# US 7,744,835 B2 · Nanostructure material, method for the preparation thereof > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 7,744,835 B2 - Document ID: US7744835B2 - Status: Granted - Kind: B2 - Application number: 11/665,921 - Filed: 2005-10-18 - Published: 2009-10-22 - Granted: 2010-06-29 - Earliest claimed: 2004-10-22 - Assignees: Batscap; Centre National De La Recherche Scientifique - Inventors: Dominique Guyomard; Joël Gaubicher; Marc Deschamps; Matthieu Dubarry; Philippe Moreau - Web page: https://patentgrep.com/patent/US7744835B2 ## CPC - H01M 4/622: {being polymers} - B01J 23/22: Vanadium - H01M 4/133: Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx - H01M 4/625: {Carbon or graphite} - H01M 10/052: Li-accumulators - H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries - H01M 10/0562: Solid materials - H01M 10/0565: Polymeric materials, e.g. gel-type or solid-type - H01M 2004/028: {Positive electrodes} - Y02E 60/10: Energy storage using batteries - Y10S 977/773: Nanoparticle, i.e. structure having three dimensions of 100 nm or less - Y10S 977/811: Of specified metal oxide composition, e.g. conducting or semiconducting compositions such as ITO, ZnOx - Y10T 428/292: In coating or impregnation - Y10T 428/2993: Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.] - 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 - Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract The invention relates to a nanostructured material. The material is a nanostructured carbonaceous material composed of agglomerates of small needles of Li1+αV3O8 and of β-LixV2O5 (0.1≦α≦0.25 and 0.03≦x≦0.667) surrounded by a noncontinuous layer of spherical carbon particles. It is obtained by a process consisting in preparing a carbonaceous precursor gel by bringing carbon, α-V2O5 and a Li precursor into contact in amounts such that the ratio of the [V2O5]/[Li] concentrations is between 1.15 and 1.5 and that the (carbon)/(carbon+V2O5+Li precursor) ratio by weight is from 10 to 15 and in subjecting the gel to a heat treatment comprising a 1st stage at 80° C.-150° C. for 3-12 h and a 2nd stage between 300° C. and 350° C. for 10 min to 1 hour, under an nitrogen or argon atmosphere. Applications: positive electrode active material. ## Claims ### Claim 1 A process for the preparation of a carbonaceous material comprising preparing a carbonaceous precursor gel and subjecting said gel to a heat treatment, wherein: the precursor gel is prepared by bringing carbon, α-V2O5 and a Li precursor into contact in a reaction medium in amounts such that the ratio of the [α-V2O5]/[Li] molar concentrations is between 1.15 and 1.5 and that the (carbon)/(carbon+α-V2O5+Li precursor) ratio by weight is from 10 to 15%; and the heat treatment is carried out in two stages: a first stage at a temperature of between 80° C. and 150° C. for a time of 3 to 12 hours and a second stage under a nitrogen or argon atmosphere at a temperature of between 300° C. and 350° C. for a time of between 10 min and 1 hour. ### Claim 2 (depends on 1) The process as claimed in claim 1, wherein: the Li precursor is LiOH.H2O; and α-V2O5 and LiOH.H2O are introduced into an aqueous carbon suspension under a nitrogen atmosphere. ### Claim 3 (depends on 2) The process as claimed in claim 2, wherein the concentrations of precursors are between 0.75 mol/l and 3 mol/l for α-V2O5 and between 0.55 mol/l and 2.2 mol/l for LiOH.H2O. ### Claim 4 (depends on 1) The process as claimed in claim 1, wherein an aqueous solution comprising from 10 to 50% by volume of hydrogen peroxide is added to the reaction medium. ### Claim 5 (depends on 4) The process as claimed in claim 4, wherein the concentrations are from 0.05 mol/l to 2 mol/l for α-V2O5 and from 0.04 mol/l to 1.5 mol/l for the Li precursor. ### Claim 6 (depends on 4) The process as claimed in claim 4, wherein the lithium precursor is LiOH.H2O, LiCl, LiNO3 or a lithium salt of a carboxylic acid. ### Claim 7 (depends on 6) The process as claimed in claim 6, wherein the lithium salt of carboxylic acid is lithium acetylacetonate, lithium acetate, lithium stearate, lithium formate, lithium oxalate, lithium citrate, lithium lactate, lithium tartrate or lithium pyruvate. ### Claim 8 (depends on 4) The process as claimed in claim 4, wherein an aqueous suspension of α-V2O5 and of carbon is prepared and an aqueous peroxide solution is added thereto, the lithium precursor being introduced into the aqueous suspension of α-V2O5 and of carbon before the addition of the peroxide solution or after the addition of the peroxide solution. ### Claim 9 (depends on 4) The process as claimed in claim 4, wherein the respective amounts of Li precursor and of α-V2O5 in the reaction medium are such that 0.08 mol.l−1<[Li]<0.7 mol.l−1 and 0.1 mol.l−1<[V2O5]<1 mol.l−1. ### Claim 10 A nanostructured carbonaceous material comprising agglomerates of small needles of Li1+αV3O8 and of β-LixV2O5 (0.1≦α≦0.25 and 0.03≦x≦0.667) surrounded by a noncontinuous layer of spherical carbon particles, wherein the Li1+αV3O8 needles and the β-LixV2O5 needles have a length (1) from 40 to 100 nm, a width (w) such that 4