An easy approach for preparation of graphitic carbon nitride nanosheet (CNNS) from stripping graphitic carbon nitride by strong acid and ultrasonic technology was demonstrated in this study. Transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Uv-vis absorption spectroscopy and fluorescent spectrometry were employed to characterize the CNNS. The Results showed that the CNNS had been prepared successfully. The as-synthesized CNNS exhibited excellent emission property as well as excitation-independent emission behavior, and fluorescence quantum yields can reach approximately 19.3%. At the same time, the CNNS was characterized by cyclic voltammetry, which showed that the CNNS had excellent electrochemical performance.%通过混酸剥离法制备石墨相氮化碳纳米片（CNNS），该方法制备过程简单.透射电子显微镜、X射线衍射光谱、X射线光电子能谱、傅里叶变换红外光谱、紫外可见吸收光谱与荧光光谱对CNNS的形貌等进行表征，结果显示，混酸剥离法可以成功实现CNNS的制备，研究结果同时显示所制备的CNNS的荧光量子产率达到19.3%，且其荧光激发不依赖于发射，同时，通过电化学循环伏安法测试其性能，发现其导电性能优异.
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