• 专利标题:   Synthesis of sheet-shaped lithium-manganese phosphate-graphene composite used for electrode material of lithium-ion battery, adding aqueous graphene oxide solution to carbon-coated lithium-manganese phosphate sheet, and spray-drying.
  • 专利号:   CN103928680-A
  • 发明人:   CHEN Y, JIAO Z, JIANG Y, QUE X, XU W, WU M, ZHAO B, LU M
  • 专利权人:   UNIV SHANGHAI
  • 国际专利分类:   H01M004/58
  • 专利详细信息:   CN103928680-A 16 Jul 2014 H01M-004/58 201468 Pages: 12 Chinese
  • 申请详细信息:   CN103928680-A CN10112130 24 Mar 2014
  • 优先权号:   CN10112130

▎ 摘  要

NOVELTY - Organic carbon source is dissolved in organic solvent (b), obtained solution is added to sheet of lithium-manganese phosphate, and calcined to obtain organic carbon source-coated sheet of lithium-manganese phosphate. The obtained material is added to tubular furnace, and heated to obtain carbon-coated lithium-manganese phosphate sheet. Aqueous graphene oxide solution is added to carbon-coated lithium-manganese phosphate sheet, spray-dried, and calcined to obtain sheet-shaped lithium-manganese phosphate-graphene composite. USE - Synthesis of sheet-shaped lithium-manganese phosphate-graphene composite used for electrode material of lithium-ion battery. ADVANTAGE - The method provides sheet-shaped lithium-manganese phosphate-graphene composite having high stability, high tap density and excellent conductivity, by a simple process. DETAILED DESCRIPTION - Manganese source is dissolved in deionized water, and resulting mixture is added to three-necked round bottom flask filled with predetermined amount of organic solvent (a). The mixed solution is heated, stirred at 90-150 degrees C for 1-5 hours, aqueous solution of phosphorus source and lithium source is added to the obtained solution at a speed of 1-5 ml/minute and cooled for 2-6 hours. The resulting solution is centrifuged, washed with deionized water and ethanol, and dried at 60-100 degrees C to obtain sheet of lithium-manganese phosphate. A predetermined amount of organic carbon source is dissolved in organic solvent (b), obtained solution is added to sheet of lithium-manganese phosphate, ultrasonic processing is carried out for 10-60 minutes, and calcined to obtain organic carbon source-coated sheet of lithium-manganese phosphate. The obtained material is ground to powder, powder is added to tubular furnace, heated at 300-600 degrees C for 2-8 hours under inert atmosphere at a rate of 1-30 degrees C/minute, and gas flow rate of 10-50 ml/minute to obtain carbon-coated lithium-manganese phosphate sheet. Aqueous graphene oxide solution is added to carbon-coated lithium-manganese phosphate sheet in 1-4 hours, ultrasonic processing is carried out at 140-250 degrees C for 10-60 minutes, and spray-dried. The resulting material is added to tubular furnace, and calcined at 400-800 degrees C for 2-8 hours under inert nitrogen atmosphere at heating rate of 1-30 degrees C/minute and gas flow rate of 10-50 ml/minute to obtain sheet-shaped lithium-manganese phosphate-graphene composite. The molar ratio of lithium, manganese and phosphorus is 1-1.1:1:1. Lithium source is lithium sulfate. Manganese source is manganese sulfate. Phosphorus source is ammonium phosphate. The organic solvent (a) is diethylene glycol. The molar ratio of sheet of lithium-manganese phosphate and carbon source is 1:20-1:10. The organic carbon source is glucose. The organic solvent (b) is methanol. The inert gas atmosphere is nitrogen source. The addition amount of graphene oxide to lithium-manganese phosphate is 1-5 wt.%.