• 专利标题:   Preparation of three-dimensional graphene grown-composite electrode material used as battery cathode material, involves immersing graphene electrode material in tin tetrachloride and thioacetamide mixture, washing and drying.
  • 专利号:   CN106299315-A, CN106299315-B
  • 发明人:   LIU X, CHAO D, SHEN Z, ZHU C
  • 专利权人:   UNIV HEILONGJIANG SCI TECHNOLOGY
  • 国际专利分类:   B82Y030/00, H01M010/054, H01M004/36, H01M004/58, H01M004/62
  • 专利详细信息:   CN106299315-A 04 Jan 2017 H01M-004/36 201724 Pages: 15 Chinese
  • 申请详细信息:   CN106299315-A CN10899978 14 Oct 2016
  • 优先权号:   CN10899978

▎ 摘  要

NOVELTY - Preparation of three-dimensional graphene grown-composite electrode material involves immersing a flexible three-dimensional graphene electrode material in mixed solution of tin tetrachloride and thioacetamide, reacting at 70-90 degrees C for 35-50 minutes such that plate-like sulfide array is grown on the three-dimensional graphene electrode skeleton, adding anhydrous ethanol, reacting at 70-90 degrees C for 35-50 minutes, removing the electrode material, washing with deionized water and absolute ethanol for 2-4 times and drying in a vacuum oven for 12-24 hours. USE - Preparation of three-dimensional graphene grown-composite electrode material used as battery cathode material. ADVANTAGE - The method provides three-dimensional graphene grown-composite electrode material having coulomb efficiency of more than 90% and storage capacity at low magnification of more than 900 mAh/g, and can be stable for more than 200 cycles. The battery provided with the three-dimensional graphene grown-composite electrode material has high specific capacity. DETAILED DESCRIPTION - Preparation of three-dimensional graphene grown-composite electrode material involves immersing a flexible three-dimensional graphene electrode material in mixed solution of tin tetrachloride and thioacetamide, reacting at 70-90 degrees C for 35-50 minutes such that plate-like sulfide array is grown on the three-dimensional graphene electrode skeleton, adding anhydrous ethanol, reacting at 70-90 degrees C for 35-50 minutes, removing the electrode material, washing with deionized water and absolute ethanol for 2-4 times and drying in a vacuum oven for 12-24 hours. The flexible three-dimensional graphene electrode material is prepared by immersing foamed nickel in 5-10% hydrochloric acid solution for 10-20 minutes, washing the resultant foam with deionized water and anhydrous ethanol for 1-3 times, obtaining cleaned foamed nickel, placing the foamed nickel in a chemical-vapor deposition furnace tube, introducing methane, hydrogen and argon, heating at 1000-1100 degrees C and 10-20 degrees C/minute for 2-15 minutes, cooling the resultant foam to room temperature at 100-200 degrees C/minute, obtaining graphene-coated foamed nickel, immersing the graphene-coated foamed nickel in iron(III) chloride and hydrochloric acid mixed solution for 12-24 hours, removing the foamed nickel, washing with deionized water for 1-3 times, obtaining washed graphene-coated foamed nickel, drying in an oven at 60-80 degrees C for 5-12 hours and obtaining flexible three-dimensional graphene electrode material. The concentration of hydrochloric acid in the iron(III) chloride and hydrochloric acid mixed solution is 5 %mass. The content of iron(III) chloride in the iron(III) chloride and hydrochloric acid mixed solution is 0.3-1 mol/L. The mixed solution of tin tetrachloride and thioacetamide is prepared by adding tin tetrachloride and thioacetamide in molar ratio of 1:3, to anhydrous ethanol, stirring at room temperature and 100-300 rpm for 10-30 minutes. The volume ratio of tin tetrachloride and anhydrous ethanol is (0.6-1 g):50 mL. The volume ratio of the mixed solution of tin tetrachloride and thioacetamide, and absolute ethanol is 1:1.