基于电极交换剥离技术制备少层石墨烯及其特性研究

Fabrication and Characterization of Graphene with Few Layers Based on Electrode Exchange Stripping Technology

摘要: 以石墨为原料电化学阳极剥离石墨烯引起了越来越多的关注，但在电化学剥离中离子嵌入非常快，石墨电极往往会瓦解，从而导致石墨烯产率较低且层数分布不均，电化学阴阳极交换剥离技术可有效改善石墨烯的质量。本实验以石墨箔作为对电极，基于电极交换剥离技术制备少层石墨烯。利用扫描电镜、透射电镜、原子力显微镜、拉曼光谱等表征，对比阴阳极交换前后两次剥离石墨烯的表面形貌、层数以及缺陷程度，并通过在DFM溶液中静置保存研究其稳定性。结果表明：相比于第一次剥离的石墨烯，第二次交换阴阳极后剥离得到的石墨烯边缘褶皱更明显，表现得更加透明，层数为单层或双层，且缺陷更小。通过在DMF溶液中静置保存，发现第一次剥离的石墨烯2 h就出现分层现象，而第二次阴阳极交换剥离的石墨烯保存220天不发生沉降，且随着交换次数的增加，石墨烯的稳定性越好。

Abstract: Electrochemical anodic exfoliated graphene from graphite as a raw has attracted more and more attention. However, in the process of electrochemical stripping, ion embedding is very fast, and the graphite electrode tends to collapse, resulting in low graphene yield and an uneven layer dis-tribution. Electrochemical cathode and anode exchange stripping technology can effectively im-prove the quality of graphene. In this work, graphite foil was used as the counter electrode, and few layers of graphene were prepared based on electrode exchange stripping technology. Scanning electron microscopy, transmission electron microscopy, atomic force microscopy and Raman spectroscopy were used to characterize the surface morphology, the number of layers and defect degree of graphene peeled before and after anode exchange. And the stability of graphene was studied by keeping in DFM solution. The results showed that compared with the graphene peeled for the first time, the graphene obtained after the second exchange of anode and cathode peeled off had more obvious edge folds, more transparent, fewer defects, and the number of layers was single or double. By keeping in DMF, it was found that the exfoliated graphene for the first time showed delamination in 2 h, while the exfoliated graphene by the second cathode and anode exchange was stored for 220 days without delamination, and the stability of the graphene became better with the increase of exchange times.