▎ 摘　　要

Scalable production of large size and high quality graphene is an important prerequisite to fully realize its commercial applications. Herein, we propose a high-efficient route for preparing few-layer graphene. The secondary exfoliation of unexfoliated graphite flakes from electrochemical exfoliation was achieved by using ultrasonication assisted microwave exfoliation technique. The results show that the as-prepared sample has a C/O of 15.2, a thickness of about 1 nm and a transverse dimension of over 100 nm, and the Raman spectrogram shows low defects upon reduction of the sample. These results suggest that electrolytic graphene can be exfoliated to form graphene nanosheets under ultrasonic-assisted microwave technology, thus indicating that the current method has great potential for synthesizing high-quality graphene at an industrial-scale.