon onto a substrate suitable for this purpose, such as a copper foil substrate. PECVD can be performed at a variety of temperatures, such as 300°C to 800°C, 300°C to 600°C, 300°C to 500°C, 300°C to 400°C, or 350°C. As is known in the art, the power can be varied (e.g., 25 W RF), the required silane gas flow rate can be varied, and the processing time can be varied.

[0079] Regardless of the process, silicon impregnated into porous carbon is envisioned to possess certain properties optimal for its use as an energy storage material. For example, the size and shape of the silicon can be varied accordingly to match the degree and nature of the pore volume within the porous carbon particles, without being bound by theory. For instance, silicon can be impregnated into the pores within porous carbon particles comprising pore sizes from 5 nm to 1000 nm, such as 10 nm to 500 nm, 10 nm to 200 nm, 10 nm to 100 nm, 33 nm to 150 nm, or 20 nm to 100 nm, by deposition using CVD or other suitable processes. Other ranges of carbon pore sizes, whether micropores, mesopores, or macropores, are also envisioned, as described elsewhere in this disclosure.

[0080] The oxygen content in silicon can be less than 50%, for example less than 30%, for example less than 20%, for example less than 15%, for example less than 10%, for example less than 5%, for example less than 1%, for example less than 0.1%. In some embodiments, the oxygen content in silicon is from 1% to 30%. In some embodiments, the oxygen content in silicon is from 1% to 20%. In some embodiments, the oxygen content in silicon is from 1% to 10%. In some embodiments, the oxygen content in porous silicon materials is from 5% to 10%.

[0081] In some embodiments where silicon contains oxygen, oxygen is incorporated such that silicon exists as a mixture of silicon and silicon oxide of the general formula SiOx, where x is a non-integer (real number) that can vary continuously from 0.01 to 2. In some embodiments, the fraction of oxygen present on the surface of nanoporous silicon is higher than that inside the particles.

[0082] In some embodiments, silicon includes crystalline silicon. In some embodiments, silicon includes polycrystalline silicon. In some embodiments, silicon includes micropolycrystalline silicon. In some embodiments, silicon includes nanopolycrystalline silicon. In some other embodiments, silicon includes amorphous silicon. In some other embodiments, silicon includes both crystalline and amorphous silicon.

[0083] In some embodiments, the carbon scaffold to be impregnated with silicon or otherwise embedded may include various carbon allotropes and / or geometries. For this purpose, the carbon scaffold to be impregnated with silicon or otherwise embedded may include graphite, nanographite, graphene, nanographene nanoparticles, conductive carbon (e.g., carbon black), carbon nanowires, carbon nanotubes, and combinations thereof.

[0084] In some embodiments, the carbon scaffold impregnated with silicon or otherwise embedded is removed to produce a template-based silicon material with desired size characteristics. Removal of the scaffold carbon can be achieved, as is known in the art, for example, by thermal activation under conditions in which the silicon does not undergo undesirable changes in its electrochemical properties. Alternatively, if the scaffold is a porous polymer or other material soluble in a suitable solvent, the scaffold can be removed by dissolution.

[0085] D. Dual fine particle removal

[0086] In various implementation schemes, refer to Figure 2 The dual fine particle removal system 24 performs a first fine particle removal and a second fine particle removal. The first fine particle removal includes a particle size reduction device (e.g., a grinder) 42, configured to reduce the size of the porous carbon material received from the porous carbon generation system 22 via a feeder 44. The grinder 42 produces porous carbon particles of acceptable size and particle size distribution. The grinder 42 may also produce fine carbon particles (i.e., carbon dust). In one embodiment, the grinder 42 is a dual-row spiral jet grinder. The top discharge of the jet grinder outputs carbon dust to a dust collector 46. The bottom discharge of the jet grinder outputs (acceptably sized) coarse carbon particles to an ejector (i.e., an ejector T-shaped structure) 48. The ejector 48 includes a port connected to the grinder 42, an inlet port having a fine high-flow filter 50 to prevent debris from contaminating the ground carbon. The injector 48 also includes an outlet port that can be directly connected to the separator 54 of the second fine particle removal assembly or connected to the separator 54 or the mill bag chamber 56 via a diverter 52. The diverter 52 allows for automatic or manual control of the output of carbon particles from the mill 42 to the separator 54 or directly to the mill bag chamber 56.

[0087] In various embodiments, separator 54 also removes particles from the carbon material output from mill 42 that do not meet a predefined particle size standard. Separator 54 is connected to mill bag chamber 56 so that fine carbon particles can be collected in mill bag chamber 56 and coarse particles can be collected separately. Separator 54 may be a cyclone separator or an equivalent device.

[0088] In various implementations, an exhaust device or fan 58 is connected to the injector 48, distributor 52, separator 54, and mill bag chamber 56 to carry low-fine carbon particles from the mill 42 through the injector 48 to the distributor 52, separator 54, and / or mill bag chamber 56. An external fan 58 can pull coarse low-fine carbon particles through the cyclone separator 54 for secondary fine particle removal. The dual fine particle removal system 24 mitigates the difference between the flow of grinding air in the mill 42 and the flow of delivery air through the cyclone separator 54, which allows for complete decoupling of particle size control in the mill 42 from particle separation control in the separator 54, since both devices (42, 54) rely on airflow velocity as a process input.

[0089] In various implementations, the motor of fan 58 is interlocked with the controls of mill 42 such that if fan 58 is turned off, the airflow within mill 42 and the moving components of feeder 44 are shut down. External fan 58 pulls 300 scfm to 700 scfm (standard cubic feet per minute) through ejector 48 and cyclone separator 54 to separate coarse and fine particles.

[0090] In various implementations, the controller 60 sends control signals to the feeder 44, grinder 42, distributor 52 and / or separator 54 based on the status of the fan 58 or input from the user via the user interface device 62.

[0091] Reference Figure 3 Method 80 performs dual fine particle removal. At box 82, method 80 grinds the porous carbon scaffold material to produce porous carbon scaffold particles and fine carbon particles. At box 84, method 80 performs a first separation of the fine carbon particles from the porous carbon scaffold particles. At box 86, method 80 entrains the porous carbon scaffold particles into a separator or grinding mill bag chamber. At box 88, method 80 performs a second separation of the remaining fine carbon particles from the porous carbon scaffold particles.

[0092] Detailed Implementation Plan

[0093] Implementation Scheme 1. A system comprising: a grinder configured to grind a porous carbon scaffold material to produce porous carbon scaffold particles and carbon fine particles, and to separate the porous carbon scaffold particles from the carbon fine particles; a fan configured to carry the porous carbon scaffold particles from the grinder; and a separator configured to receive the carried-in porous carbon scaffold particles and further separate the porous carbon scaffold particles from the remaining carbon fine particles.

[0094] Implementation Scheme 2. The system of the aforementioned implementation scheme, wherein the grinding machine includes a spiral jet grinder.

[0095] Implementation Scheme 3. The system of Implementation Scheme 1, wherein the separator includes a cyclone separator.

[0096] Implementation Scheme 4. The system of the aforementioned implementation scheme further includes a T-shaped connector, the T-shaped connector comprising: an input port connected to the spiral jet mill; an air inlet port; and an exhaust port pneumatically connected to the cyclone separator and the fan.

[0097] Implementation Scheme 5. The system of the aforementioned implementation scheme, wherein the T-joint is an injector T-shaped object.

[0098] Implementation Scheme 6. The system of the aforementioned implementation scheme further includes a diverter connected between the exhaust port of the T-joint and the cyclone separator.

[0099] Implementation Scheme 7. The system of the aforementioned implementation scheme further includes a grinding mill bag chamber connected to the distributor.

[0100] Implementation Scheme 8. The system of the aforementioned implementation scheme, wherein the grinding mill bag chamber is connected to the separator.

[0101] Implementation Scheme 9. The system of the aforementioned implementation scheme further includes a dust collector connected to the first outlet port of the grinding mill.

[0102] Implementation Scheme 10. The system of the aforementioned implementation scheme further includes a controller configured to control the operation of the jet mill, the jet mill feeder, or the separator based on the operating status of the fan.

[0103] Implementation Scheme 11. A method comprising: grinding a porous carbon scaffold material using a dual-emission jet mill to produce porous carbon scaffold particles and fine carbon particles, separating the fine carbon particles from the porous carbon scaffold particles, entraining the porous carbon scaffold particles from the dual-emission jet mill to a separator, and using the separator to separate the remaining fine carbon particles from the entrained porous carbon scaffold particles.

[0104] Implementation Scheme 12. The aforementioned method, wherein the grinding includes spiral jet grinding.

[0105] Implementation Scheme 13. The aforementioned method, wherein separation includes cyclone separation.

[0106] Implementation Scheme 14. The aforementioned method, wherein entrainment includes applying forced air using a fan.

[0107] Implementation Scheme 15. In the aforementioned implementation scheme, the method further includes diverting the entrained porous carbon scaffold particles to prevent them from going to the separator based on the fact that the entrained porous carbon scaffold particles meet at least one predefined requirement.

[0108] Implementation Scheme 16. The method of the aforementioned implementation scheme, wherein the diversion includes diverting the entrained porous carbon support particles to a bagging device.

[0109] Implementation Scheme 17. The method of the aforementioned implementation scheme further includes controlling the operation of the jet mill, the jet mill feeder, or the separator based on the operating status of the fan.

[0110] Implementation Scheme 18. A system comprising: a porous carbon generation system configured to generate a porous carbon scaffold material; a dual fine particle removal system; and a chemical vapor infiltration system configured to permeate the pores of the porous carbon scaffold particles with silicon. The dual fine particle removal system comprises: a grinder configured to grind the porous carbon scaffold material to generate porous carbon scaffold particles and carbon fine particles, and to separate the porous carbon scaffold particles from the carbon fine particles; a fan configured to carry the porous carbon scaffold particles from the grinder; and a separator configured to further separate the porous carbon scaffold particles from the remaining carbon fine particles.

[0111] Implementation Scheme 19. The system of the aforementioned implementation scheme, wherein the grinder includes a spiral jet grinder, the separator includes a cyclone separator, and the dual fine particle removal system further includes: a T-joint connected to the spiral jet grinder, the T-joint having an input port connected to the spiral jet grinder, an air inlet port and an exhaust port pneumatically connected to the cyclone separator and the fan; a diverter connected between the exhaust port of the T-joint and the cyclone separator; and a grinder bag chamber connected to the diverter.

[0112] Implementation Scheme 20. The system of the aforementioned implementation scheme, wherein the dual fine particle removal system further includes a controller configured to control the operation of the spiral jet mill, the jet mill feeder, or the cyclone separator based on the operating status of the fan.

[0113] As can be understood from the above, although this document describes specific embodiments of the present disclosure for illustrative purposes, various modifications may be made without departing from the spirit and scope of the present disclosure.

[0114] The above implementation schemes can be combined to provide further implementation schemes.

[0115] All U.S. patents, U.S. patent application publications, U.S. patent applications, foreign patents, foreign patent applications, and non-patent publications (including U.S. Patent Application No. 63 / 586,508, filed September 29, 2023) mentioned in and / or listed in the application data sheet are incorporated herein by reference in their entirety. If necessary, aspects of the embodiments may be modified to incorporate concepts from various patents, applications, and publications to provide further embodiments.

Claims

1. The system, including: Grinding machine, the grinding machine being configured as follows: Grinding porous carbon scaffold materials to produce porous carbon scaffold particles and carbon fine particles; as well as Separate the porous carbon scaffold particles from the fine carbon particles; A fan configured to carry the porous carbon support particles from the grinder; and A separator configured to receive entrained porous carbon scaffold particles and further separate the porous carbon scaffold particles from the remaining carbon fines.

2. The system of claim 1, wherein the grinding machine comprises a spiral jet grinder.

3. The system of claim 2, wherein the separator comprises a cyclone separator.

4. The system of claim 3, further comprising a T-joint, the T-joint comprising: The input port is connected to the spiral jet mill; Air intake port; and An exhaust port, which is pneumatically connected to the cyclone separator and the fan.

5. The system of claim 4, wherein the T-joint is an injector T-shaped component.

6. The system of claim 4 further includes a diverter connected between the exhaust port of the T-joint and the cyclone separator.

7. The system of claim 6 further includes a grinding chamber connected to the distributor.

8. The system of claim 7, wherein the grinding mill bag chamber is further connected to the separator.

9. The system of claim 1 further includes a dust collector connected to a first outlet port of the grinder.

10. The system of claim 1, further comprising a controller configured to control the operation of the jet mill, the jet mill feeder, or the separator based on the operating state of the fan.

11. Methods, including: A dual-emission jet mill was used to grind porous carbon scaffold materials to produce porous carbon scaffold particles and fine carbon particles. Separate the carbon fine particles from the porous carbon scaffold particles; The porous carbon support particles are carried from the dual-emission jet mill to the separator; as well as The separator is used to separate the remaining carbon particles from the entrained porous carbon scaffold particles.

12. The method of claim 11, wherein the grinding comprises helical jet grinding.

13. The method of claim 12, wherein separation using the separator comprises cyclone separation.

14. The method of claim 13, wherein the entrainment includes applying forced air using a fan.

15. The method of claim 14, further comprising diverting the entrained porous carbon support particles to a separator based on the entrained porous carbon support particles meeting at least one predefined requirement.

16. The method of claim 15, wherein diversion includes diverting the entrained porous carbon support particles to a bagging device.

17. The method of claim 14, further comprising controlling the operation of the jet mill, the jet mill feeder, or the separator based on the operating state of the fan.

18. The system includes: A porous carbon generation system configured to generate porous carbon scaffold materials; Dual fine particle removal system, the dual fine particle removal system comprising: Grinding machine, the grinding machine being configured as follows: Grinding the porous carbon scaffold material to produce porous carbon scaffold particles and fine carbon particles; and Separate the porous carbon scaffold particles from the fine carbon particles; A fan configured to carry the porous carbon support particles from the grinder; and A separator, configured to further separate the porous carbon scaffold particles from the remaining fine carbon particles; and A chemical vapor infiltration system configured to permeate the pores of the porous carbon scaffold particles with silicon.

19. The system of claim 18, wherein: The grinding machine includes a spiral jet grinding machine; The separator includes a cyclone separator; as well as The dual fine particle removal system also includes: A T-joint, wherein the T-joint is connected to the spiral jet mill, and the T-joint comprises: The input port is connected to the spiral jet mill; Intake port; and An exhaust port, which is pneumatically connected to the cyclone separator and the fan; A diverter, the diverter being connected between the exhaust port of the T-joint and the cyclone separator; and A grinding mill bag chamber, which is connected to the distributor.

20. The system of claim 19, wherein the dual fine particle removal system further comprises a controller configured to control the operation of the spiral jet mill, the jet mill feeder, or the cyclone separator based on the operating state of the fan.

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