专利号:US-7601318-B2 优先权日:2000-09-26 标 题:Method for synthesis of carbon-coated redox materials with controlled size 发明人:ARMAND MICHEL; GAUTHIER MICHEL; MAGNAN JEAN-FRANCOIS; RAVET NATHALIE 权利人:HYDRO QUEBEC; CENTRE NAT RECH SCIENT; UNIV MONTREAL 摘要:A method for the synthesis of compounds of the formula C—Li x M 1−y M′ y (XO 4 ) n , where C represents carbon cross-linked with the compound Li x M 1−y M′ y (XO 4 ) n , in which x, y and n are numbers such as 0≦x≦2, 0≦y≦0.6, and 1≦n≦1.5, M is a transition metal or a mixture of transition metals from the first period of the periodic table, M′ is an element with fixed valency selected among Mg 2+ , Ca 2+ , Al 3+ , Zn 2+ or a combination of these same elements and X is chosen among S, P and Si, by bringing into equilibrium, in the required proportions, the mixture of precursors, with a gaseous atmosphere, the synthesis taking place by reaction and bringing into equilibrium, in the required proportions, the mixture of the precursors, the procedure comprising at least one pyrolysis step of the carbon source compound in such a way as to obtain a compound in which the electronic conductivity measured on a sample of powder compressed at a pressure of 3750 Kg·cm −2 is greater than 10 −8 S·cm −1 . The materials obtained have excellent electrical conductivity, as well a very improved chemical activity.
专利号:US-9174846-B2 优先权日:2009-09-18 标题 :Ferric phosphate and methods of preparation thereof 发明人:BECK LARRY W; SOLTANI MAHROKH; WANG LIYA 权利人:BECK LARRY W; SOLTANI MAHROKH; WANG LIYA; A123 SYSTEMS LLC 摘要:High-purity crystalline ferric phosphate material with desirable characteristics for use in synthesis of nano-sized LFP cathode material are described. The ferric phosphate dihydrate material has as disclosed herein has a molar ratio of phosphorous to iron is from about 1.001 to about 1.05, a surface area of from about 25 m 2 /g to about 65 m 2 /g, and is substantially free of metallic or magnetic impurities. Methods of synthesizing high-purity crystalline ferric phosphate material with desirable characteristics for use in synthesis of nano-sized LFP cathode material are also described. In some embodiments, one or more magnetic traps are used during the reaction process and/or after the formation of the final product to remove magnetic impurities. In some embodiments, a synthetic method of ferric phosphate using multiple steps is described, wherein the intermediate of the synthesis is isolated and purified to improve the purity of the ferric phosphate material. In some embodiments, an iron compound is added to an aqueous solution of phosphoric acid. The solution pH and temperature are controlled to ensure the complete dissolution of the iron compound. The desired iron phosphate crystalline material can be obtained with high purity and high crystalline phase purity by controlling the pH and temperature of the solution.
专利号:US-2024025744-A1 优先权日:2022-07-22 标 题 :Method for preparing ultra cheap iron phosphate 发明人:HUANG ROBERT BRIAN; HUANG RICHARD BRIAN 权利人:HUANG ROBERT BRIAN; HUANG RICHARD BRIAN; WATIX TECH LLC 摘要:This method synthesizes low-cost, high-performance iron phosphate that can be used for producing lithium-ion battery cathodes. It has three main steps: (S1) the synthesis of a iron (II,III) phosphate solution by mixing waste iron oxide (FeO, Fe 2 O 3 ), low purity iron powder, and sulfuric acid in an aqueous solvent, followed by the addition of phosphoric acid; (S2) the addition of hydrogen peroxide to the previous solution, followed by pH balancing chemicals to yield crude iron phosphate; and (S3) the stirring of the previous solution to precipitate iron (III) phosphate, followed by an aging step, a filtering step, a washing step, and a drying step to obtain iron phosphate, which may be in the form of a hydrate. This straightforward approach uses waste iron oxide to minimize costs, while still yielding a fairly pure iron phosphate with excellent capacity, cycling stability, and broad physical and chemical properties suitable for battery production.
专利号:US-2004033360-A1 优先权日:2000-09-26 标 题 :Method for synthesis of carbon-coated redox materials with controlled size
专利号:US-2010065787-A1 优先权日:2000-09-26 标题 :Method for synthesis of carbon-coated redox materials with controlled size
专利号:CN-106876705-B 优先权日:2017-03-31 标 题:A kind of preparation method of in-situ synthesis of carbon/carbon nanotube-coated lithium iron phosphate composite material
参考文献:10.1134/s1027451023030266 摘要:Isaev DD, Kriventsov VV, Petrov SA, Bystrov VS, Bulina NV. Substitution in the Structure of Hydroxyapatite Doped with Iron Cations Upon Mechanochemical Synthesis. J. Surf. Investig. 2023 Jun;17(3):687–93. doi: 10.1134/s1027451023030266. 参考文献:10.1007/s42461-023-00896-x 摘要:Pandey N, Biswas A, Tripathy SK. Hydrometallurgical Processing of Low-Grade Ni-Rich Chromite Overburden. Mining, Metallurgy & Exploration. 2023 Dec 28;41(1):1–20. doi: 10.1007/s42461-023-00896-x.