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以超临界乙醇为介质剥离石墨制备了石墨烯,考察了实验条件对石墨烯收率的影响.当石墨/乙醇质量浓度为0.32mg/mL,温度为250℃,压力为26 MPa,反应时间为0.5h时,石墨烯的收率为12.49％.在该实验条件下,经过6次反复冷热循环过程后,石墨烯的收率达到最大为21.32％.采用透射电子显微镜(TEM)、X射线衍射仪(XRD)及拉曼光谱(Raman)等技术对石墨烯样品进行表征,TEM分析结果表明,超临界法可剥离得到薄层石墨烯;XRD和拉曼分析结果表明,由该方法可以得到结构缺陷较少的优质石墨烯.,Supercritical ethanol is employed as medium to make graphene by exfoliation of graphite.The influences of experimental parameters on graphene yield are systematically investigated and discussed.The graphene yield reaches 12.49％ when the initial graphite concentration in ethanol is 0.32 mg·mL-1,temperature is at 250℃,pressure is 26 MPa and reaction time is 0.5 hour.The maximum yield 21.32％ is reached after six times’ repeated exfoliation under those optimum conditions.The graphene samples are characterized by Transmission Electron Microscopy (TEM),X-ray diffraction (XRD) and Raman Spectroscopy.TEM results suggest that the thin layer graphene is prepared by supercritical method.The results from XRD and Raman show that the prepared graphene exhibits high quality and intact lattice structure.