# US 9,039,916 B1 · In situ oxide removal, dispersal and drying for copper copper-oxide > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,039,916 B1 - Document ID: US9039916B1 - Status: Granted - Kind: B1 - Application number: 12/961,030 - Filed: 2010-12-06 - Granted: 2015-05-26 - Earliest claimed: 2009-12-15 - Assignees: SDCmaterials, Inc. - Applicants: Stephen Edward Lehman, Jr. - Inventors: Stephen Edward Lehman, Jr. - Web page: https://patentgrep.com/patent/US9039916B1 ## CPC - B28B 3/025: {Hot pressing, e.g. of ceramic materials} - B01J 23/42: Platinum - B01J 23/8926: {Copper and noble metals} - B01J 37/00: Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts - B28B 23/0081: {Embedding aggregates to obtain particular properties} - B28B 23/0087: {Lightweight aggregates for making lightweight articles} - B32B 5/30: one layer {being formed of particles, e.g. chips,} granules, powder - B32B 7/12: using interposed adhesives or interposed materials with bonding properties - B32B 37/14: characterised by the properties of the layers - B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites - B82Y 40/00: Manufacture or treatment of nanostructures - C01B 33/027: by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material - C23C 4/134: Plasma spraying - F41H 1/02: Armoured or projectile- or missile-resistant garments; Composite protection fabrics {(F41H5/04 takes precedence)} - F41H 5/0471: {Layered armour containing fibre- or fabric-reinforced layers (in combination with ceramic layers F41H5/0428, with metal layers F41H5/0457)} - F41H 5/0492: {Layered armour containing hard elements, e.g. plates, spheres, rods, separated from each other, the elements being connected to a further flexible layer or being embedded in a plastics or an elastomer matrix} - H01B 1/02: mainly consisting of metals or alloys - H05K 1/0306: {Inorganic insulating substrates, e.g. ceramic, glass} - H10P 72/74: {using temporarily an auxiliary support} - H10W 44/00: Electrical arrangements for controlling or matching impedance - B22F 1/147: {Making a dispersion} - B32B 2037/1253: {curable adhesive} - B32B 2262/0253: Polyolefin fibres - B32B 2264/104: Oxysalt, e.g. carbonate, sulfate, phosphate or nitrate particles - B32B 2264/107: Ceramic - B32B 2307/558: Impact strength, toughness - B32B 2571/02: defensive, e.g. armour plates or anti-ballistic clothing - H05K 1/16: incorporating printed electric components, e.g. printed resistors, capacitors or inductors - Y02E 60/10: Energy storage using batteries - Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product - Y10T 428/12576: Boride, carbide or nitride component - Y10T 428/24983: Hardness - Y10T 428/25: Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles - Y10T 428/252: Glass or ceramic [i.e., fired or glazed clay, cement, etc.] [porcelain, quartz, etc.] - Y10T 428/26: Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension - Y10T 428/28: Web or sheet containing structurally defined element or component and having an adhesive outermost layer - Y10T 428/2916: including boron or compound thereof [not as steel] - B28B: SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER (foundry moulding B22C; working stone or stone-like material B28D; shaping of substances in a plastic state, in general B29C; making layered products not composed wholly of these substances B32B) - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM - B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04) - F41H: ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL - H01B: CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES (selection for magnetic properties H01F1/00; waveguides H01P {; printed circuits H05K}) - H05K: PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS - H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10 - H10W: GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10 - B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER - Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION - Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract A method for removing copper-oxide from copper powder, the method comprising: providing a copper powder defined by each particle having a copper core and a copper-oxide layer surrounding the copper core; disposing the particles in an etching solution in a container, wherein the etching solution removes the copper-oxide layer from each particle; decanting the etching solution and by-products; washing the particles; disposing the washed particles in an organic solvent; coating each copper core with an organic material from the organic solvent; dispersing the particles in the organic solvent; and providing the copper powder as dispersed copper cores that are absent a copper-oxide layer and have an organic coating, wherein the steps of dispersing in the etching solution, decanting, washing, disposing in the organic solvent, coating, and dispersing are performed in situ with the plurality of particles disposed in liquid, absent any exposure of the copper cores to air. ## Claims ### Claim 1 A method for removing copper-oxide from copper powder, the method comprising: providing a copper powder defined by a plurality of particles, each particle in the plurality of particles having a copper core and a copper-oxide layer surrounding the copper core, the copper core selected from the group consisting of a pure copper and a copper alloy; disposing the plurality of particles in an etching solution in a container, wherein the etching solution removes the copper-oxide layer from each particle; decanting the etching solution and the by-products resulting from the copper-oxide removal; washing the plurality of particles, wherein substantially all of the remaining etching solution and substantially all of the by-products are removed from the container holding the plurality of particles; disposing the washed plurality of particles in an organic solvent; directly coating the surface of each copper core in the plurality of particles with an organic material from the organic solvent; dispersing the plurality of particles in the organic solvent; and providing the copper powder as a plurality of dispersed copper cores that are absent a copper-oxide layer surrounding each copper core, each copper core having an organic coating, wherein the steps of disposing in the etching solution, decanting, washing, disposing in the organic solvent, coating, and dispersing in the organic solvent are performed in situ with the plurality of particles disposed in liquid, absent any exposure of the copper cores to air. ### Claim 2 (depends on 1) The method of claim 1, wherein the step of providing the copper powder comprises providing the copper powder in a dry state. ### Claim 3 (depends on 1) The method of claim 1, wherein the step of disposing the plurality of particles in the etching solution further comprises each one of the plurality of particles retaining substantially all of the copper core. ### Claim 4 (depends on 1) The method of claim 1, wherein the etching solution comprises acetic acid and water. ### Claim 5 (depends on 4) The method of claim 4, wherein the etching solution comprises between approximately 0.1% and 1.0% acetic acid. ### Claim 6 (depends on 1) The method of claim 1, wherein the organic solvent comprises tetraethylene glycol and water. ### Claim 7 (depends on 1) The method of claim 1, further comprising the step of storing the plurality of dispersed and coated copper cores in the organic solvent. ### Claim 8 (depends on 7) The method of claim 7, wherein the organic solvent comprises tetraethylene glycol. ### Claim 9 (depends on 1) The method of claim 1, wherein the copper powder is a nano-powder having an average grain size less than 250 nanometers. ### Claim 10 (depends on 1) The method of claim 1, wherein the copper powder is a submicron powder having an average grain size less than 1 micron. ### Claim 11 (depends on 1) The method of claim 1, wherein the copper powder is ultra-fine powder having an average grain size less than 100 microns. ### Claim 12 (depends on 1) The method of claim 1, wherein the copper powder is fine powder having an average grain size less than 500 microns. ### Claim 13 A method for removing copper-oxide from copper powder, the method comprising: providing a copper powder defined by a plurality of particles, each particle in the plurality of particles having a copper core and a copper-oxide layer surrounding the copper core, the copper core selected from the group consisting of a pure copper and a copper alloy; disposing the plurality of particles in an etching solution in a container, the etching solution comprising acetic acid and water, wherein the etching solution removes the copper-oxide layer from each particle; decanting the etching solution and the by-products resulting from the copper-oxide removal; washing the plurality of particles, wherein substantially all of the remaining etching solution and substantially all of the by-products are removed from the container holding the plurality of particles; disposing the washed plurality of particles in an organic solvent, the organic solvent comprising tetraethylene glycol and water; directly coating the surface of each copper core in the plurality of particles with an organic material from the organic solvent; dispersing the plurality of particles in the organic solvent; and providing the copper powder as a plurality of dispersed copper cores that are absent a copper-oxide layer surrounding each copper core, each copper core having an organic coating, wherein the steps of disposing in the etching solution, decanting, washing, disposing in the organic solvent, coating, and dispersing in the organic solvent are performed in situ with the plurality of particles disposed in liquid, absent any exposure of the copper cores to air. ### Claim 14 (depends on 13) The method of claim 13, wherein the step of providing the copper powder comprises providing the copper powder in a dry state. ### Claim 15 (depends on 13) The method of claim 13, wherein the step of disposing the plurality of particles in the etching solution further comprises each one of the plurality of particles retaining substantially all of the copper core. ### Claim 16 (depends on 13) The method of claim 13, wherein the etching solution comprises between approximately 0.1% and 1.0% acetic acid. ### Claim 17 (depends on 13) The method of claim 13, further comprising the step of storing the plurality of dispersed and coated copper cores in the organic solvent. ### Claim 18 (depends on 13) The method of claim 13, wherein the copper powder is a nano-powder having an average grain size less than 250 nanometers. ### Claim 19 (depends on 13) The method of claim 13, wherein the copper powder is a submicron powder having an average grain size less than 1 micron. ### Claim 20 (depends on 13) The method of claim 13, wherein the copper powder is ultra-fine powder having an average grain size less than 100 microns. ### Claim 21 (depends on 13) The method of claim 13, wherein the copper powder is fine powder having an average grain size less than 500 microns.