• 专利标题:   Manufacture of lithium-sulfur battery positive electrode material involves adding positive electrode material such as sulfur, carbon-sulfur composite material or organic polysulfur compound in solution containing nano two-dimensional hydroxyl transition metal oxide, stirring, washing and drying.
  • 专利号:   CN116154124-A
  • 发明人:   JIN C, WANG W, LU J
  • 专利权人:   PLA ACAD MILITARY SCI CHEM DEFENSE INST
  • 国际专利分类:   B82Y040/00, H01M010/052, H01M004/36, H01M004/38, H01M004/60, H01M004/62
  • 专利详细信息:   CN116154124-A 23 May 2023 H01M-004/36 202351 Chinese
  • 申请详细信息:   CN116154124-A CN11437205 17 Nov 2022
  • 优先权号:   CN11437205

▎ 摘  要

NOVELTY - Manufacture of lithium-sulfur battery positive electrode material involves dissolving transition metal salt in distilled water and protecting under nitrogen, dripping a distilled aqueous solution containing a reducing agent chosen from sodium sulfite, stannous chloride, oxalic acid, potassium borohydride, sodium borohydride, and ethanol and basic compound chosen from sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate, and sodium dihydrogen phosphate to the transition metal salt solution at 0.1-2 mL/minutes, continuing stirring reaction for 1-3 hours to obtain a nano two-dimensional hydroxyl transition metal oxide precursor, dissolving the precursor in an alcohol solvent, stirring to obtain a nanometer two-dimensional hydroxyl transition metal oxide, placing the metal oxide in 100 ml weakly acidic aqueous solution, stirring and placing 1-5 g lithium-sulfur battery positive electrode material, stirring, washing the obtained product and drying. USE - Manufacture of lithium-sulfur battery positive electrode material. ADVANTAGE - The prepared nano two-dimensional hydroxyl transition metal oxide can modulate the microscopic electronic structure of the material and improve the reactivity, promote the ring-opening polymerization of 1,3 dioxolane in the ether-based electrolyte, realize in-situ surface gelation, effectively inhibit the side reactions, volume expansion and dissolution of intermediate products accompanying the charge and discharge process, and has high specific capacity and high volumetric energy density and excellent cycle stability. DETAILED DESCRIPTION - Manufacture of lithium-sulfur battery positive electrode material involves dissolving 0.03-0.18 mol transition metal salt in 100 ml distilled water and protecting under nitrogen, dripping a distilled aqueous solution containing reducing agent and basic compound to the transition metal salt solution at 0.1-2 mL/minutes, in which the lower speed is 100-200 rpm/minute and stirring for 1-2 hours, after the reducing agent and the basic compound solution are dripped, continuing stirring reaction for 1-3 hours to obtain a nano two-dimensional hydroxyl transition metal oxide precursor, dissolving the precursor in an alcohol solvent, stirring at 500-800 rpm in an open environment at room temperature for 12-48 hours, to obtain a nanometer two-dimensional hydroxyl transition metal oxide, placing the metal oxide in 100 ml weakly acidic aqueous solution, at pH value of 5-7 and rotation speed of 100-200 rpm, stirring for 2-5 hours, and placing 1-5 g lithium-sulfur battery positive electrode material, stirring for 1-2 hours at a rotation speed of 100-200 rpm, washing the obtained product with 50-100 mL/time methanol and 50-100 mL/time deionized water, and drying at a vacuum degree of -0.01-0.02 MPa for 12 hours. The transition metal salt is one or more of ferric nitrate, ferric chloride, ferric sulfate, ferrous sulfate, ferric oxalate, 2-hydroxy ferric propionate, iron carboxylate, nickel nitrate, nickel chloride, nickel sulfate, nickel oxalate, cobalt nitrate, cobalt chloride, cobalt sulfate, cobalt oxalate, manganese nitrate, manganese chloride, manganese sulfate, and manganese oxalate. The molar concentration of the transition metal salt in the transition metal salt solution is 0.3-1.8 mol/L. The reducing agent is one or more of sodium sulfite, stannous chloride, oxalic acid, potassium borohydride, sodium borohydride, and ethanol. The molar ratio of transition metal salt and reducing agent is 1: 1.5-5.5. The basic compound is sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate, or sodium dihydrogen phosphate. The mass ratio of the total mass of the transition metal salt and the reducing agent to the basic compound is 1:0.05-0.1. The alcohol solvent is one or more of methanol, ethanol, ethylene glycol, or diethylene glycol. The weakly acidic aqueous solution is one or more of acetic acid, carbonic acid, silicic acid, nitrous acid, hydrosulfuric acid, hydrofluoric acid, hypochlorous acid, hydrocyanic acid, sulfurous acid, and phosphoric acid. The mass ratio of the nanometer two-dimensional hydroxyl transition metal oxide to the positive electrode material of the lithium-sulfur battery is 100:1.0-10.0. The positive electrode material of the lithium-sulfur battery is one or more of elemental sulfur, carbon-sulfur composite materials, and organic polysulfur compounds. The carbon-sulfur composite material is a mesoporous carbon-based sulfur composite material, a carbon nanotube-based carbon-sulfur composite material or a graphene-based carbon-sulfur composite material. The organic polysulfide compound is sulfurized polyacrylonitrile, thiocyanuric acid or sulfurized polypropylene.