# US 11,439,979 B2 · Method of making colloidal selenium nanoparticles > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,439,979 B2 - Document ID: US11439979B2 - Status: Granted - Kind: B2 - Application number: 16/937,443 - Filed: 2020-07-23 - Published: 2021-12-23 - Granted: 2022-09-13 - Earliest claimed: 2020-06-23 - Assignees: Tripod Nano Technology Corporation - Applicants: Tripod Nano Technology Corporation - Inventors: Chung-Jung Hung; Chun-Lun Chiu; Chia-Chi Chang; Hsin-Chang Huang; Teng-Chieh Hsu; Meng-Hsiu Chih; Jim-Min Fang - Web page: https://patentgrep.com/patent/US11439979B2 ## CPC - B01J 20/3078: {Thermal treatment, e.g. calcining or pyrolizing} - C01B 19/02: Elemental selenium or tellurium - B01J 20/0262: {Compounds of O, S, Se, Te} - B01J 20/3085: {Chemical treatments not covered by groups B01J20/3007 - B01J20/3078} - C01P 2002/84: by UV- or VIS- data - C01P 2002/85: by XPS, EDX or EDAX data - C01P 2002/88: by thermal analysis data, e.g. TGA, DTA, DSC - C01P 2004/04: obtained by TEM, STEM, STM or AFM - C01P 2004/51: Particles with a specific particle size distribution - C01P 2006/40: Electric properties - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS ## Abstract Provided is a method of making colloidal selenium nanoparticles. The method includes the steps as follows: Step (A): providing a reducing agent and an aqueous solution containing a selenium precursor; Step (B): mixing the aqueous solution containing the selenium precursor and the reducing agent to form a mixture solution in a reaction vessel and heating the mixture solution to undergo a reduction reaction and produce a composition containing selenium nanoparticles, residues and a gas, and guiding the gas out of the reaction vessel, wherein an amount of the residues is less than 20% by volume of the mixture solution; and Step (C): dispersing the selenium nanoparticles with a medium to obtain the colloidal selenium nanoparticles. The method has advantages of simplicity, safety, time-effectiveness, cost-effectiveness, high yield and eco-friendliness. ## Claims ### Claim 1 A method of making colloidal selenium nanoparticles, comprising steps of: Step (A): providing a reducing agent and an aqueous solution containing a selenium precursor; Step (B): mixing the aqueous solution containing the selenium precursor and the reducing agent in a reaction vessel to form a mixture solution and heating the mixture solution to undergo a reduction reaction and produce a composition containing selenium nanoparticles, residues and a gas in the reaction vessel, and guiding the gas out of the reaction vessel during the heating; wherein the heating continues until an amount of the residues is less than 20% by volume of the mixture solution; wherein a heating temperature in Step (B) ranges from 50° C. to 200° C.; and Step (C): dispersing the selenium nanoparticles with a medium to obtain the colloidal selenium nanoparticles at a dispersion temperature ranging from 20° C. to 80° C.; wherein the reducing agent comprises a first reducing agent or a second reducing agent; wherein the first reducing agent is selected from the group consisting of: citric acid, lactic acid, glycolic acid, ascorbic acid, oxalic acid, tartaric acid, 1,4-butanediol, glycerol, acetaldehyde, monosaccharide, disaccharide and any combination thereof; and the second reducing agent is selected from the group consisting of: poly(ethylene glycol), polyvinylpyrrolidone, polysaccharide and any combination thereof. ### Claim 2 (depends on 1) The method as claimed in claim 1, wherein the selenium precursor of the aqueous solution comprises a selenium halide, a selenium ion, a selenous acid, a selenite ion, a selenate ion or a selenosulfate ion. ### Claim 3 (depends on 1) The method as claimed in claim 1, wherein guiding the gas out of the reaction vessel during the heating in Step (B) comprises guiding the gas produced from the reduction reaction out of the reaction vessel and then trapping the gas with water in a tank. ### Claim 4 (depends on 1) The method as claimed in claim 1, wherein a heating temperature in Step (B) ranges from 70° C. to 160° C. ### Claim 5 (depends on 1) The method as claimed in claim 1, wherein the dispersion temperature in Step (C) ranges from 50° C. to 80° C. ### Claim 6 (depends on 1) The method as claimed in claim 1, wherein a molar concentration of the selenium precursor of the aqueous solution ranges from 0.05 M to 3.0 M. ### Claim 7 (depends on 6) The method as claimed in claim 6, wherein when the reducing agent comprises the first reducing agent, a molar ratio of the first reducing agent relative to the selenium precursor ranges from 1 to 50. ### Claim 8 (depends on 1) The method as claimed in claim 1, wherein Step (A) comprises: Step (a1): treating a selenium powder with an aqueous solution containing an oxidant to provide the aqueous solution containing the selenium precursor; and Step (a2): providing the reducing agent. ### Claim 9 (depends on 1) The method as claimed in claim 1, wherein the medium in Step (C) comprises water or an aqueous solution including a dispersing agent; wherein the dispersing agent comprises citric acid, lactic acid, poly(lactic acid), ascorbic acid, tannic acid, malic acid, sodium hydroxide, polyarginine, lysine, glutamic acid, asparagine, oleylamine, ethylene glycol, glycerol, glucose, maltose, maltitol, polyvinylpyrrolidone, chitosan, polyvinyl alcohol, poly(ethylene glycol), or any combination thereof. ### Claim 10 (depends on 9) The method as claimed in claim 9, wherein a molar concentration of the dispersing agent ranges from 0.001 M to 1.0 M. ### Claim 11 (depends on 9) The method as claimed in claim 9, wherein a molar ratio of the dispersing agent relative to the selenium nanoparticles ranges from 0.1 to 100.