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为了制备高质量、少层数的石墨烯薄膜,分别用25%HCl、2 mol/L FeCl_3腐蚀液及电化学抛光法处理铜箔,改善其表面平整度,然后利用化学气相沉积法在其表面生长石墨烯。通过调整2 mol/L Fe Cl3腐蚀铜箔的时间和电化学抛光铜箔的参数,根据SEM表征结果确定出腐蚀时间为30 s,抛光电压为10 V,抛光时间为60 s时,铜箔表面最为平整。这些方法处理铜箔后生长的石墨烯经拉曼光谱表征后得出,随着铜箔表面逐渐平整,铜箔表面更易生长出少层数,高质量的石墨烯薄膜。实验中还通过调整化学气相沉积(CVD)炉中通乙烯的时间来制备石墨烯。经SEM和拉曼光谱表征可知,延长生长时间,石墨烯薄膜的层数变厚,生长时间过短则石墨烯生长不连续。生长时间为30 s时,可生长出单层高质量的石墨烯薄膜,且石墨烯薄膜均匀致密;生长时间为60 s时,铜箔表面沉积一层石墨。所以生长单层石墨烯,控制生长时间是必要的。
In order to prepare high-quality, few-layer graphene thin films, the copper foil was treated with 25% HCl, 2 mol / L FeCl 3 etching solution and electrochemical polishing method respectively to improve the surface flatness. Then, chemical vapor deposition Graphene is grown. By adjusting the time of etching copper foil with 2 mol / L FeCl3 and the parameters of electrochemical copper foil, the surface of copper foil was determined according to the SEM characterization results when the etching time was 30 s, the polishing voltage was 10 V and the polishing time was 60 s The most smooth. The Raman spectra of the graphene grown after these treatments of copper foil show that as the surface of the copper foil is gradually flattened, a few layers of high quality graphene film are more easily grown on the copper foil surface. In the experiment, graphene was also prepared by adjusting the time of passing ethylene in a chemical vapor deposition (CVD) furnace. The results of SEM and Raman spectroscopy showed that when the growth time was prolonged, the number of graphene films became thicker and the growth time was too short, the growth of graphene was discontinuous. When the growth time is 30 s, a single layer of high quality graphene film can be grown, and the graphene film is uniform and compact. When the growth time is 60 s, a layer of graphite is deposited on the surface of the copper foil. Therefore, the growth of single-layer graphene, control of growth time is necessary.