• 专利标题:   Preparing graphene-loaded copper-reinforced copper-based composite material used in e.g. electronic device, by ultrasonically vibrating hydroxylated copper flakes and dispersed graphene to obtain mixed layered material, drying, adding to graphite mold, pressurizing, sintering, cooling and demolding.
  • 专利号:   CN113604697-A, CN113604697-B
  • 发明人:   JU B, CHEN G, LIU M, YANG W, WU G, XIU Z
  • 专利权人:   HARBIN INST TECHNOLOGY
  • 国际专利分类:   B22F001/00, B22F001/02, B22F003/105, B22F009/04, C22C001/05, C22C009/00, C23C014/18, B22F001/068, B22F001/18, C22C001/059
  • 专利详细信息:   CN113604697-A 05 Nov 2021 C22C-001/05 202219 Chinese
  • 申请详细信息:   CN113604697-A CN10929317 13 Aug 2021
  • 优先权号:   CN10929317

▎ 摘  要

NOVELTY - Preparing graphene-loaded copper-reinforced copper-based high thermal conductivity composite material involves: (1) weighing multilayer graphene nanosheets and copper metal powder; (2) ball milling copper metal powder and grinding aid to obtain a sheet-shaped copper metal powder; (3) depositing copper atoms on a surface of multilayer graphene nanosheets to obtain copper-loaded graphene; (4) preparing polyvinyl alcohol aqueous solution, adding the sheet-shaped copper metal powder, stirring, heat-preserving to obtain hydroxylated copper flakes, and preparing dispersed graphene by using copper-loaded graphene; (5) adding hydroxylated copper flakes and dispersed graphene to containers, and ultrasonically vibrating to obtain a mixed layered material; (6) drying the obtained mixed layered material; and (7) adding the obtained graphene-copper mixed powder to a graphite mold, pressurizing, sintering, cooling, and then demolding. USE - The method is useful for preparing graphene-loaded copper-reinforced copper-based high thermal conductivity composite material used in aerospace, aviation, and electronic device. ADVANTAGE - The method provides graphene-loaded copper-reinforced copper-based high thermal conductivity composite material, which has excellent mechanical property and performs self-assembly and adsorption under ultrasonic vibration, and solves the problem of uneven graphene dispersion in the current graphene-reinforced copper-based composite material. DETAILED DESCRIPTION - Preparing graphene-loaded copper-reinforced copper-based high thermal conductivity composite material involves: (1) weighing 0.3-5 %mass multilayer graphene nanosheets and 95-99.7 %mass copper metal powder with a particle size of 1-15 microm; (2) adding the copper metal powder and a grinding aid to a ball mill tank according to the ball-to-material ratio of (2-20):1, and ball milling at 100-400 rpm for 2-15 hours to obtain a sheet-shaped copper metal powder with a planar size of 30-70 microm and a thickness of 100-300 nm; (3) depositing copper atoms on the surface of multilayer graphene nanosheets by plasma physical vapor deposition while stirring to obtain copper-loaded graphene whose copper loading amount of is 3-6%; (4) dissolving polyvinyl alcohol in water at 50-90degrees Celsius to a polyvinyl alcohol aqueous solution, adding the sheet-shaped copper metal powder, evenly stirring, heat-preserving in a water bath at 80degrees Celsius for 1-15 hours to obtain hydroxylated copper flakes, adding the copper-loaded graphene to 3-5% stannous chloride solution, ultrasonically processing for 10-100 minutes, then transferring to 3-5% palladium(II) chloride solution, ultrasonically processing for 10-100 minutes, rinsing with deionized water, and ultrasonically dispersing in absolute ethanol to obtain processed graphene nanosheets, adding to deionized water with 5 %mass sodium edetate, and ultrasonically dispersing to obtain dispersed graphene; (5) adding the hydroxylated copper flakes and the dispersed graphene to two containers respectively, ultrasonically vibrating, setting a switch at the opening of the container to control the switch to be turned on every 5-30 seconds, so that the dispersed graphene pass through a pipeline, then depositing and precipitating autonomously under the action of gravity in other container, leaving still for 4-8 hours to form a layered structure of graphene copper to obtain a mixed layered material; (6) drying the obtained mixed layered material in a drying oven at 60-90degrees Celsius to obtain graphene-copper mixed powder; and (7) adding the graphene-copper mixed powder to a graphite mold, placing on a press table together with the mold, pressurizing the mixed powder at 2-10 MPa and a pressure speed of 0.1-30 mm/minute and maintaining the pressure for 3-20 minutes, transferring the pre-pressed mixture together with the mold to a plasma sintering furnace, heating the furnace from room temperature to 800-1070degrees Celsius within 10-60 minutes under a protective atmosphere, sintering at 800-1070degrees Celsius for 2-30 minutes, cooling along with the furnace, and then demolding.