▎ 摘 要
NOVELTY - Preparing large-area graphene on silicon substrate based on nickel film annealing comprises washing silicon substrate, carbonizing and growing a layer of carbon layer on the substrate, heating, introducing propane and silane, growing C3-silicon carbide heteroepitaxial film, placing in a graphene growth device, hydrogen etching and removing the compounds generated by hydrogen etching, reacting with carbon tetrachloride vapor to produce carbon film, depositing a layer of nickel film on the carbon film, introducing argon gas and annealing to obtain graphene film and removing nickel film. USE - The graphene is useful for manufacturing microelectronic devices, biological sensors and sealing gas and liquid. ADVANTAGE - The graphene: has area of 12 inches and low porosity; and is provided with continuous smooth surface. DETAILED DESCRIPTION - Preparing large-area graphene on silicon substrate based on nickel film annealing comprises (i) sequentially washing the 4-12 inches silicon substrate using mixed solution of aqueous ammonia and hydrogen peroxide, and mixed solution of hydrochloric acid and hydrogen peroxide; (ii) placing the cleaned silicon substrate in a chemical vapor deposition (CVD) reaction chamber and vacuumizing the reaction chamber until the vacuum level reaches 10-7 mbar; (iii) heating to the carbonization temperature of 1000-1200 degrees C under the protection of hydrogen, introducing propane at the flow rate of 30 ml/minute, carbonizing for 4-8 minutes and growing a layer of carbon layer on the substrate; (iv) heating to C3-silicon carbide growth temperature of 1200-1350 degrees C, introducing propane and silane, growing C3-silicon carbide heteroepitaxial film for 30-60 minutes, and cooling to room temperature under the protection of hydrogen to obtain C3-silicon carbide epitaxial thin film; (v) (va) placing the C3-silicon carbide film in a graphene growth device, opening the heating power supply, heating the reaction chamber to 1600 degrees C, and hydrogen etching to remove scratches on the C3-silicon carbide substrate, and (vb) removing the compounds generated by hydrogen etching; (vi) adjusting the heating power supply voltage, adjusting the temperature of the reaction chamber to 800-1000 degrees C, opening the vent valve, introducing argon gas and carbon tetrachloride gas into the mixing chamber, mixing completely, introducing the mixed gas into the quartz tube reaction chamber via a gas passage, and reacting carbon tetrachloride vapor and C3-silicon carbide substrate in the reaction chamber for 30-120 minutes to produce carbon film; (vii) placing the carbon film into an electron beam vapor deposition device, and depositing a layer of nickel film of 400-600 nm thickness on the carbon film; (viii) placing the resulting film in a graphene growth device, heating to 1000-1250 degrees C, introducing argon gas and annealing for 10-20 minutes to obtain nickel film covered carbon film reconstructed graphene i.e. graphene sample film; and (ix) placing the graphene sample film in hydrochloric acid and copper sulfate solution for removing nickel film.