▎ 摘 要
NOVELTY - 0.05-5 g Ferrous phosphate/three-dimensional graphene composite, 0.05-5 g lithium source and 0.05-5 g carbon source are placed in agate mortar, and 10-30 mL ethanol is added and ground. Mixture is placed in tubular furnace under argon atmosphere at the heating rate of 2-10 degrees C, pre-heated and calcined sample is removed. To resultant material, 0.05-5 g carbon source is added, and ground under argon gas at heating rate of 2-10 degrees C/minute at 300-800 degrees C for 1 to 20 hours, to obtain lithium iron phosphate/three-dimensional graphene/carbon composite material. USE - Preparation of lithium iron phosphate/three-dimensional graphene/carbon composite material. ADVANTAGE - The method efficiently and economically provides lithium iron phosphate/three-dimensional graphene/carbon composite material having excellent cycle performance and electrochemical performance, by simple method without affecting the environment. DETAILED DESCRIPTION - Ferrous phosphate precursor is obtained by dissolving iron source and phosphorus source in distilled water, obtaining 0.1-1 mol/L aqueous solution such that the molar ratio of iron with respect to phosphorus is 1:1-3, stirring the mixture at room temperature using DF-101S heated thermostatic magnetic stirrer, adjusting the pH to 1-7 using 1 mol/L ammonia, continuously stirring for 0.5-2 hours, transferring to polytetrafluoroethylene-lined reactor, processing in an oven at 80-200 degrees C for 6-20 hours, natural cooling to room temperature, filtering the solution, washing using deionized water and anhydrous ethanol, and placing washed pale yellow precipitate in an oven at 60-120 degrees C. Three-dimensional graphene gel is obtained by adding 1-100 mL 98 %mass concentrated sulfuric acid to 0-20 degrees C ice water bath, stirring, gradually adding 1-10 g graphite powder, 1-10 g sodium nitrate and 1-10 g potassium manganate, reacting for 1-3 hours, gradually adding 50-200 mL deionized water, reacting at 20-100 degrees C for 1-50 minutes, adding 1-100 mL 30 %mass hydrogen peroxide, obtaining bright yellow solution without bubbles, washing using hot water at the concentration of 1-10 mg/mL, washing using 7% dilute hydrochloric acid and deionized water, adding 0.01-0.1 g nickel chloride heaxahydrate, ultrasonically mixing at room temperature for 1-5 hours, naturally cooling to room temperature, and freeze-drying. Ferrous phosphate/three-dimensional graphene composite material is obtained by adding 10-100 mL 1-10 mg/ml Three-dimensional graphene gel solution to 0.1-10 g ferrous phosphate precursor, stirring at room temperature for 1-5 hours, adding 0.01-0.1 g nickel chloride hexahydrate, ultrasonically processing, cooling to room temperature, washing using deionized water for 12-96 hours, freeze-drying for 12-96 hours, placing dried sample in a tubular furnace under argon atmosphere, calcining at 300-800 degrees C for 1-20 hours at the heating rate of 2-10 degrees C/minute. 0.05-5 g Ferrous phosphate/three-dimensional graphene composite, 0.05-5 g lithium source and 0.05-5 g carbon source are placed in agate mortar, and 10-30 mL ethanol is added and ground. The mixture is placed in a tubular furnace under argon atmosphere at the heating rate of 2-10 degrees C, pre-heated at 300-800 degrees C for 1-20 hours, and calcined sample is removed. To the resultant material, 0.05-5 g carbon source is added, and ground under argon gas at the heating rate of 2-10 degrees C/minute at 300-800 degrees C for 1 to 20 hours, to obtain lithium iron phosphate/three-dimensional graphene/carbon composite material. The iron source is ferrous oxalate, ferric oxide, ferric nitrate and/or ferrous sulfate. The phosphorous source is phosphoric acid, ammonium phosphate, dihydrogen phosphate and/or ammonium dihydrogen phosphate. The lithium source is lithium acetate, lithium hydroxide and/or lithium carbonate. The carbon source is citric acid, glucose, acetylene black, sucrose and/or ascorbic acid.