• 专利标题:   Preparing graphene/metal phosphide/C nano composites useful for lithium ion battery or a sodium ion battery cathode material, comprises preparing metal oxide nanosphere, preparing metal oxide C nano ball and metal phosphide/C nano ball.
  • 专利号:   CN107275622-A, CN107275622-B
  • 发明人:   WANG H, WANG X, LIU X, WANG G, BAI J
  • 专利权人:   UNIV NORTHWEST, UNIV NORTHWEST
  • 国际专利分类:   B82Y030/00, H01M004/36, H01M004/58, H01M004/583
  • 专利详细信息:   CN107275622-A 20 Oct 2017 H01M-004/36 201781 Pages: 15 Chinese
  • 申请详细信息:   CN107275622-A CN10564796 11 Jul 2017
  • 优先权号:   CN10564796

▎ 摘  要

NOVELTY - Preparing graphene/metal phosphide/C nano composites comprises (i) dissolving metal chloride salt and sodium acetate in ethylene glycol, and ultrasonically dispersing, cooling, washing (ii) dispersing metal oxide nano ball and glucose into distilled water, transferring, reacting, washing and drying (iii) placing metal oxide/C nanosphere and sodium hypophosphite into a quartz boat, heating, calcining, cooling and (iv) dispersing metal phosphide/C nano ball into de-ionized water, and ultrasonically dispersing freezing, drying and cooling. USE - The composites is useful for lithium ion battery or a sodium ion battery cathode material (claimed). DETAILED DESCRIPTION - Preparing graphene/metal phosphide/C nanocomposites comprises (i) dissolving the metal chloride salt and sodium acetate in ethylene glycol, and ultrasonically dispersing for 20-40 minutes to obtain the mixed solution, adding the mixed solution into a hydrothermal reaction kettle, reacting at the temperature 180-220 degrees C lower, for 6-10 hours, naturally cooling to the room temperature to obtain the reaction product I, washing the reaction product I with distilled water for 3-5 times, cleaning the reaction product I with absolute ethyl alcohol for 3-5 times and where the temperature is 60-80 degrees C lower, drying for 10-12 hours to obtain metal oxide nano ball, where the metal chloride is iron(III) chloride hexahydrate, cobalt(II) chloride hexahydrate, nickel chloride hexahydrate, tin(IV) chloride pentahydrate or molybdenum(II) chloride hexahydrat, the mass ratio of the mass of the metal chloride to ethylene glycol is (1-5g):100ml. The mass ratio of sodium acetate and ethylene glycol is (5-10g):100 ml, (ii) dispersing the metal oxide nano ball and glucose into distilled water, adding absolute ethyl alcohol, ultrasonic dispersing for 10-30 minutes under ultrasonic power of 20-40W to obtain a reaction liquid, transferring reaction liquid into the hydrothermal reaction kettle is 160-200 degrees C lower reacting for 1-3 hours, naturally cooling to the room temperature to obtain the reaction product II, washing reaction product II with distilled water for 3-5 times, cleaning the reaction product II with absolute ethyl alcohol for 3-5 times, drying at 60-80 degrees C lower, drying for 10-12 hours to obtain metal oxide C nano ball, where the volume weight ratio with distilled water and metal oxide nanometer ball is (0.5-21 g):3 5ml; the mass of glucose and distilled water volume ratio is (1-2g):35ml. The volume ratio of anhydrous ethanol to distilled water is (5-15):35, (iii) placing the metal oxide/C nanosphere and sodium hypophosphite obtained in step (ii) into a quartz boat, placing the quartz boat into tubular furnace, under a protective atmosphere of argon, where the tube furnace at a heating speed is 1-3 degrees C/minutes, heating to 300-400 degrees C and calcining at 300-400 degrees C 1-3 hours, naturally cooling to room temperature to obtain the metal phosphide/C nano ball, where the mass ratio of the metal oxide/C nanosphere to sodium hypophosphite is (1-2):( 10-20), (iv) dispersing the metal phosphide/C nano ball into de-ionized water, adding graphite oxide solution, and ultrasonically dispersing under the ultrasonic power is 20-40 W lower for 10-20 minutes, freezing and drying at -20 to -30 degrees C for 10-12 hours to obtain the mixture, placing the mixture into tubular furnace, under the protection of argon atmosphere, the tube furnace at a heating rate of 1-3 degrees C/minutes, raising the temperature to 550-650 degrees C, where the temperature is 550-650 degrees C lower carbonizing for 1-3 hours, naturally cooling to room temperature to obtain the graphene metal phosphide/nano composite material, where the mass ratio of metal phosphide/C nanospheres to deionized water is (80-100 mg):100ml, the volume ratio of the graphite oxide solution and the deionized water is (10-30):100 and the concentration of graphene oxide is 6 mg. mL -1-9 mg.mL-1.