# US 10,479,696 B2 · Method for preparing molybdenum oxide nanoparticles > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,479,696 B2 - Document ID: US10479696B2 - Status: Granted - Kind: B2 - Application number: 15/178,609 - Filed: 2016-06-10 - Published: 2016-12-15 - Granted: 2019-11-19 - Earliest claimed: 2015-06-12 - Assignees: University-Industry Cooperation Group of Kyung Hee University - Applicants: University-Industry Cooperation Group of Kyung Hee University - Inventors: Jinsoo Kim; Sang Hyuk Im; Su Ha; Han-Seul Choi; Woo-Sik Kim; Sung Pil Yoon; Jonghee Han - Web page: https://patentgrep.com/patent/US10479696B2 ## CPC - C01G 39/02: Oxides; Hydroxides - B01J 2/04: in a gaseous medium {(if combined with suspending the material in a gas, e.g. fluidised beds B01J2/16)} - C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram - C01P 2004/03: obtained by SEM - C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer - C01P 2006/12: Surface area - C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20) - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS ## Abstract Provided is a method for preparing molybdenum oxide nanoparticles, including (a) preparing a precursor solution by dissolving a molybdenum salt in a first polar solvent, (b) generating an aerosol by applying ultrasonic waves to the precursor solution, and spraying the aerosol to a pre-heated reactor using a carrier gas, (c) obtaining molybdenum oxide micron-sized particles by pyrolyzing the aerosol, and (d) obtaining molybdenum oxide nanoparticles by dispersing the molybdenum oxide micron-sized particles in a second polar solvent and performing a solvothermal reduction reaction. ## Claims ### Claim 1 A method for preparing molybdenum oxide nanoparticles, comprising: (a) preparing a precursor solution by dissolving a molybdenum salt in a first polar solvent; (b) generating an aerosol by applying ultrasonic waves to the precursor solution, and spraying the aerosol to a pre-heated reactor using a carrier gas; (c) obtaining molybdenum oxide micron-sized particles by pyrolyzing the aerosol; and (d) obtaining molybdenum oxide nanoparticles by dispersing the molybdenum oxide micron-sized particles in a second polar solvent and performing a solvothermal reduction reaction, wherein the molybdenum oxide micron-sized particles are polycrystalline, wherein a BET specific surface area of the molybdenum oxide nanoparticles is at least 100 m2/g. ### Claim 2 (depends on 1) The method of claim 1, wherein the molybdenum salt is one selected from the group consisting of lithium molybdate (Li2MoO4), calcium molybdate (CaMoO4), potassium molybdate (K2MoO4), sodium molybdate (NaMoO4), molybden chloride (MoCl5, MoCl3, MoOCl4), ammonium molybdate ((NH4)6Mo7O24.H2O), and a mixture thereof. ### Claim 3 (depends on 1) The method of claim 1, wherein the first polar solvent is one selected from the group consisting of methanol, ethanol, propanol, butanol, methoxyethanol, ethoxyethanol, lactone, acetonitrile, n-methyl-2-pyrrolidone (NMP), formic acid, nitromethane, acetic acid, dimethylsulfoxide, distilled water, and a mixture thereof. ### Claim 4 (depends on 1) The method of claim 1, wherein a concentration of the precursor solution is in a range of 0.05 to 0.5 M. ### Claim 5 (depends on 1) The method of claim 1, wherein the carrier gas is one selected from the group consisting of air, nitrogen, oxygen, helium, argon, and a mixture thereof. ### Claim 6 (depends on 1) The method of claim 1, wherein, in the step (c), the pyrolysis temperature is in a range of 450 to 650° C. ### Claim 7 (depends on 1) The method of claim 1, wherein, in the step (c), the molybdenum oxide micron-sized particles are molybdenum trioxide (MoO3). ### Claim 8 (depends on 1) The method of claim 1, wherein the second polar solvent is a mixture of distilled water and a reducing solvent. ### Claim 9 (depends on 8) The method of claim 8, wherein the second polar solvent is prepared by mixing the distilled water and the reducing solvent in a weight ratio of 1 to 3:1. ### Claim 10 (depends on 6) The method of claim 6, wherein, in the step (c), the pyrolysis temperature is in a range of 560 to 640° C. ### Claim 11 (depends on 10) The method of claim 10, wherein, in the step (d), the solvothermal reduction reaction is performed at least for 10 hours. ### Claim 12 (depends on 6) The method of claim 6, wherein, in the step (c), the pyrolysis temperature is in a range of 460 to 540° C. ### Claim 13 (depends on 12) The method of claim 12, wherein, in the step (d), the solvothermal reduction reaction is performed at least for 2 hours. ### Claim 14 (depends on 1) The method of claim 1, wherein, in the step (d), the solvothermal reduction reaction temperature is in a range of 100 to 300° C. ### Claim 15 (depends on 1) The method of claim 1, wherein the molybdenum oxide nanoparticles are represented by Formula 1: MoO3-X [Formula 1] where X is 0