# US 10,245,642 B2 · Methods for producing metal powders > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,245,642 B2 - Document ID: US10245642B2 - Status: Granted - Kind: B2 - Application number: 15/051,267 - Filed: 2016-02-23 - Published: 2016-08-25 - Granted: 2019-04-02 - Earliest claimed: 2015-02-23 - Assignees: Nanoscale Powders LLC - Applicants: Nanoscale Powders LLC - Inventors: David Henderson; Andrew Matheson; Richard Van Lieshout; Donald Finnerty; John W. Koenitzer - Web page: https://patentgrep.com/patent/US10245642B2 ## CPC - B22F 9/24: starting from liquid metal compounds, e.g. solutions - B22F 9/20: starting from solid metal compounds - C22B 5/04: by aluminium, other metals or silicon - B22F 1/054: Nanosized particles - B22F 1/056: {Submicron particles having a size above 100 nm up to 300 nm} - B22F 2201/10: Inert gases - B22F 2202/17: use of centrifugal or vortex forces - B22F 2301/052: Aluminium - B22F 2301/054: Alkali metals, i.e. Li, Na, K, Rb, Cs, Fr - B22F 2301/056: Alkaline metals, i.e. Ca, Sr, Ba, Ra - B22F 2302/45: Others, including non-metals - 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 - C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS ## Abstract A method for producing a metal powder includes maintaining molten reducing metal in a sealed reaction vessel that is substantially free of oxygen and water, establishing a vortex in the molten reducing metal, introducing a metal halide into the vortex so that the molten reducing metal is in a stoichiometric excess to the metal halide, thereby producing metal particles and salt, removing unreacted reducing metal, removing the salt, and recovering the metal powder. The molten reducing metal can be a Group I metal, a Group II metal, or aluminum. ## Claims ### Claim 1 A method for producing a metal powder, the method comprising: a) maintaining molten reducing metal in a sealed reaction vessel that is free of oxygen and water, the molten reducing metal comprising a Group I metal, a Group II metal, or aluminum; b) establishing a vortex in the molten reducing metal by stirring the molten reducing metal with a bladed stirrer in the reaction vessel at a speed of about 500 rpm to about 6000 rpm; c) introducing a metal halide into the vortex so that the molten reducing metal is in a stoichiometric excess to the metal halide, thereby producing metal particles and a salt; d) removing unreacted reducing metal; e) removing the salt; and f) recovering the metal powder. ### Claim 2 (depends on 1) The method of claim 1, wherein the metal halide includes a chloride of tantalum, nickel, aluminum, zirconium, vanadium, tin, titanium, silicon, niobium, or hafnium. ### Claim 3 (depends on 2) The method of claim 2, wherein the molten reducing metal comprises sodium. ### Claim 4 (depends on 2) The method of claim 2, wherein the molten reducing metal comprises potassium. ### Claim 5 (depends on 2) The method of claim 2, wherein the molten reducing metal comprises sodium and potassium. ### Claim 6 (depends on 2) The method of claim 2, wherein the molten reducing metal comprises magnesium. ### Claim 7 (depends on 2) The method of claim 2, wherein the molten reducing metal comprises calcium. ### Claim 8 (depends on 2) The method of claim 2, wherein the molten reducing metal comprises aluminum. ### Claim 9 (depends on 2) The method of claim 2, wherein the molten reducing metal is maintained at a temperature of about 150° C. to about 850° C. ### Claim 10 (depends on 9) The method of claim 9, wherein the molten reducing metal is maintained at a temperature of about 150° C. to about 350° C. ### Claim 11 (depends on 10) The method of claim 10, wherein the molten reducing metal is maintained at a temperature of about 200° C. to about 250° C. ### Claim 12 (depends on 2) The method of claim 2, wherein the molten reducing metal is maintained at a temperature of about 600° C. to about 700° C. ### Claim 13 (depends on 2) The method of claim 2, wherein the molten reducing metal is in at least a 5:1 stoichiometric excess to the metal halide. ### Claim 14 (depends on 1) The method of claim 1, wherein the metal halide is a mixture of metal halides. ### Claim 15 (depends on 1) The method of claim 1, wherein the vortex is created by stirring the molten reducing metal with a bladed stirrer in the reaction vessel at a speed of about 1000 rpm to about 4000 rpm. ### Claim 16 (depends on 1) The method of claim 1, wherein the vortex is created by stirring the molten reducing metal with a bladed stirrer in the reaction vessel at a tip speed of about 4000 feet per minute to about 6000 feet per minute. ### Claim 17 (depends on 1) The method of claim 1, wherein the reaction vessel that is free of oxygen and water is filled or purged with an inert gas prior to or while maintaining the molten reducing metal in the sealed reaction vessel. ### Claim 18 (depends on 1) The method of claim 1, wherein removing the unreacted reducing metal comprises siphoning off the unreacted reducing metal. ### Claim 19 (depends on 1) The method of claim 1, wherein removing the unreacted molten reducing metal comprises evaporating the unreacted reducing metal. ### Claim 20 (depends on 1) The method of claim 1, wherein removing the unreacted reducing metal comprises reacting the unreacted reducing metal with an anhydrous chloride. ### Claim 21 (depends on 20) The method of claim 20, wherein the anhydrous chloride is anhydrous hydrogen chloride or chloride gas. ### Claim 22 (depends on 1) The method of claim 1, wherein removing the salt comprises washing the metal particles with water. ### Claim 23 (depends on 1) The method of claim 1, wherein removing the salt comprises evaporating by heating and sweeping with an inert gas. ### Claim 24 (depends on 1) The method of claim 1, further comprising drying the metal powder after recovering the metal powder. ### Claim 25 (depends on 1) The method of claim 1, wherein the metal powder is an alloy. ### Claim 26 (depends on 1) The method of claim 1, wherein the metal halide comprises a powder. ### Claim 27 (depends on 1) The method of claim 1, wherein the metal halide comprises a liquid.