Metal particles and their preparation method using electrolytic dispersion

Abstract

In one aspect, a method for making metal particles is disclosed, comprising: adding a plurality of metal elements to a plasma reactor containing a circulating fluid and two electrodes; vaporizing the metal elements to form a metal vapor using a plasma generated by at least one discharge pulse between the electrodes; and condensing the metal vapor to form metal particles. In some embodiments, the metal particles comprise metal oxide particles. In some embodiments, the metal particles are useful as part of a pharmaceutical composition or a dietary supplement.

Description

[Technical Field]

[0001] Related Applications This application claims priority to U.S. Provisional Application Serial No. 62 / 881,031, filed July 31, 2019, the contents of which are incorporated herein by reference in their entirety. [Background technology]

[0002] Submicron- and nanometer-sized particles have attracted great interest in many applications due to their unique properties, such as strong absorption, scattering, and magnetic moment, as well as their biological and chemical compatibility. The composition, structure, and size of submicron- and nanometer-sized particles are important characteristics that affect their properties. The preparation methods of submicron- and nanometer-sized particles, which determine their composition, structure, and size, are an important challenge for technological applications.

[0003] To prepare submicron- and nanometer-sized particles, two approaches are commonly used: top-down and bottom-up. In the top-down approach, bulk materials are used as starting materials and then reduced in size by crushing, typically by crushing and grinding. This method has the advantages of versatility, simplicity, and low cost. However, this method typically produces polydisperse particles containing impurities and defects, with a minimum size of approximately 0.8 μm. On the other hand, the bottom-up method creates objects from small building blocks that spontaneously assemble into useful structures. This approach allows for the creation of smaller structures, facilitating tailoring. However, submicron- and nanometer-sized particles produced by this method often require complex and expensive procedures and can be difficult to reproduce and scale up.

[0004] Therefore, better methods for preparing submicron and nanometer-sized particles are needed.

[0005] In some embodiments, a method for producing metal particles is disclosed. In these embodiments, the method can include adding a plurality of metal elements to a plasma reactor including a circulating fluid and two electrodes, evaporating the metal elements to form a metal vapor using a plasma generated by at least one discharge pulse between the electrodes, and condensing the metal vapor to form metal particles. In some embodiments, the method can further include transporting the metal particles to a precipitation tank coupled to the plasma reactor, precipitating the metal particles in the precipitation tank, removing the precipitate from the precipitation tank, sublimating the precipitate, drying the precipitate, and grinding the precipitate.

[0006] In these embodiments and others, the metal particles may be transported to the settling tank by a circulating fluid.

[0007] In some embodiments, the metallic element can be selected from the group consisting of an iron-containing element, an aluminum-containing element, a titanium-containing element, and a tungsten-containing element, or any combination thereof.

[0008] In some embodiments, the circulating fluid may be comprised of water, hydrogen peroxide, or a combination thereof.

[0009] In some embodiments, the metal particles can have a size between 2 nm and 60 μm, or between 2 nm and 30 μm, or between 2 nm and 1 μm.

[0010] In some embodiments, the metal particles can include metal oxide particles.

[0011] In some embodiments, the metal particles can include iron oxide particles, hi these embodiments, the iron oxide particles can absorb microwaves.

[0012] In some embodiments, the metal particles include alumina particles.

[0013] In some embodiments, methods are disclosed for extracting ions of a metal from a liquid sample using the metal particles described above. In these embodiments, the methods can include mixing the metal particles with the liquid sample, reacting the metal particles with the ions, solidifying the reacted metal particles to form a slurry, and filtering the slurry.

[0014] In some embodiments, filtering of the slurry is performed using a filter having a mesh size between 0.1 μm and 25 μm.

[0015] In some embodiments, the degree of extraction of ions from the liquid sample is between 80% and 100%.

[0016] In some embodiments, the metal particles are part of a pharmaceutical composition for oral or intravenous administration, or a dietary supplement, which may include, but is not limited to, a beverage. The prior art documents relevant to the invention of this application are as follows (including documents cited in the international phase after the international filing date and documents cited when the application entered the national phase in other countries). (Prior art document) (Patent document) (Patent Document 1) U.S. Patent Application Publication No. 2013 / 178356 (Patent Document 2) U.S. Patent Application Publication No. 2014 / 255716 (Patent Document 3) International Publication No. 2011 / 155473 (Non-patent literature) (Non-patent document 1) BERND HALBEDEL ET AL, "Iron oxide nanopowder synthesized by electroerosion dispersion (EED) - Properties and potential for microwave applications", CURRENT APPLIED PHYSICS, Vol. 18, No. 11, 10 August 2018 (2018-08-10), page 1410-1414 (Non-patent document 2) MK MONASTYROV, "Electroerosion dispersion-prepared nano- and submicrometre-sized aluminum and alumina powders as power-accumulating substances", NANOTECHNOLOGY PERCEPTIONS, Vol. 4, No. 2, 30 July 2008 (2008-07-30), page 179-187 [Brief explanation of the drawings]

[0017] The present disclosure will be described with reference to the following figures, which are presented for purposes of illustration only and are not intended to be limiting. [Figure 1] FIG. 1A is a flow chart illustrating various steps in an exemplary embodiment for preparing metal particles using an electrolyte dispersion (EED) system according to aspects of the present disclosure. [Figure 2] FIG. 2 is a schematic diagram of a plasma reactor according to an embodiment of the present disclosure. [Figure 3] FIG. 3 is a schematic diagram of an EED system including a generator, a plasma reactor, a settling tank, a circulation pump, and a control system according to an embodiment of the present disclosure. [Figure 4] FIG. 4 is a schematic diagram of a control system of one embodiment of an EED system including a central processing unit (CPU), an interface, a communication port, a storage device, a controller, a read-only memory (ROM), and a random access memory (RAM) in accordance with aspects of the present disclosure. [Figure 5] FIG. 5 is an image showing a laboratory setup for electrolytic dispersion of metal elements according to an embodiment of the present disclosure. [Figure 6A] FIG. 6A is an image showing a top view of an EED plasma reactor for dispersion of Ti and Al in a liquid, according to an embodiment of the present disclosure. [Figure 6B] FIG. 6B is an image depicting EEC particles containing TiC, Ti, and Al according to an embodiment of the present disclosure (scale bar, 90 μm). [Figure 7A] FIG. 7A is an image showing a top view of an EED plasma reactor for the synthesis of iron oxide particles using Fe chips, according to an embodiment of the present disclosure. [Figure 7B] FIG. 7B is a transmission electron microscope (TEM) bright-field image showing aggregates of iron oxide EED particles according to an embodiment of the present disclosure (scale bar, 100 nm). [Figure 7C] FIG. 7C is a TEM bright-field image depicting an aggregate of iron oxide EED particles having primary particles with diameters of about 20 nm to about 50 nm, according to an embodiment of the present disclosure (scale bar, 50 nm). [Figure 7D] FIG. 7D is a scanning electron microscope (SEM) image depicting an aggregate of iron oxide EED particles having primary particles with diameters of about 7 nm to about 8 nm, according to an embodiment of the present disclosure (scale bar, 100 nm). [Figure 8] FIG. 8 is a table showing the density and particle size of iron oxide EED particles according to an embodiment of the present disclosure. [Figure 9]FIG. 9 is a plurality of graphs showing X-ray diffractometer (XRD) diagrams of iron oxide EED particles before microwave heating (dark bottom line) and after microwave heating (thin top line), according to an embodiment of the present disclosure. [Figure 10] FIG. 10 is a set of graphs showing hysteresis curves of iron oxide EED particles before (dark line) and after (dashed line) microwave heating, according to an embodiment of the present disclosure. [Figure 11] FIG. 11 is a table presenting magnetic values ​​of iron oxide EED particles, Fe 3 O 4 (Comparative Example), and Fe (Comparative Example) at room temperature according to an embodiment of the present disclosure. [Figure 12A] FIG. 12A is a plurality of graphs presenting heating curves (Δθ, [K]) over time (t [s]) for iron oxide EED particles (EED powder), Ti-substituted barium hexaferrite powder synthesized by glass crystallization technique (Comparative Example), and Magsilica® (Evonik) (Comparative Example) heated in a 2.45 GHz microwave oven in accordance with an embodiment of the present disclosure. [Figure 12B] FIG. 12B is a plurality of graphs presenting the heating rate (Δθ / Δt, [K]) over time (t [s]) for iron oxide EED particles (EED powder), Ti-substituted barium hexaferrite powder synthesized by glass crystallization technique (Comparative Example), and Magsilica® (Evonik) (Comparative Example) according to an embodiment of the present disclosure. [Figure 13] FIG. 13 is an image depicting crystalline alumina EED particles according to an embodiment of the present disclosure (scale bar, 2 μm). [Figure 14] FIG. 14 is an image depicting amorphous alumina EED particles according to an embodiment of the present disclosure (scale bar, 200 nm). [Figure 15] FIG. 15 is a table presenting results from the extraction of heavy metal ions from galvanic drain liquid samples using iron oxide EED particles, according to an embodiment of the present disclosure. [Figure 16] FIG. 16 is a table presenting results from the purification of contaminated water from electroplating production using amorphous aluminum oxide EED particles, according to an embodiment of the present disclosure. [Figure 17A] FIG. 17A is a histogram of mass distribution of Co EED particles according to an embodiment of the present disclosure. [Figure 17B] FIG. 17B is a histogram of particle mass distribution of a hard-tolerant EED powder according to an embodiment of the present disclosure. [Figure 17C] FIG. 17C is a histogram of particle mass distribution of Ni EED powder according to an embodiment of the present disclosure. [Figure 18A] FIG. 18A is a photograph of a military product made of a tungsten carbide alloy according to an embodiment of the present disclosure. [Figure 18B] FIG. 18B is a photograph of EED powder produced from the military product disclosed in FIG. 18A in accordance with an embodiment of the present disclosure; and [Figure 18C] FIG. 18C is a TEM image of the powder disclosed in FIG. 18B (scale bar, 20 μm), according to an embodiment of the present disclosure. [Figure 19] FIG. 19 is a perspective view of one embodiment of the present disclosure. DETAILED DESCRIPTION OF THE INVENTION

[0018] It will be understood that, for clarity, the following discussion describes various aspects of embodiments of the applicant's teachings while omitting specific details where convenient or appropriate. For example, discussion of like or similar features in alternative embodiments may be somewhat omitted. Well-known ideas or concepts may also be discussed in less detail for the sake of brevity. Those skilled in the art will recognize that some embodiments of the applicant's teachings may not require certain of the specifically described details in every implementation, but these are described herein only to provide a thorough understanding of the embodiments. Similarly, it will be apparent that the described embodiments can be modified or varied in accordance with common general knowledge without departing from the scope of the present disclosure. The following detailed description of the embodiments should not be construed in any way as limiting the scope of the applicant's teachings.

[0019] Various terms are used herein consistent with their common meaning in the art. For clarity, the following terms are defined below.

[0020] As used herein, the term "about" indicates a variation around a numerical value of up to 10%, unless the context dictates otherwise.

[0021] This disclosure relates to powder metallurgy and to a method for producing nanoscale and ultrafine powders of polyvalent iron oxide in aqueous solution. The technical achievements are the automation of the technological process, the improvement of the working and environmental conditions of production, the reduction of energy costs as a cost of the final product, and the possibility of large-scale batch production. The production of nanodispersed polyvalent iron oxide powders can find a wide range of applications in the nano, petroleum, chemical, and electronics industries, as well as in medicine, energy, biology, and agriculture.

[0022] Furthermore, minor process adjustments can alter the spherical shape and morphological characteristics of metal particles, and alter their surface properties to facilitate coating with carbohydrates (e.g., carboxymaltose). Because EED-produced iron particles can be administered through the intestinal wall of humans and animals, similar to Vifor Pharma's FERINJECT®, oral administration may be more effective than iron tablets, potentially eliminating the need for iron tablets in humans. In this way, iron can be absorbed into the bloodstream from the digestive tract. Furthermore, Fe3+ EED-iron may improve iron infusion by enabling the coating of specialized iron nanoparticles with shapes and surface properties that enable novel coating techniques.

[0023] As discussed in more detail below, in some embodiments, submicron- and nanometer-sized particles are produced using an electroerosion dispersion (EED) system that includes: (i) a plasma reactor including two electrodes, a circulating fluid, and a loading port for loading material into the plasma reactor; (ii) a generator connected to the electrodes to provide an electrical discharge to the plasma reactor; (iii) a settling tank in which the produced particles settle; and (iv) a pump connected to the plasma reactor and the settling tank for circulating the fluid. The EED system may also be designed so that the circulating fluid transports the produced particles from the plasma reactor to the settling tank. Submicron- and nanometer-sized particles, e.g., submicron- and nanometer-sized metal oxide particles, can be produced from bulk metal materials using the EED system. Without being limited to a particular theory, in some embodiments, the bulk metal material is heated to a relatively high temperature in the plasma reactor by plasma generated by pulsed discharges. This results in the bulk material vaporizing and then condensing into microdroplets in a cooler region of the plasma reactor. In an oxygen-containing medium (e.g., water), the condensed droplets can be oxidized by oxygen to form metal oxide particles. In certain embodiments, the oxygen is generated by a plasma resulting from the decomposition of water. Under non-equilibrium conditions caused by short electrical discharges, metal and metal oxide particles with different compositions, oxidation states, and sizes can be produced.

[0024] In some cases, the stoichiometry of the produced particles depends on the characteristics of the raw materials (i.e., composition, chips, shavings, granules, impurities, etc.) and the characteristics of the circulating fluid (i.e., composition, temperature, flow rate, etc.), as well as the stoichiometry of the electrode material. By varying the above factors and controlling the discharge parameters (e.g., voltage, discharge frequency, pulse shape, etc.), it is possible to determine the characteristics of the produced particles, such as their composition, size (from a few nanometers to a few microns), shape (spherical, highly surface-developed, etc.), and phase (amorphous, glassy, ​​crystalline, etc.). Varying the type and composition of the circulating fluid (e.g., water, distilled water, kerosene, etc.) with appropriate additive amounts offers the possibility of synthesizing pure metals, oxides, carbides, and nitrides. The methods disclosed herein can produce particles suitable for the production of materials with unique properties (e.g., refractoriness, hardness, ductility, brittleness, radioactivity, chemical activity, magnetic properties, and adsorption capacity).

[0025] In some embodiments, the raw material is in the form of granules, shavings, regularly shaped particles, or irregularly shaped particles. The raw material can be one or more of iron, cast iron, or steel. In other embodiments, the raw material is iron ore. Examples of iron ore include, but are not limited to, one or more of magnetite, hematite, goethite, limonite, or siderite.

[0026] In some embodiments, the circulating fluid can have a temperature of at least 20°C, or at least 25°C, or at least 30°C, or at least 40°C, or at least 50°C, or at least 60°C, or at least 70°C, or at least 80°C, or at least 90°C. In some embodiments, the circulating fluid can be circulated through the plasma reactor during particle production. In some embodiments, the circulating fluid can be stopped circulating during particle production. In some embodiments, the circulating fluid can have a flow rate of between about 0.01 liters / minute and about 60 liters / minute, or between about 0.1 liters / minute and about 40 liters / minute, or between about 1 liter / minute and about 20 liters / minute, or between about 2 liters / minute and about 10 liters / minute, or between about 2 liters / minute and about 5 liters / minute, or between about 2 liters / minute and about 3 liters / minute, etc. In some embodiments, the circulating fluid can have a flow rate of at least 0.01 liters / minute, or at least 0.1 liters / minute, or at least 1 liter / minute, or at least 2 liters / minute, or at least 3 liters / minute, or at least 5 liters / minute, or at least 10 liters / minute, or at least 20 liters / minute, or at least 40 liters / minute, or at least 60 liters / minute.

[0027] In some embodiments, the prepared EED particles are about 2 nm to about 60 μm in size, or about 2 nm to about 30 μm in size, or about 2 nm to about 15 μm in size, or about 2 nm to about 10 μm in size, or about 2 nm to about 5 μm in size, or about 2 nm to about 1 μm in size, or about 2 nm to about 0.5 μm in size, or about 2 nm to about 0.1 μm in size, or about 2 nm to about 0.2 μm in size, or about 2 nm to about 0.05 μm in size, or about 2 nm to about 100 nm in size, or about 2 nm to about 200 nm in size, or about 2 nm to about 300 nm in size, or about 2 nm to about 400 nm in size, or about 2 nm to about 500 nm in size. In certain embodiments, for medicinal iron infusion preparation particles, the Fe3+ particle diameter is typically about 60 nm to about 180 nm. In some embodiments, the impurities in the prepared particles are the same as those in the starting material. In other embodiments, the impurities in the produced particles are different from those in the starting material.

[0028] The fabrication of metal particles by electrophoretic dispersion (EED) has several advantages. For example, the produced particles can be relatively pure, monodisperse, different sizes (i.e., micron-, submicron-, and nanometer-sized), different shapes (i.e., spherical or with highly developed surfaces and high dislocation densities), different phases (i.e., amorphous, glassy, ​​and crystalline), and possess unique properties (e.g., magnetic properties, chemically active adsorbents, and flocculants). Furthermore, the EED process is environmentally friendly (i.e., no drain is required but can be used as needed; it does not emit gases or dust), has low specific energy (i.e., approximately 1.5–3 kW for the production of approximately 1 kg of particles), requires compact equipment, and is easily scalable.

[0029] EED metal particles and their oxides can be used in a variety of applications. For example, EED particles can be used to purify liquid samples and as additives in 3D printing. In EED printing, modifying the properties of metal particles can simplify the 3D printing process and add tensile strength to printed metal objects. For example, nickel EED particles and particle oxides can be used in catalysts, coatings, polymers, fibers, batteries, porcelain, pigments, aircraft parts manufacturing, electronic, optical, and medical devices, and generally as a platinum replacement in different applications. For example, copper EED particles and particle oxides can be used in aviation, biology, and metallurgy, as antibacterial and bactericidal compounds, and in electronic and optical devices. For example, iron EED particles and particle oxides can be used in water purification, magnets, ferrites, coatings, polymer and metallurgical powder manufacturing, pharmaceutical compositions or supplements in medicine and biology, memory storage devices, and as additives such as reinforcing agents or fillers. For example, aluminum EED particles and particle oxides can be used for water purification and in the production of jewelry, optical lenses, grinding pastes, and rocket fuel. Titanium EED particles and particle oxides can be used as antibacterial agents, bactericides, UV stabilizers, additives, high-strength coatings, pigments, and metallurgical powders. For example, zinc EED particles and particle oxides can be used as antibacterial and bactericidal compounds and in the production of polymers, fibers, coatings, hydrogen fuel cells, solar cells, and metallurgical powders. For example, tungsten EED particles and particle oxides can be used in the production of wear-resistant coatings, cutting and drilling tools, armor piercing cores, contacts for high-current switches, and metallurgical powders. For example, molybdenum EED particles and particle oxides can be used as catalysts and in the production of coatings, polymers, corrosion inhibitors, and metallurgical powders. For example, silver EED particles and particle oxides can be used as antibacterial agents, catalysts, and additives, and to coat aircraft parts. Gold EED particles and particle oxides can be used in electronics, medical, aviation, and jewelry, as catalysts and additives.Platinum EED particles and particulate oxides can be used, for example, in electronics, medicine, aviation, hydrogen fuel cells, precision machinery manufacturing, and as additives.

[0030] In some embodiments, the EED particles are formed of one or more of iron, iron oxide, or iron hydroxide, or a combination of one or more of the foregoing compositions. Examples of iron include, but are not limited to, iron alone or as a compound or alloy with one or more of chromium, copper, molybdenum, zinc, cobalt, nickel, cadmium, manganese, arsenic, tin, lead, aluminum, cesium, and strontium. Iron may also include ferric iron, such as ferric oxyhydroxide. Iron oxides include Fe 3+ , Fe 2+ , Fe+O+OH, Fe3+OH, and FeO, FeO2, Fe3O4, Fe4O5, Fe5O6, Fe5O7, Fe 25 O 32 , Fe 13 O 19 and Fe2O3, α-Fe2O3 (α-phase), β-Fe2O3 (β-phase), γ-Fe2O3 (γ-phase), or ε-Fe2O3 (ε-phase). Examples of iron hydroxides include iron(II) hydroxide (Fe(OH)2) and iron(III) hydroxide (Fe(OH)3), iron(III) hydroxide, hydrated iron oxyhydroxides (iron oxyhydroxides), and combinations thereof.

[0031] In these embodiments, iron oxide EED particles are effective for extracting metal and heavy metal ions from liquid samples. These metals include, but are not limited to, iron, chromium, copper, molybdenum, zinc, cobalt, nickel, cadmium, manganese, arsenic, tin, and lead. In other embodiments, alumina EED particles are fabricated. In these embodiments, the alumina EED particles are effective for extracting metal and heavy metal ions from liquid samples. These metals include, but are not limited to, iron, chromium, copper, molybdenum, zinc, cobalt, nickel, cadmium, manganese, arsenic, tin, lead, aluminum, barium, cesium, and strontium.

[0032] Extraction of metal or heavy metal ions from a liquid sample can be achieved by mixing a dry or wet powder of EED particles with the liquid sample. By way of example, the EED particles can be iron oxide EED particles, alumina EED particles, or a combination thereof. The mixture can then be allowed to stagnate for a predetermined period of time, mixed manually, or mixed using a shaker, sonicator, magnetic stir bar, vortex mixer, or any combination thereof. The predefined period can be between about 2 minutes and about 240 minutes, between about 2 minutes and about 180 minutes, between about 2 minutes and about 120 minutes, between about 2 minutes and about 60 minutes, between about 2 minutes and about 30 minutes, between about 2 minutes and about 15 minutes, between about 2 minutes and about 8 minutes, or between about 2 minutes and about 4 minutes. After the EED particles react with the ions, the reacted metal particles can solidify to form a slurry. The slurry can then be passed through a filter. The filter can have a mesh size of about 0.05 μm to about 100 μm, or about 0.05 μm to about 50 μm, or about 0.1 μm to about 25 μm, or about 0.5 μm to about 15 μm, or about 1 μm to about 10 μm, or about 100 nm to about 500 nm, or about 100 nm to about 200 nm, or about 100 nm to about 300 nm, or about 100 nm to about 400 nm. In some embodiments, the filter can have a mesh size of about 0.05 μm, or about 0.1 μm, or about 0.5 μm, or about 1 μm, or about 10 μm, or about 15 μm, or about 25 μm, or about 50 μm, or about 100 μm. The degree of extraction of ions from a liquid sample can be between about 50% and about 100%, or between about 60% and about 100%, or between about 70% and about 100%, or between about 80% and about 100%, or between about 90% and about 100%, or between about 95% and about 100%, or between about 99% and about 100%, or between about 99.5% and about 100%. In some embodiments, the degree of extraction of ions from a liquid sample can be at least 50%, or at least 60%, or at least 70%, or at least 80%, or at least 90%, or at least 95%, or at least 99%.

[0033] In some embodiments, the EED particles have electromagnetic properties and can absorb microwaves. In these embodiments, the fabricated EED particles exhibit microwave absorption values ​​similar to or greater than commercially available particles. As an example, some iron oxide EED particles disclosed herein enable microwave absorption values ​​comparable to hexaferrite powder and greater than iron oxide Magsilica® powder. Applications involving high-frequency electromagnetic fields (e.g., satellite television, mobile phones, WLAN technology, traffic and aviation surveillance radar, microwave heating, drying, sintering, and even automotive and medical applications) require low-cost absorbing materials, such as the iron oxide EED particles disclosed herein, to reduce electromagnetic exposure to biological systems and ensure safe and reliable operation of equipment and devices (e.g., preventing radio signal leakage). The iron oxide EED particles disclosed herein can also be used to fabricate composites for microwave-induced curing bonding or magnetically soft composites.

[0034] In some embodiments, the EED particles have other uses. For example, the particles can be used as an inactive ingredient in a pharmaceutical composition, an active ingredient in a pharmaceutical composition (optionally with a carbohydrate coating to allow precise delivery in the GI tract or other absorption site as desired), an inactive ingredient in a dietary supplement, an active ingredient in a dietary supplement (e.g., where the metal has nutritional benefits when ingested by humans or animals), an adsorbent material, an absorbent material, a mineral supplement for crop production, a raw material for powder metallurgy (whether for ceramics or metal alloys), a nucleating agent for metallurgical applications, a nucleating agent for chemical applications, an industrial catalyst (e.g., Al2O3 particles, alone or in combination with other catalysts, can be used as one or more of the following for hydrogen production or reforming in transportation or stationary applications such as propulsion of automobiles, boats, ships, airplanes, rockets, trains, trucks, etc.), a laboratory catalyst, a support or substrate particle for a separate catalyst, a preservative, antioxidant, or stabilizer in a pharmaceutical composition, or a preservative, antioxidant, or stabilizer in a dietary supplement. In some embodiments, the EED particles are formed as part of a composite that can be used for any of the above applications. For example, in one embodiment, the EED particles are used or contained in one or more of ferric sodium gluconate, ferric carbohydrate complexes, ferric sucrose complexes, ferric maltose complexes, ferric carboxymaltose complexes, ferric dextrose complexes, etc. In yet another embodiment, the EED particles are complexed with any amino acid. In yet another advantageous embodiment, the EED particles are useful for inclusion in animal feed, thereby enabling more rapid growth and weight gain, even when the same caloric feed intake is otherwise provided in the animal's diet. Such animals include, but are not limited to, domestic and wild animals, including one or more of horses, donkeys, cows, zebu, Bali cattle, yaks, buffalo, gaillards, sheep, goats, reindeer, Bactrian camels, Arabian camels, llamas, alpacas, pigs, rabbits, guinea pigs, poultry (chickens, ducks, geese, turkeys, etc.), dogs, cats, birds, etc.

[0035] In some embodiments, it is believed that the unique particle composition, microstructural morphology, surface area and morphological characteristics, and particle size, in particular, combine to increase absorption in humans or animals, thereby providing beneficial effects. In particular, by way of example, the iron EED particles of the present disclosure are believed to increase absorption in humans as part of a dietary supplement or pharmaceutical composition. Without wishing to be bound by theory, it is believed that the iron EED particles of the present disclosure have increased absorption, allowing them to be used as pharmaceutical compositions absorbed through the gastrointestinal tract.

[0036] Referring to the flowchart in FIG. 1 as well as FIGS. 2-4, in a method for producing micron-, submicron-, and nanometer-sized particles according to one or more embodiments of the present teachings, one or more metal elements can be added to a plasma reactor in the presence of a circulating fluid, such as an organic fluid, an inorganic fluid, or a combination thereof. By way of example, the inorganic fluid can be water, hydrogen peroxide, or a combination thereof. The circulating fluid can also include other elements, such as one or more electrolytes, monosaccharides, disaccharides, polysaccharides, or any combination thereof. By way of example, the electrolyte can be sodium chloride, potassium chloride, calcium chloride, lithium chloride, ferric chloride, sodium nitrate, potassium nitrate, magnesium nitrate, potassium nitrate, silver nitrate, sodium acetate, ammonium acetate, sodium carbonate, potassium carbonate, calcium carbonate, sodium bicarbonate, copper sulfate, or any ion thereof, or any combination thereof. By way of example, the monosaccharide can be glucose, fructose, galactose, or any combination thereof. By way of example, the disaccharide can be maltose, sucrose, lactose, or any combination thereof. By way of example, the polysaccharide may be cellulose, chitosan, pectin, starch, glycogen, or any combination thereof. In some embodiments, the metallic element used to make the particles comprises an alkali metal, an alkaline earth metal, a transition metal, a post-transition metal, or a metalloid, or any combination thereof. Some examples of such metals include, but are not limited to, iron, aluminum, nickel, cobalt, tungsten, copper, zinc, lead, molybdenum, tantalum, tin, vanadium, chromium, titanium, niobium, silicon, and zirconium.

[0037] More specifically, the plasma reactor 200 includes an upper portion 202 consisting of an inlet 210 designed to load material into the plasma reactor, two electrodes (cathode / anode) 216 / 218, and an inlet designed to apply an electrical discharge to the plasma reactor, and a channel 212 for circulating a fluid (not shown). The plasma reactor also includes one or more walls 204, a bottom portion 206 including a mesh bottom portion 208 for pumping the circulating fluid, and a channel 214 for circulating the fluid. The plasma reactor defines a cavity space 220 in which particles are produced.

[0038] 3 is a schematic diagram of an electrophoretic dispersion (EED) system 300. In some embodiments, the EED system includes, in addition to the plasma reactor 200, a generator 302, a precipitation tank 304, a circulation pump 306, and a control system 308. Metal elements disposed within the plasma reactor 200 are vaporized to form metal vapor when plasma is generated by at least one discharge pulse from electrodes 216 and 218. The metal vapor is condensed to produce metal particles, which are then transported to the precipitation tank 304 for precipitation. The precipitate is then removed from the precipitation tank and subjected to sublimation, drying, and pulverization.

[0039] As described above, the electrolyte dispersion (EED) system 300 includes multiple functional elements controllable by one or more control systems. As an example, FIG. 4 schematically illustrates an exemplary implementation of a control system 308, which includes a central processing unit (CPU) 400 for controlling the operation of one or more elements of the system. The control system also includes an interface 402, a communication port 404 for communicating with various components of the system, a memory device 406, a controller 408, a random access memory (RAM) 412, and a read-only memory (ROM) 410. As an example, instructions for producing particles can be stored in the ROM 410, RAM 412, or other memory device 406, and a processor can access those instructions to control the operation of the various functional units of the system under the control of the control system 308. For example, the instructions can provide the duration and power of each electrical pulse generated in a plasma reactor and the velocity of a circulating fluid passing through the plasma reactor.

[0040] The production of nano-dispersed polyvalent iron oxide powders can find a wide range of applications in the nano, petroleum, chemical and electronic industries as well as medicine, energy, biology and agriculture.

[0041] In one embodiment, the EED process begins by loading the feedstock into a reaction chamber. The reaction chamber is made of a dielectric material. The dielectric material can be electrically insulating, thermally insulating, or both electrically and thermally insulating. During operation, cooled, recycled water is pumped into the reaction chamber. During operation, a pulse generator sends a current discharge through one or more electrodes that are in direct contact with the layer of feedstock present in the reaction chamber.

[0042] The raw material is loaded onto a perforated partition plate in a reactor made of a dielectric material. To ensure a specific optical distribution density of the moving discharge in the loaded layer of raw material, cooled, recycled, clear water is continuously circulated under pressure within the reactor chamber. This creates a "pseudo-boiling layer" floating above the partition, preventing the formation of localized plasma discharges that could lead to localized melting zones. In certain embodiments, one or more electrodes contact the raw material in the plasma reactor. In some embodiments, recycled, cooled, clear water is circulated under pressure to achieve a "fluidized" layer of raw material, such as when the raw material is in granular form. The amount of discharge contact in the raw material layer is maintained at approximately the same level at the start of the EED process and throughout the entire gradual melting. Furthermore, the frequency of the current applied by the electrodes is 500-800 Hz, the amplitude of the pulsed current is within 8-20 kA, and the voltage is 100-800 V. These values ​​are merely examples and can be varied depending on the desired range of dispersed raw material and the resulting product.

[0043] Ensuring an optimal specific density of the distribution of moving discharges in the loaded layer of material is achieved by continuous circulation of cooled, clear water under pressure within the EED plasma reactor. In some embodiments, the total number of discharge contacts in the layer of feedstock is maintained at approximately the same level both at the beginning of loading the reactor and throughout the entire course of slow electroerosive dissolution.

[0044] Referring now to FIG. 19, one embodiment of an EED apparatus 1901 and related components is shown. An electric pulse generator 1902 generates electric pulses with controlled parameters including one or more of voltage, repetition rate, duty cycle, discharge current stabilization, and pulse shape. The EED plasma reactor 1903 is where the process of electrolytic dispersion of granules (chips, shot, etc.) from iron, steel, or cast iron takes place. A bunker 1904 stores raw materials such as chips, shot, and pellets that are fed into the EED plasma reactor 1903. A vibratory feeder controls 1905 the feedstock dosage to the EED plasma reactor 1903. One or more settling tanks 1906 settle the water suspension of product materials such as magnetite and also provide clarification and cooling of the working fluid. One or more electric valves, depicted as 1907a, 1907b, and 1907c, automate the process of periodically unloading the settling tank volume containing the working fluid and one or more product materials, such as magnetite. A circulation pump 1908 circulates the working fluid to create a controlled fluidized bed of granules and continuous circulation of water within a closed circle. The working fluid first passes through the EED plasma reactor 1903, then through one or more settling tanks 1906, and finally through one or more electric valves 1907a, 1907b, and 1907c before returning to the pump 1908 and the plasma reactor 1903. Current transformers CT1 and CT2 each acquire information regarding the average integrated current intensity of the discharge pulses generated by pulse generator 1902. This information serves to control the operation of the vibratory feeder, maintain the reactor load distribution granules at a predetermined level, and ensure that their volume decreases as the granules are processed. Current transformer CT2 retrieves information about the instantaneous pulse current, which is used by a first software controller 1909 to control the operation of the vibratory feeder 1905 to maintain a predetermined level of reactor load material, the volume of which decreases as the granules are processed. Furthermore, software controller 1910 controls the circulation pump 1908 by operating through a frequency converter 1911.

[0045] A timer 1912 is controlled based on accumulated information about the time and operating mode of the equipment obtained by the first software controller 1909 and the second software controller 1910. The timer 1912 periodically opens one or more electrically driven valves 1907a, 1907b, or 1907c to release the settled magnetite paste from the settling tank. The frequency converter 1911 is designed to smoothly change the frequency of the supply network of the circulation pump 1908, thereby smoothly changing its pressure-flow characteristics. This allows for a "pseudo-boiling" or "fluidized" layer of granules, thereby avoiding the formation of localized melts of the granules. The timer 1912 controls the remote opening of one or more of the valves 1907a, 1907b, or 1907c to control the release of the settled magnetite paste or other product from the settling tank 1906.

[0046] Applicant has also characterized the conditions present in the plasma channels of electrical microdischarges. In these plasma channels, temperatures are approximately 1×10 4 ℃~approx. 1.5×10 4 °C, and the amount of electrical energy in the spark contact zone between the granules is less than about 1 J. As a result of the volumetric electrospark treatment during dispersion of steel (cast iron, iron) granules or shavings in water with a pulse discharge current of up to 20 kA, magnetite powders with particle sizes of about 2 to about 3 nm have been obtained. Without wishing to be bound by theory, the applicant believes that with corresponding parameters of the pulse discharge, the smallest particles, down to the atomic level, can be obtained by the EED method.

[0047] The size of the particles is determined by one or more of the duration of the discharge, the energy of the discharge, the physical parameters of the dispersibility, the size and morphology, the composition of the dispersible material, the thermodynamic properties of the working fluid such as boiling point and heat capacity, and the hydraulic properties of the movement of the working fluid in the reactor.

[0048] In some embodiments, the specific energy consumption per particle formation is controlled, thereby controlling the size of the formed particles and maintaining the specific density of the dispersion. This is achieved by stabilizing the integrated discharge current of the pulse generator, selecting a predetermined repetition rate of the discharge pulses, and shortening the duration of the discharge between the granules. Without wishing to be bound by theory, given the highly stochastic nature of the emergence and movement of plasma channels in the granule volume and the numerous spark contacts between the granules, hydrodynamic adjustment of the pressure-flow characteristics of the circulation pump plays a key role in solving this problem.

[0049] In one embodiment, the number of transitioning discharge chains depends on the degree of load on the plasma reactor. Therefore, it can be controlled by adjusting the load on the plasma reactor. When the plasma reactor is loaded to its maximum capacity of the feedstock, the number of transitioning discharge chains is also maximized. However, the load should not be so high that local melting occurs instead of electrolytic corrosion.

[0050] In one embodiment, a two-channel mode of operation control is provided, which provides a flexible control system for stabilizing the dispersion of the generated magnetite. In particular, when the first software controller and the second software controller are used as described herein, this controls the peak current load that may occur during position compression of the layer of feedstock. This increases the dispersion of the feedstock and therefore increases the operating life of the device.

[0051] Example Although the present invention has been described in considerable detail with reference to certain preferred embodiments thereof, other versions are possible. Therefore, the spirit and scope of the appended claims should not be limited to the description and preferred versions contained within. Various aspects of the present invention will be described with reference to the following non-limiting examples.

[0052] material The iron pieces and electrodes were made of structural carbon steel.

[0053] The polyvalent iron oxide was prepared from carbon steel (St3 (DSTU 2651-94 / GOST 380-94), A568M (ASTM International), or 1.0116 (DIN EN 10025)).

[0054] Tap water was used to prepare the EED particles.

[0055] MagSilica® and Ti-substituted barium hexaferrite powder were used as standard materials to analyze the heating behavior of EED particles. MagSilica® is a nanoscale oxide powder containing Fe3O4 in the core and SiO2 in the shell. This powder is used as an adhesive to bond materials such as glass and plastic. Ti-substituted barium hexaferrite powder was developed for the production of electromagnetic shielding materials in the microwave range and for bonding and debonding in high-frequency electric fields.

[0056] Experimental equipment for electrodeposition dispersion processing of metal particles Metal particles were produced using an EED (Electroerosion Dispersion) experimental apparatus (Figure 5). The EED apparatus consists of a pulse generator 1, a tank 2, a sedimentation tank 3, and a pump 4.

[0057] The installation area of ​​EED is approximately 5m 2 Approximately 7m from 2The pulse generator 1 generated a discharge in the plasma reactor 2 over a wide range of frequencies and voltages (i.e., about 100 Hz to about 500 Hz, about 10 Hz to about 1000 Hz, about 100 V to about 500 V, or about 10 V to about 800 V). Both the plasma reactor 2 and the precipitation tank 3 were connected by a pump 4. The EED installation required low energy intensity (i.e., about 1.5 kW to about 3 kW) to generate about 1 kg of particles. The synthesis rate was about 1 kg / h to about 2 kg / h. However, by increasing the volume of the plasma reactor to about 20 L, the productivity of the EED facility could be increased to about 5 kg / h. The EED process is environmentally acceptable and does not emit electronic agents, gases, or particulates. The EED method generates about 10 6 Temperature gradients of up to K / mm were possible. Metal vapors and microdroplets were almost instantly released (τ ≒ 10 ?6 When particles are produced under these conditions, they have unique particle properties, such as a distorted crystal lattice, a high dislocation density, and a high surface area and specific surface area of ​​the crystal grains.

[0058] Features The density of the EED particles was measured by first drying them in a vacuum desiccator by gas pycnometry with argon using an AccuPyc II 1340 instrument (sold by Micromeritics Instrument Corporation, Norcross, USA) and then analyzing them by high-precision mass measurement using a Balance MC 210 P instrument (sold by Sratorius AG, Göttingen, Germany).

[0059] The particle size distribution of EED particles was measured. Specifically, EED particles were first diluted with double-distilled water to a sample concentration of 0.15 mg / mL and sonicated in a bath sonicator at 35 kHz for 3 minutes using a Sonorex Digital 10P instrument (sold by Bandelin electronic GmbH & Co. KG, Berlin, Germany) to deagglomerate and disperse the particles. The EED particles were then analyzed by dynamic light scattering using a Malvern Zetasizer 3000 HS instrument (Malvern Instruments Inc., Malvern, UK). Each sample was measured in triplicate and statistically evaluated.

[0060] The size and morphology of primary particles, aggregates, and agglomerates of EED particles were measured by transmission electron microscopy (TEM) using a Tecnai 20S (sold by FEI Company, Hillsboro, USA) and scanning electron microscopy (SEM) using a Hitachi S-4800 (sold by Hitachi Ltd, Missisuga, Canada).

[0061] Phase analysis of the EED particles was performed using a Siemens / Bruker D-5000 X-ray diffractometer (XRD) system (sold by Bruker Corporation, Billerica, USA) using a theta / theta vertical goniometer system (Bragg-Brentano configuration) with optional spinner (phi) rotation and Cu-Kα radiation (λ = 1.540598 Å). Measurements were performed at room temperature, and phase identification was performed by comparing the measurement patterns with the JCPDS (Joint Committee on Powder Diffraction Standards) data card (International Centre for Diffraction Data, PDF-2 2018).

[0062] Fe in EED particles 2+ Serimetry and selenometric titration were carried out to determine the amount of Ce. 4+ Fe 2+ is oxidized to Fe 3+A redox titration was performed with the EDTA solution, and the electrochemical potential was monitored. The experimental design consisted of a Pt indicator electrode and a calomel reference electrode. To prepare the analytical sample, 300 mg of EED particles were heated with 100 mL of 8.5 M HCl at 95 °C for 2 h under N2 current until complete dissolution. After cooling for several minutes, 20 mL of 40% HClO and 100 mL of double-distilled, gas-free water were added to the sample. A standard solution of 0.1 M Ce(SO4)2 was used as the titrant.

[0063] The magnetization of the EED particles was measured using a vibrating sample magnetometer (VSM) 293904C (Princeton Instruments, Trenton, USA) at room temperature with a powder sample of approximately 40 mg mass, and an applied magnetic field strength of H = ±1.15 × 10 6 The measured curve m(H0) was converted to M(H) using equations (I) and (II). [ka] where M is the magnetization, m is the measured magnetic moment, and m s is the mass of the sample, ρ S is the density of the sample, [ka] where H is the magnetic field strength in the sample, H0 is the applied magnetic field strength, and N is the demagnetization factor.

[0064] The demagnetization factor N of each sample prepared is calculated at point H = J H c The slope tan α of the hysteresis loop M(H) at θ was determined iteratively using equation (III). [ka]

[0065] Magnetic parameters, especially saturation magnetization (M s ), coercive force ( J H C ) and remanent magnetization (M r) was deduced from the corrected hysteresis loop M(H), where J is a measure of the coercivity when the magnetic polarization J is zero.

[0066] The microwave absorption of the synthesized EED particles was measured. Specifically, the same mass (1 g) was packed into a silica glass crucible (inner diameter 20 mm), and the heating curve (Δθ(t)) of the sample was measured in a 2.45 GHz special microwave oven AFKP® MW17.3 (sold by AFK Deutschland GmbH, Hamburg, Germany) equipped with an IR sensor OptrisCT® (sold by Optris GmbH, Berlin, Germany). The measurement was repeated three times to determine temperature-dependent changes (e.g., oxidation). [Example]

[0067] Preparation of TiC / Ti / Al EED particles TiC / Ti / Al particles were fabricated using electrolytic dispersion (EED) (Figure 6A-B). Specifically, aluminum and titanium bulk materials were dispersed in a liquid using EED (Figure 6A), and the liquid was constantly pumped through a plasma reactor, which consisted of two electrodes and a plasma. The resulting EED particles had diameters in the micron and submicron range (Figure 6B). [Example]

[0068] Preparation of iron oxide EED particles Iron oxide particles were prepared using electroerosion dispersion (EED) (Figures 7A-D). Specifically, metallic iron chips were dispersed in water using EED. Water was constantly passed through a plasma reactor, which consisted of two electrodes and a plasma (Figure 7A). The particles were transported to a precipitation chamber, where the precipitation process proceeded. The precipitate was removed from the precipitation chamber, sublimated, dried in vacuum or air, and finally briefly pulverized. The obtained EED particles formed aggregates (Figure 7B), with primary particles of approximately 20 nm to approximately 50 nm in diameter (Figure 7C), and particles of approximately 7 nm to approximately 8 nm in diameter (Figure 7D). [Example]

[0069] Density and size of iron oxide EED particles The density and particle size of the iron oxide EED particles were measured (Figure 8). Before microwave heating, the density was 5.347 ± 0.015 g / cm. 3 ) and after heating (5.393±0.036g / cm 3 ) is calculated by multiplying the theoretical density of magnetite (ρ th =5.175g / cm 3 ) is almost the same as or slightly larger than the theoretical density of the synthesized iron oxide EED particles, which is 7.874 g / cm 3 Fe and theoretical density 5.88g / cm 3 The phase analysis described below reveals that the powder further contains heavy phases such as FeO. 10,3 =3.6μm to D 90,3 = 11.8 μm, and the index characterizes the volume-weighted percentage. The measured particle size partly reflects the size of particle aggregates or agglomerates rather than the size of the primary particles synthesized. [Example]

[0070] Phase analysis of iron oxide EED particles Phase analysis of the iron oxide EED particles was performed (Figure 9). The two figures in Figure 9 show the results of X-ray diffraction analysis of EED particles before (bottom dark line) and after (top light line) microwave heating. The primary phase in both EED particles was magnetite (Fe3O4). The secondary phase was metallic iron (Fe), with a minor proportion. Another detected phase was wüstite (FeO). This correlates well with the conclusions from the density measurements shown in Figure 8 and described above. Furthermore, these results indicate that reducing conditions occurred during the EED process due to the rapid solidification of the iron vapor and microdroplets generated and insufficient oxygen production. Similar phase compositions and particle sizes were also obtained with other iron oxide particles synthesized by underwater discharge. [Example]

[0071] Magnetic properties of iron oxide EED particles The magnetic properties of iron oxide EED particles were analyzed (Fig. 10, Fig. 11).

[0072] Figure 10 shows two hysteresis curves of iron oxide EED particles. The curves are corrected hysteresis curves before (dark line) and after (thin dashed line) microwave heating. It can be seen that the EED particles exhibit magnetic properties (saturation magnetization Ms = 301.0 kA / m, saturation polarization JS = 378.2 mT). Both hysteresis curves show the soft magnetic behavior of EED particles with Fe3O4 as the main phase. Furthermore, the effect of heating in an air atmosphere during microwave annulation was also observed. In iron oxide particles containing Fe and FeO, these phases are oxidized by microwave heating, resulting in a decrease in saturation magnetization (M S ) decreases, and the coercive force ( J H c ) was expected to increase.

[0073] Figure 11 shows the magnetic properties of iron oxide EED particles, Fe3O4, and Fe at room temperature. The saturation magnetization (M S ) is larger than the known magnetization value of Fe3O4, but smaller than that of nanoscale Fe particles. Here, the magnetic properties of ferromagnetic / ferrimagnetic materials are considered to depend on the size of the material, and the iron oxide EED particles are considered to contain a certain amount of metallic iron particles, as marked in Figure 9.

[0074] The magnetization (M S ) is larger than that of the metal oxide. However, metal particles without a barrier film are not stable in air, so they are easily oxidized, and their magnetization changes or disappears. This is the reason why the (M S ) decline and ( J H c ) is the reason for the increase.

[0075] Fe in relation to mass in iron oxide EED particles 2+ The content of Fe in magnetite was measured by coulometric titration and found to be 53.83±1.23 wt.%. This value is within the theoretical Fe content in magnetite. 2+This result also indicates the presence of other iron phases within the particles. During the analysis, the EED particles were dissolved in the acid solution, and Fe 2+ In acid medium under N2 flow, Fe was converted to Fe 2+ is oxidized to H + is reduced to H2. Assuming that the proportion of FeO is zero, it can be determined that approximately 30 wt.% of the iron oxide EED particles is Fe.

[0076] Fe in iron oxide EED particles after microwave heating 2+ The amount of Fe was only 43.51±1.11 wt.%. This amount is smaller than the value of the EED particles before microwave heating. This is because Fe was oxidized during microwave heating, resulting in about 10 wt.% Fe. 2+ This is consistent with the X-ray results and the change in the hysteresis curve.

[0077] Measurement of magnetic behavior, Fe 2+ The results of content measurement, phase analysis, and TEM analysis proved that iron oxide EED particles absorb microwaves. [Example]

[0078] Heating behavior of iron oxide EED particles The heating behavior of the iron oxide EED particles was analyzed (Figs. 12A and 12B). The figures shown in Figs. 12A and 12B show the heating behavior of the synthesized iron oxide EED particles (EED powder) in comparison with Ti-substituted barium hexaferrite powder and the commercially available iron oxide powder Magsilica® (Evonik Industries AG, Essen, Germany). The thermal behavior was measured by the heating curve (Δθ(t)) and the corresponding heating rate (Δθ / Δt(t)) in the microwave range of 2.45 GHz. The measurement of the heating behavior of the iron oxide EED particles (EED powder) was repeated three times (1 st Repeated measurements: EED powder, repeated measurements once, 2 nd Repeated measurements: "EED powder, repeated measurements" and "3 rd (Three replicates "EED powder, three replicates").

[0079] The heating curve (Δθ(t)) of the iron oxide EED particles changed during the initial microwave treatment but remained nearly constant thereafter. This was due to a slight change in the metallic phase, Fe, due to oxidation. This was confirmed by magnetization measurements (Figures 10 and 11) and cerium titration. Because iron oxide EED particles are easy to prepare and inexpensive, they were compared with Ti-substituted barium hexaferrite powder and iron oxide powder, MagSilica®. The time-dependent heat release (Δθ(t)) and heat release rate (Δθ / Δt(t)) of the iron oxide EED particles were found to be similar to those of the Ti-substituted barium hexaferrite powder, but greater than those of the commercially available MagSilica® powder. The calculated heating rate (Δθ / Δt) at the start of heating for the iron oxide EED particles was approximately 40 K / s. This is two-thirds of the heating rate of the Ti-substituted barium hexaferrite powder. [Example]

[0080] Preparation of crystalline alumina EED particles Crystalline alumina particles were produced using electrophoretic dispersion (EED) (Figure 13). Specifically, aluminum bulk material was dispersed in a liquid by EED, and the liquid was constantly pumped into a plasma reactor consisting of two electrodes and plasma. The obtained EED particles had a diameter of approximately 1 μm. [Example]

[0081] Preparation of amorphous alumina EED particles Amorphous alumina (Al2O3) particles were produced using the electrolyte dispersion method (EED) (Fig. 14). Specifically, aluminum bulk material was dispersed in a liquid by EED, and the liquid was constantly sent to a plasma reactor, which consisted of two electrodes and plasma. The obtained EED particles had a specific surface area (S) of 137 m 2 / g and the porosity (Rpor) was 24A (tilda). [Example]

[0082] Liquid sample processing using iron oxide EED particles The liquid sample was treated with iron oxide EED particles (Figure 15). Iron oxide EED particles were used as a flocculant to extract metal and heavy metal ions from the galvanic drain aqueous sample. Specifically, dry powder of iron oxide EED particles, consuming 6–7 g per 1 g of impurities, was added to the liquid sample and stirred for 8–10 minutes. After flocculation was complete, the resulting slurry was passed through a self-cleaning filter with a 10 μm mesh size (e.g., AMIAD). The quality of the treated galvanic drain aqueous sample met the requirements of the Water Pollution Control Act. [Example]

[0083] Liquid sample processing using aluminum oxide EED particles The liquid sample was treated with aluminum oxide EED particles (Figure 16). The aluminum oxide EED particles were used as a flocculant to extract metal and heavy metal ions from the wastewater sample. [Example]

[0084] Preparation of EED particles of cobalt, nickel, and hard alloys Cobalt, nickel, and hard alloy particles were produced by the EED method (FIGS. 17A to 17C). The histograms shown in FIGS. 17A to 17C show the mass distribution of the cobalt, nickel, and hard alloy EED particles. [Example]

[0085] Recycling of tungsten carbide alloys by EED A tungsten carbide alloy was recycled with EED (Figures 18A-C). This alloy was obtained from munitions and converted into particles using EED. Figure 18B shows the resulting EED powder consisting of tungsten particles, and Figure 18C shows a TEM image of the resulting EED powder.

Claims

1. A method for producing particles, comprising: adding a plurality of metal elements to a plasma reactor having two electrodes and containing a circulating fluid; evaporating the metal element to form a metal vapor using a plasma generated by at least one discharge pulse between the electrodes; condensing the metal vapor to form particles; the particles comprise one or more of a pure metal, a metal oxide, a metal carbide, or a metal nitride; and The method of making, wherein the circulating fluid comprises a monosaccharide, a disaccharide, a polysaccharide, or any combination thereof.

2. The method for producing particles according to claim 1, further comprising: transporting the particles to a precipitation tank coupled to the plasma reactor; allowing the particles to settle in the settling tank to form a precipitate; removing the sediment from the settling tank; sublimating the precipitate; drying the precipitate; and grinding the precipitate; A method of making the same.

3. 3. The method for producing particles according to claim 2, wherein the particles are carried to the settling tank by the circulating fluid.

4. 2. The method of claim 1, wherein the metal element is selected from the group consisting of an iron-containing element, an aluminum-containing element, a titanium-containing element, and a tungsten-containing element, or a combination thereof.

5. 10. The method of claim 1, wherein the circulating fluid comprises water, hydrogen peroxide, or a combination thereof.

6. 10. The method of claim 1, wherein each particle has a diameter between 2 nm and 60 μm.

7. 10. The method of claim 1, wherein each particle has a diameter between 2 nm and 30 μm.

8. 10. The method of claim 1, wherein each particle has a diameter between 2 nm and 1 μm.

9. The method of claim 1 , wherein the particles comprise metal oxide particles.

10. 10. The method of claim 1, wherein the particles comprise iron oxide particles.

11. 11. The method of claim 10, wherein the iron oxide particles are microwave absorbing.

12. The method of claim 1 , wherein the particles comprise alumina particles.

13. A method for extracting metal ions from a liquid sample using the particles according to any one of claims 11 to 12, comprising: mixing the particles with the liquid sample; reacting the particles with the ions; agglomerating the reacted particles to form a slurry; and filtering the slurry; A method comprising:

14. 14. The method for extracting metal ions from a liquid sample according to claim 13, wherein the slurry is filtered using a filter with a mesh size between 0.1 μm and 25 μm.

15. 14. The method of extracting ions of a metal from a liquid sample according to claim 13, wherein the degree of extraction of ions from the liquid sample is between 80% and 100%.

16. 1. A method of forming a pharmaceutical composition, comprising: adding a plurality of metal elements to a plasma reactor having two electrodes and containing a circulating fluid; evaporating the metal element to form a metal vapor using a plasma generated by at least one discharge pulse between the electrodes; condensing the metal vapor to form particles; and and forming a pharmaceutical product using the particles, the particles comprise one or more of a pure metal, a metal oxide, a metal carbide, or a metal nitride; and The method, wherein the circulating fluid comprises a monosaccharide, a disaccharide, a polysaccharide, or any combination thereof.

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