• 专利标题:   Preparing nano lithium titanate-graphene porous composite electrode material, comprises preparing graphite oxide dry powder by Hummers method, ball milling dry powder, sintering and cooling naturally to room temperature.
  • 专利号:   CN111392766-A
  • 发明人:   XIANG Y, ZHAO P, CAO G, ZHANG W, ZHANG H, JIN C, QIU J, MING H
  • 专利权人:   PLA ACAD MILITARY SCI CHEM DEFENSE INST
  • 国际专利分类:   B82Y030/00, B82Y040/00, C01B032/184, C01G023/00
  • 专利详细信息:   CN111392766-A 10 Jul 2020 C01G-023/00 202064 Pages: 8 Chinese
  • 申请详细信息:   CN111392766-A CN11103696 13 Nov 2019
  • 优先权号:   CN11103696

▎ 摘  要

NOVELTY - Preparing nano lithium titanate-graphene porous composite electrode material, comprises (i) preparing graphite oxide dry powder by Hummers method or modified Hummers method, (ii) dissolving the titanium source in a mixed system of organic solvent and acetic acid and stirring evenly to obtain sol A, (iii) adding lithium source to sol A and mixing uniformly to obtain dispersion B, (iv) adding dry graphite oxide powder to dispersion B, and ball milling to obtain a suspension slurry of nanometer lithium titanate precursor intercalated graphite oxide, (v) placing the nano-lithium titanate precursor intercalated graphite oxide suspension slurry 60-150 degrees C to completely dry, (vi) ball milling the dry powder of nanometer lithium titanate precursor intercalated graphite oxide at a speed of 200-800 revolutions/minute for 1-5 hours, and placing in an inert atmosphere for sintering, heating to 750-900 degrees C at a rate of 3-10 degrees C/min, keeping at constant temperature for 1-6 hours, and cooling. USE - The method is useful for preparing nano lithium titanate-graphene porous composite electrode material. ADVANTAGE - The method has good consistency and high concentration of graphene oxide suspension, good repeatability and potential industrial application value. The composite material has excellent high-rate performance, capacity of 100mAh g/1 at a rate of 100 C, and reaching the international advanced level. DETAILED DESCRIPTION - Preparing nano lithium titanate-graphene porous composite electrode material, comprises (i) using 300-8000 mesh natural flake graphite as raw material, preparing graphite oxide dry powder by Hummers method or modified Hummers method, (ii) dissolving the titanium source in a mixed system of organic solvent and acetic acid and stirring evenly to obtain sol A, where the mass ratio of titanium source to organic solvent is 1:0.25-9, and the volume ratio of organic solvent to acetic acid in the mixed system is 1:0.03-0.1, (iii) adding the lithium source to sol A and mixing uniformly to obtain dispersion B, where the molar ratio of lithium to titanium is 1:0.8-0.9, (iv) adding dry graphite oxide powder to dispersion B, and ball milling at a speed of 200-800 revolutions/minute for 5-10 hours to obtain a suspension slurry of nanometer lithium titanate precursor intercalated graphite oxide, where the titanium source and graphite oxide dry powder is 1:0.5-0.05, (v) placing the nano-lithium titanate precursor intercalated graphite oxide suspension slurry at 60-150 degrees C to completely dry it to obtain a dry powder of nano-lithium titanate precursor intercalated graphite oxide, (vi) ball milling the dry powder of nanometer lithium titanate precursor intercalated graphite oxide at a speed of 200-800 revolutions/minute for 1-5 hours, and placing in an inert atmosphere for sintering, heating to 750-900 degrees C at a rate of 3-10 degrees C/min, keeping at constant temperature for 1-6 hours, and cooling down naturally to obtain nano lithium titanate/graphene porous composite material, where the titanium source comprises tetrabutyl titanate, isopropyl titanate, n-propyl titanate, ethyl titanate, titanium sulfate, titanium chloride or orthotitanic acid, the organic solvent is methanol, ethanol, propanol or butanol, the lithium source comprises lithium hydroxide, lithium carbonate or lithium acetate and the inert atmosphere is argon or nitrogen.