采用N-甲基吡咯烷酮（NMP）与正丁醇（NBA）二元溶剂体系液相剥离法制备石墨烯，探究高浓度、高质量石墨烯的制备条件，通过比较不同体积比溶剂对石墨的剥离效果，得出最佳剥离体积比为V（NMP）∶V（NBA）=1.5∶1。通过正交试验得到初始石墨质量浓度对剥离后石墨烯的浓度影响最大，超声功率、时间、温度次之。结果表明，初始石墨质量浓度为10 mg/mL时，制备的石墨烯80%以上为少层石墨烯，结构完整，片层大小最大可达到3~4 μm，石墨烯溶液质量浓度最高达到7.2 mg/mL。该体系制备的石墨烯产率与片层大小比以往文献的报道均有大幅度提高。

Graphene is prepared through liquid phase exfoliation in a binary solvent system composing of N-methyl pyrrolidone (NMP) and n-butyl alcohol (NBA) to explore the conditions of preparing high quality and high concentration graphene.Through comparing the exfoliation effects of graphite within different volumetric ratio of solvents,the optimal ratio is confirmed as V(NMP):V(NBA)=1.5:1.It is found via orthogonal experiments that the initial mass concentration of graphite has the greatest influence on the concentration of graphene after exfoliation,followed by the ultrasonic power,time and temperature.The result shows that 80% of prepared graphene are of less layer,with structural integrity and 3-4 microns in lamella size,and the mass concentration of graphene solution can reach 7.2 mg·mL^-1 when the initial mass concentration of graphite is 10 mg·mL^-1.The yield and lamella size of graphene prepared in this system has a significant improvement than that reported in previous literatures.

赵木(1991-),女,硕士生,主要从事石墨烯制备工艺的研究,zhaomutd@tju.edu.cn