• 专利标题:   Preparation of N-type single-layer sulfur-doped graphene film involves heat-treating copper foil, transferring graphene from copper foil to silicon substrate, cutting, fixing on polyethylene terephthalate, etching copper foil and washing.
  • 专利号:   CN112678810-A
  • 发明人:   ZHOU Y, CAO N, LI P
  • 专利权人:   UNIV CHINA ELECTRONIC SCI TECHNOLOGY
  • 国际专利分类:   C01B032/186, C01B032/194
  • 专利详细信息:   CN112678810-A 20 Apr 2021 C01B-032/186 202146 Pages: 9 Chinese
  • 申请详细信息:   CN112678810-A CN11461808 09 Dec 2020
  • 优先权号:   CN11461808

▎ 摘  要

NOVELTY - Preparation of N-type single-layer sulfur-doped graphene film involves placing dibenzyl disulfide and treated copper foil in temperature zone (A) and temperature zone (B) of tube furnace, heating in hydrogen/argon atmosphere to grow sulfur-doped graphene, cooling, transferring prepared graphene from copper foil to silicon dioxide/silicon substrate, cutting the copper foil, fixing on polyethylene terephthalate with tape edge, spin-coating foil with poly(methyl methacrylate) solution, homogenizing the glue, spinning, drying, then cut off the tape on the four sides of the copper foil, removing the polyethylene terephthalate at the bottom, placing in ferric chloride aqueous solution, washing the bottom with deionized water to remove the underlying graphene, placing in ferric chloride aqueous solution to etch the copper foil, placing film in deionized water for 10 minutes, and drying with hot plate, soaking in acetone, isopropanol and deionized water in order, and blow drying. USE - Preparation of N-type single-layer sulfur-doped graphene film. ADVANTAGE - The prepared single-layer sulfur-doped graphene film has high mobility and exhibit typical N-type transport characteristics in air. DETAILED DESCRIPTION - Preparation of N-type single-layer sulfur-doped graphene film involves soaking copper foil in 10 vol.% hydrochloric acid solution for 2 minutes, placing in deionized water for cleaning, replacing the deionized water several times to remove hydrochloric acid residue on the surface of the copper foil, placing in ethanol to remove the water on the surface of the copper foil, drying with dry nitrogen, placing dibenzyl disulfide and treated copper foil in temperature zone (A) and temperature zone (B) of tube furnace, respectively, evacuating vacuum to 7x 10-4 Pa to grow sulfur-doped graphene, raising the zone (B) temperature to 700, heat preserving in hydrogen/argon atmosphere for 20 minutes, further heating at zone temperature (A) of 150-300 degrees C for 30 minutes and zone temperature (B) of 900-1050 degrees C in hydrogen/argon atmosphere for 30 minutes to grow sulfur-doped graphene, naturally cooling to room temperature, transferring the prepared graphene from the copper foil to the silicon dioxide/silicon substrate through poly(methyl methacrylate) (PMMA) wet transfer process for the next step of structural and electrical characterization, cutting the copper foil with graphene into the required shape, fixing it on polyethylene terephthalate with tape edge, then spin-coating the front side of the graphene/copper foil with poly(methyl methacrylate) solution comprising 3 %mass poly(methyl methacrylate) powder and ethyl lactate, homogenizing the glue at 1000 rpm for 10 seconds, spinning it at 3000 rpm for 30 seconds, placing it on a hot plate at 120 degrees C for 10 minutes, then cut off the tape on the four sides of the copper foil and removing the polyethylene terephthalate at the bottom, placing it in 1 mol/L ferric chloride aqueous solution for 5 minutes, picking up the copper foil with tweezers, washing the bottom with deionized water to remove the underlying graphene, placing in ferric chloride aqueous solution to etch the copper foil for 15-6 hours, placing film in deionized water for 10 minutes, so that the film is washed with deionized water for 3 times, taking out the film with silicon substrate, and drying with hot plate at 50 degrees C for 15 minutes, 80 degrees C for 5 minutes and 100 degrees C for 5 minutes, changing the acetone twice to remove PMMA glue, soaking in acetone for 10 minutes, isopropanol for 10 minutes, and deionized water for 10 minutes in order, and blow drying with nitrogen gun.