# US 7,608,158 B2 · Method of maintaining particle size > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 7,608,158 B2 - Document ID: US7608158B2 - Status: Granted - Kind: B2 - Application number: 11/374,633 - Filed: 2006-03-13 - Published: 2006-11-02 - Granted: 2009-10-27 - Earliest claimed: 2006-03-13 - Assignees: Board of Regents, The University of Texas System - Inventors: J. Ping Liu - Web page: https://patentgrep.com/patent/US7608158B2 ## CPC - B22F 1/142: Thermal or thermo-mechanical treatment - B22F 2998/00: Supplementary information concerning processes or compositions relating to powder metallurgy - B22F 2998/10: Processes characterised by the sequence of their steps - B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy - C22C 2202/02: Magnetic - 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 The present invention includes particle compositions and methods of fabrication that prevent agglomeration, thereby maintaining particle size and/or shape. Particles of the present invention were prepared after embedding chemically disordered metal-containing particles in at least one salt to form a dispersion. The dispersion of particles in salt was treated to temperatures of at least about 500 degrees Centigrade for several hours. Particles were easily recovered from the dispersion and did not agglomerate. The particles were also absent contaminating salts after performing simple washing and/or rinsing steps. Structural, compositional and/or magnetic characterizations of the metal-containing particles confirmed that they had not agglomerated. When particles with an fcc structure formed a dispersion with at least one salt, the method yielded the formation of particles having an fct structure with high magnetic anisotropy and without a substantial change in size and/or shape. When desired, however, particles shape and/or size may be changed. ## Claims ### Claim 1 A method of maintaining magnetic nanoparticle size comprising: providing two or more magnetic nanoparticles in a nanoscale dispersion, wherein each nanoparticle contains at least one metal, an initial nanoparticle size and shape, and does not interact with a pulverized salt at a treatment temperature; wherein the two or more magnetic nanoparticles are selected from the group consisting of iron-platinum, cobalt-platinum, samarium-cobalt, ceramic material, intermetallic particles, iron-cobalt, and neodymium-iron-boron; mixing the two or more magnetic nanoparticles with the pulverized salt that includes a melting point higher than 500 degrees Centigrade in the nanoscale dispersion; treating the nanoscale dispersion with heat at the treatment temperature that is at least about 500 degrees Centigrade; and isolating the two or more nanoparticles from the nanoscale dispersion, wherein the isolated two or more magnetic nanoparticles have not agglomerated and have an annealed size and shape substantially the same as the initial nanoparticle size and shape. ### Claim 2 (depends on 1) The method of claim 1, wherein heat treating occurs under a reducing or neutral atmosphere for a period of time of at least about one hour to at least about five hours. ### Claim 3 (depends on 1) The method of claim 1, further comprising cooling the dispersion to an ambient temperature before isolating. ### Claim 4 (depends on 3) The method of claim 3, wherein cooling is performed in an environment selected from the group consisting of argon and a forming gas. ### Claim 5 (depends on 1) The method of claim 1, wherein isolating includes washing the dispersion with a washing solution comprising water to remove the at least one salt and then centrifuging at about 6000 rpm for 15 minutes. ### Claim 6 (depends on 5) The method of claim 5, further comprising rinsing the dispersion with a rinsing solution including acetone to remove the water. ### Claim 7 (depends on 1) The method of claim 1, wherein the pulverized salt is is selected from the group consisting of sodium chloride, potassium chloride, calcium chloride, sodium bicarbonate, potassium bicarbonate, calcium bicarbonate and combinations thereof. ### Claim 8 (depends on 1) The method of claim 1, wherein the diameter of the two or more magnetic nanoparticles is in the nanometer scale between at least about 4 and 15 nm and the particles are iron-platinum including an fct structure after the treating the dispersion with step. ### Claim 9 (depends on 1) The method of claim 1, wherein the isolated two or more magnetic nanoparticles exhibit high magnetic anisotropy and coercivity values greater than 2T at room temperature. ### Claim 10 (depends on 1) The method of claim 1, wherein the salt to nanoparticle ratio is selected based upon the annealed size of the particle. ### Claim 11 A method of maintaining magnetic nanoparticle size comprising: providing two or more magnetic particles, wherein each magnetic nanoparticle is selected from the group consisting of iron-platinum, cobalt-platinum, samarium-cobalt, iron-cobalt, and neodymium-iron-boron, each magnetic nanoparticle does not interact with a pulverized salt at a treatment temperature and includes an initial nanoparticle size and shape; mixing the two or more magnetic nanoparticles with the pulverized salt at a salt to nanoparticle weight ratio from 8:1 to 400:1 to form a nanoscale dispersion; treating the nanoscale dispersion with heat at the treatment temperature that is at least about 500 degree Centigrade to obtain an annealed nanoparticle size and shape; and isolating the two or more nanoparticles from the nanoscale dispersion, wherein the isolated two or more magnetic nanoparticles exhibit high magnetic anisotropy without a substantial change in the initial nanoparticle size and shape from the annealed nanoparticle size and shape. ### Claim 12 (depends on 11) The method of claim 11, wherein the pulverized salt is selected from the group consisting of sodium chloride, potassium chloride, calcium chloride, sodium bicarbonate, potassium bicarbonate, calcium bicarbonate and combinations thereof. ### Claim 13 (depends on 11) The method of claim 11, wherein treating occurs under a reducing or neutral atmosphere. ### Claim 14 (depends on 11) The method of claim 11, further comprising cooling the dispersion to an ambient temperature before isolating. ### Claim 15 (depends on 14) The method of claim 14, wherein cooling is performed in an environment selected from the group consisting of argon and a forming gas. ### Claim 16 (depends on 11) The method of claim 11, wherein isolating includes washing the dispersion with a washing solution comprising water to remove the at least one salt. ### Claim 17 (depends on 11) The method of claim 11, further comprising rinsing the dispersion with a rinsing solution to remove the water. ### Claim 18 (depends on 11) The method of claim 11, wherein the diameter of the two or more magnetic nanoparticles is in the nanometer scale. ### Claim 19 (depends on 11) The method of claim 11, wherein the isolated two or more nanoparticles are converted to a different shape or structure and include coercivity values greater than 2T at room temperature. ### Claim 20 (depends on 11) The method of claim 11, wherein the salt to particle ratio is selected based upon the annealed nanoparticle size. ### Claim 21 A method of maintaining magnetic nanoparticle size comprising: a. providing two or more FePt nanoparticle, wherein each FePt nanoparticle contains an initial nanoparticle size and shape, does not interact with a pulverized salt at a treatment temperature, and includes an fcc structure; b. mixing the two or more FePt nanoparticles with the pulverized salt at a pulverized salt to FePt nanoparticle weight ratio from 8:1 to 400:1 and is selected based upon a final annealed size of the FePt nanoparticle, where the pulverized salt includes a melting point higher than 500 degrees Centigrade to form a nanoscale dispersion; c. heat treating the nanoscale dispersion in a reducing atmosphere and at the treatment temperature that is at least about 700 degrees Centigrade; d. cooling the nanoscale dispersion to an ambient temperature in a reducing atmosphere; and e. isolating the two or more FePt nanoparticles from the nanoscale dispersion by washing the nanoscale dispersion to remove the pulverized salt, wherein the isolated two or more FePt nanoparticles have not agglomerated, have an annealed size and shape substantially the same as the initial nanoparticle size and shape, and have an fct structure.