# US 10,312,517 B2 · In situ formation of sulfur particles using organic acids in the presence of polymer functionalized carbon > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,312,517 B2 - Document ID: US10312517B2 - Status: Granted - Kind: B2 - Application number: 15/339,224 - Filed: 2016-10-31 - Published: 2018-05-03 - Granted: 2019-06-04 - Earliest claimed: 2016-10-31 - Assignees: Toyota Motor Engineering & Manufacturing North America, Inc. - Applicants: Toyota Motor Engineering & Manufacturing North America, Inc. - Inventors: John Muldoon; Claudiu B. Bucur - Web page: https://patentgrep.com/patent/US10312517B2 ## CPC - H01M 4/604: {containing aliphatic main chain polymers} - B01J 13/06: by phase separation - H01M 4/0497: {Chemical precipitation} - H01M 4/13: Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof - H01M 4/139: Processes of manufacture - H01M 4/366: {as layered products} - H01M 4/38: of elements or alloys - H01M 4/382: {Lithium (H01M4/405 takes precedence)} - H01M 4/622: {being polymers} - H01M 4/623: {fluorinated polymers} - H01M 4/625: {Carbon or graphite} - H01M 10/052: Li-accumulators - H01M 2004/021: {Physical characteristics, e.g. porosity, surface area} - H01M 2004/028: {Positive electrodes} - H01M 2220/20: Batteries in motive systems, e.g. vehicle, ship, plane - Y02E 60/10: Energy storage using batteries - Y02T 10/70: Energy storage systems for electromobility, e.g. batteries - H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION - Y02T: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION ## Abstract A sulfur particle containing a core of elemental sulfur having homogeneously dispersed particles of a conductive carbon and branched polyethyleneimine; and a coating of branched polyethyleneimine (bPEI) encapsulating the core is provided. In the sulfur particle the dispersed particles of conductive carbon are associated with the bPEI. A cathode having an active material containing the sulfur particles and a sulfur loading of 1.0 mg S/cm2 to 10 mg/cm2 and a battery containing the cathode are also provided. ## Claims ### Claim 1 A sulfur particle, comprising: a core of elemental sulfur comprising particles homogeneously dispersed within the core; and a coating of branched polyethyleneimine (bPEI) encapsulating the core; wherein the homogeneously dispersed particles comprise a conductive carbon and branched polyethyleneimine. ### Claim 2 (depends on 1) The sulfur particle of claim 1, wherein a content of the conductive carbon in the elemental sulfur core is from 0.01 to 1.0% by weight of a total weight of the elemental sulfur core. ### Claim 3 (depends on 1) The sulfur particle of claim 1, further comprising conductive carbon on the bPEI coating. ### Claim 4 (depends on 3) The sulfur particle of claim 3, wherein a total content of conductive carbon within the elemental sulfur core and on the bPEI coating is from 0.01 to 5.0% by weight of a total weight of the sulfur particle. ### Claim 5 (depends on 1) The sulfur particle of claim 1 wherein a diameter of the core of elemental sulfur is from 200 to 1,000 nm. ### Claim 6 (depends on 1) The sulfur particle of claim 1 wherein the conductive carbon is a carbon black. ### Claim 7 (depends on 1) A method for preparing the sulfur particle of claim 1, comprising: mixing a conductive carbon in water with a branched chain polyethyleneimine (bPEI); mechanically dispersing the conductive carbon in association with the bPEI; preparing a precursor aqueous solution of at least one of a thiosulfate and a polysulfide; adding bPEI to the precursor aqueous solution; adding an organic acid to the precursor aqueous solution to precipitate elemental sulfur and obtain the sulfur particle; wherein the dispersed conductive carbon associated with bPEI is added to the precursor aqueous solution with the organic acid. ### Claim 8 (depends on 7) The method of claim 7, wherein the organic acid is at least one selected from the group consisting of oxalic acid, malic acid, succinic acid, glutaric acid adipic acid and ascorbic acid. ### Claim 9 (depends on 7) The method of claim 7, wherein a zeta potential of the conductive carbon in association with the bPEI is less than −35 mV. ### Claim 10 (depends on 1) A cathode comprising: a conductive substrate, and an active material comprising the sulfur particles of claim 1. ### Claim 11 (depends on 10) The cathode of claim 10, wherein the active material further comprises: a binder; and a conductive carbon. ### Claim 12 (depends on 11) The cathode of claim 11, wherein a content of the sulfur particles is from 50 to 90% by weight; a content of the binder is from 2 to 10% by weight; and a content of the conductive carbon is from 0 to 30% by weight; wherein the weight % is relative to a total weight of the active material. ### Claim 13 (depends on 12) A battery comprising: an anode comprising lithium; and the cathode of claim 12; wherein a loading of sulfur is from 1.0 mg S/cm2 to 10 mg/cm2. ### Claim 14 (depends on 11) The cathode of claim 11 wherein the binder is a Nafion copolymer. ### Claim 15 (depends on 11) The cathode of claim 11, wherein the conductive carbon is at least one selected from the group consisting of carbon black, acetylene black, vapor grown carbon fiber, graphene, natural graphite, artificial graphite, fulierenes, hard carbon, mesocarbon microbeads and activated carbon. ### Claim 16 (depends on 10) The cathode of claim 10, wherein a loading of sulfur is from 1.0 mg S/cm2 to 10 mg/cm2. ### Claim 17 (depends on 10) The cathode of claim 10, wherein a loading of sulfur is from 3.0 mg S/cm2 to 5 mg/cm2. ### Claim 18 (depends on 10) A battery, comprising: an anode comprising a metal as an active source of metal ions, and the cathode of claim 10. ### Claim 19 (depends on 18) The battery of claim 18, wherein the metal of the anode is lithium, and a loading of sulfur is from 1.0 mg S/cm2 to 10 mg/cm2. ### Claim 20 (depends on 19) The battery of claim 19, wherein the loading of sulfur is from 3.0 mg S/cm2 to 5 mg/cm2.