# US 8,784,728 B2 · Micro-grained, cryogenic-milled copper alloys and process > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 8,784,728 B2 - Document ID: US8784728B2 - Status: Granted - Kind: B2 - Application number: 11/567,121 - Filed: 2006-12-05 - Published: 2008-06-05 - Granted: 2014-07-22 - Earliest claimed: 2006-12-05 - Assignees: The Boeing Company - Applicants: Clifford C. Bampton; James D. Cotton; Barun Majumdar - Inventors: Clifford C. Bampton; James D. Cotton; Barun Majumdar - Web page: https://patentgrep.com/patent/US8784728B2 ## CPC - B22F 9/04: starting from solid material, e.g. by crushing, grinding or milling ({C22C1/1084 takes precedence}; crushing, grinding or milling, in general, see the relevant subclasses, e.g. B02C) - C22C 1/0425: {Copper-based alloys} - C22C 9/00: Alloys based on copper - C22C 9/01: with aluminium as the next major constituent - B22F 2009/041: {by mechanical alloying, e.g. blending, milling} - B22F 2009/043: {by ball milling} - B22F 2998/00: Supplementary information concerning processes or compositions relating to powder metallurgy - B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy - 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 - C22C: ALLOYS (treatment of alloys C21D, C22F) ## Abstract There is provided cryogenic milled copper alloys and methods of making the alloys. The alloys are fine grained and possess desirable physical properties stemming from the fine grain size. Embodiments include desirable physical properties, such as potentially high strength. Some embodiments of the cryogenic milled copper alloys may also be tailored for ductility, toughness, fracture resistance, corrosion resistance, fatigue resistance and other physical properties by balancing the alloy composition. In addition, embodiments of the alloys generally do not require extensive or expensive post-cryogenic milling processing. ## Claims ### Claim 1 A method for making a high strength copper alloy comprising: co-milling in liquid nitrogen a first mass of copper powder and a second mass of a metal powder, the metal powder comprised of a second metal that is soluble in copper and that forms stable nitrides under cryogenic milling conditions in the presence of said liquid nitrogen to form a co-milled mass of powder comprising said nitrides, said first mass of copper powder being from about 91 to about 97 wt %, said co-milled mass of powder of powder being free of Be, said stable nitrides formed during said co-milling in the presence of said liquid nitrogen; degassing said co-milled mass of powder; subjecting the co-milled mass of powder to heat and pressure; and consolidating the co-milled mass into a billet comprising an alloy of copper comprising the metal soluble in copper. ### Claim 2 (depends on 1) The method of claim 1, wherein the powder of the second metal is selected from the group of powders of metals consisting of aluminum, zirconium, hafnium, and niobium. ### Claim 3 (depends on 1) The method of claim 1, wherein the second mass of the second metal powder comprises aluminum powder and the step of milling together comprises from about 3 to about 9 wt % of aluminum powder based on the sum of the first mass of copper powder and the aluminum powder. ### Claim 4 (depends on 1) The method of claim 1, wherein the second mass of powder of the second metal comprises aluminum powder and the step of co-milling comprises co-milling about 8 wt. % of the sum of the first mass of copper powder and the aluminum powder. ### Claim 5 (depends on 1) The method of claim 1, wherein the consolidating produces a yellowish, bronze colored billet. ### Claim 6 (depends on 1) The method of claim 1, wherein the consolidating comprises any one or more of hot rolling, hot isostatic pressing, Ceracon forging and powder metallurgy. ### Claim 7 (depends on 1) The method of claim 1, wherein the consolidating process produces a copper alloy having a strength in the range from about 90 to about 110 ksi. ### Claim 8 (depends on 1) The method of claim 1, wherein the consolidating produces a copper alloy having a strength in the range from about 110 to about 140 ksi. ### Claim 9 (depends on 1) The method of claim 1, wherein the consolidating produces a copper alloy comprising nano-scale sized dispersoids of nitrides of the second metal. ### Claim 10 (depends on 1) The method of claim 1, further comprising adding a process control agent and co-milling the process control agent with the copper powder and the second metal powder. ### Claim 11 (depends on 1) The method of claim 1, wherein said co-milling produces a powder having an average grain size of less than 100 nm. ### Claim 12 (depends on 1) The method of claim 1, wherein said nitrides in said powder comprise sub-nanometer sized nitrides. ### Claim 13 (depends on 1) The method of claim 1, wherein the billet has a micro-grain size less than about 10 microns. ### Claim 14 A method for making a high strength micro-grained copper alloy comprising: co-milling in liquid nitrogen from about 97 to about 91 wt % copper powder and from about 3 to about 9 wt % aluminum powder, based on a sum of the weights of copper powder and aluminum powder; forming milled particles of a reddish, copper-color free of silver-colored agglomerates, said milled particles comprising stable nitrides, said milled particles free of Be, said stable nitrides formed during said milling in the presence of said liquid nitrogen; degassing said milled particles; and consolidating the milled particles into a fine grained billet. ### Claim 15 (depends on 14) The method of claim 14, further comprising adding a process control agent and milling the process control agent together with the copper powder and the aluminum powder. ### Claim 16 (depends on 14) The method of claim 14, wherein said milled particles have an average grain size of less than 100 nm. ### Claim 17 (depends on 14) The method of claim 14, wherein said nitrides comprise sub-nanometer sized nitrides. ### Claim 18 (depends on 14) The method of claim 14, wherein the billet has a grain size of less than about 10 microns. ### Claim 19 A method for making a high strength micro-grained copper alloy comprising: co-milling in liquid nitrogen a first mass of copper powder and a second mass of a metal powder, the metal powder comprised of a second metal that is soluble in copper and that forms stable nitrides under cryogenic milling conditions in the presence of said liquid nitrogen, to form a co-milled mass of powder comprising said nitrides, said first mass of copper powder being from about 91 to about 97 wt %, said co-milled mass of powder being free of Be, said stable nitrides formed during said co-milling in the presence of said liquid nitrogen; wherein the second mass of the second metal powder comprises from about 3 to about 9 wt % of aluminum powder; degassing said co-milled mass of powder; subjecting the co-milled mass of powder to heat and pressure; and consolidating the co-milled mass into a billet comprising an alloy of copper comprising the metal soluble in copper. ### Claim 20 (depends on 19) The method of claim 19, wherein said co-milling produces a powder having an average grain size of less than 100 nm. ### Claim 21 (depends on 19) The method of claim 19, wherein said nitrides in said powder comprise sub-nanometer sized nitrides. ### Claim 22 (depends on 19) The method of claim 19, wherein the billet has a micro-grain size of less than about 10 microns.