改进型Hummers法制备石墨烯及其表征

改进型Hummer s法制备石墨烯及其表征

龙吟1，陶呈安1，夏林1，朱慧1，王建方1,*

1国防科技大学理学院化学与生物学系，湖南长沙，410073

* E-mail: wangjianfang@

自2004年由Geim等人采用胶带剥离高定向石墨制得石墨烯[1]后，石墨烯的研究步入了一个快速发展的阶段，石墨烯的制备方法也层出不穷。目前制备石墨烯的方法主要有微机械剥离法、液相或气相直接剥离法、化学气相沉积法、氧化还原法等，其中氧化还原法因其操作简单、原料易得、成本低廉等优点，是实现石墨烯规模化制备的不二选择。本文采用改进型Hummers法[2]对天然鳞片石墨进行氧化处理得到氧化石墨，超声处理后利用水合肼进行还原得到稳定性较高的石墨烯溶液，纯化干燥后得到石墨烯粉末。利用红外光谱、拉曼光谱、X射线衍射分析、扫描电子显微镜（SEM）以及透射电子显微镜（TEM）进行结构、谱学及形貌分析。结果表明，氧化石墨表面形成以C=O、C-OH、-COOH 和C-O-C 等官能团形式的共价键型石墨层间化合物；水合肼还原氧化石墨比较完全，但仍有部分含氧基团残留；还原后的石墨烯呈半透明片状，边缘有自发形成的卷曲。

Fig. 1 TEM image of graphene Fig. 2 SEM image of graphene

关键词：石墨烯；氧化石墨烯；改进型Hummers法；

参考文献

[1] Novoselov K S, Geim A K, Morozov S V, et al.Electric field effect in atomically thin carbon films [J].

Science,2004, 306: 666-669.

[2] Hummers W, Offeman R. Preparation of graphitic oxide [J]. J. Am. Chem. Soc., 1958, 80(6): 1339.

Synthesis and characterization of graphene

by the modified Hummers method

Long Yin1, Tao Cheng’an 1, Xia Lin1, Zhu Hui1, Wang Jianfang 1,*

1Department of Chemistry and Biology, College of Science, National University of Defense

Technology, 410073, Changsha

The graphite oxide (GO) was prepared from purified natural flake graphite by the modified Hummers method. The colloidal form of graphene was subsequently prepared by ultrasonicating GO in the presence of hydrazine hydrate. The samples were characterized by FTIR, Raman, Scanning electron microscope (SEM) and Transmission electron microscope (TEM). The results suggest that the graphite is oxidized to covalent bond-type graphite intercalation compounds with various oxygen bearing functional groups (C=O, C-OH, -COOH and C-O-C). FTIR spectra show that the functional groups on graphite oxide (GO) surface are mostly removed by hydrazine hydrate. SEM image shows graphene presents translucent slide with curly edge.