物理化学学报 >> 2011, Vol. 27 >> Issue (03): 736-742.doi: 10.3866/PKU.WHXB20110320

材料物理化学 上一篇    下一篇

石墨烯薄膜的制备和结构表征

杨勇辉1, 孙红娟2, 彭同江2, 黄桥1   

  1. 1. 西南科技大学理学院, 四川 绵阳 621010;
    2. 西南科技大学矿物材料及应用研究所, 四川 绵阳 621010
  • 收稿日期:2010-09-30 修回日期:2010-12-26 发布日期:2011-03-03
  • 通讯作者: 孙红娟 E-mail:sunhongjuan@swust.edu.cn
  • 基金资助:

    西南科技大学研究生创新基金(10ycjj21)资助项目

Synthesis and Structural Characterization of Graphene-Based Membranes

YANG Yong-Hui1, SUN Hong-Juan2, PENG Tong-Jiang2, HUANG Qiao1   

  1. 1. College of Science, Southwest University of Science and Technology, Mianyang 621010, Sichuan Province, P. R. China;
    2. Institute of Mineral Materials & Application, Southwest University of Science and Technology, Mianyang 621010, Sichuan Province, P. R. China
  • Received:2010-09-30 Revised:2010-12-26 Published:2011-03-03
  • Contact: SUN Hong-Juan E-mail:sunhongjuan@swust.edu.cn
  • Supported by:

    The project was supported by the Postgraduate Innovation Fund of Southwest University of Science and Technology, China (10ycjj21).

摘要:

采用氧化还原法制备了石墨烯胶状悬浮液, 通过真空抽滤获得了石墨烯薄膜. 利用X射线衍射(XRD)、傅里叶变换红外(FTIR)光谱、拉曼(Raman)光谱、粒度分析和扫描探针显微镜(SPM)等研究了石墨烯薄膜制备过程中各阶段产物的晶体结构、粒度及分子光谱特征变化. FTIR分析结果表明, 石墨在氧化过程中结构层键合大量含氧官能团, 还原后结构层表面仍残存有部分稳定的含氧官能团. XRD结果表明, 石墨氧化后衍射峰向小角度偏移、宽化, 原有石墨峰消失. 在成膜过程中氧化石墨烯形成凝聚体,而石墨烯形成絮凝体. 粒度分析和SPM测试分析结果表明, 氧化石墨烯在水中粒径分布呈拖尾峰形, 分布范围较宽. 石墨烯在水中的粒径成单峰分布, 分布范围较窄、对称性较好且平均粒径较小. Raman测试结果表明, 石墨在氧化和还原过程中, D、G峰逐渐宽化, ID/IG逐渐增强, 样品无序度增加. 在以上分析的基础上对石墨烯制备过程的结构特征进行了归纳总结.

关键词: 石墨, 氧化石墨, 石墨烯, 氧化还原法, 晶体结构

Abstract:

A stable hydrosol of graphene was synthesized by oxidation reduction and then a flow assembly of this graphene was used to form a graphene-based membrane by vacuum extraction filtering method. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, particle size analysis, and scanning probe microscopy (SPM) were used to characterize the crystal structure, granularity, and characteristic change of the molecular spectrum of the samples in the reaction. FTIR tests show that the structural layer of graphite during the oxidation process bonds to a large number of functional groups and parts of these stable functional groups remain on the reduced structural layer of graphene. X-ray diffraction results show that the peaks of the graphite oxide shift to lower angles, become broader and the original graphite peak disappears. Suspensions of graphene oxide form condensed matter and graphene flocculating constituent during film deposition. Particle size analysis and SPM tests show that the particle sizes of the graphene oxide sheets that are dispersed in water show a tailing peak and a broad distribution while the graphene sheets show a singlet, narrower distribution, and smaller dimensions. Raman results show that during oxidation and reduction, the D peak and G peak of the samples gradually extend, ID/IG increases gradually and the degree of sample disorder increases. On the basis of the above analyses, the structural characteristics of the samples in the reaction are summarized.

Key words: Graphite, Graphite oxide, Graphene, Oxidation reduction, Crystal structure

MSC2000: 

  • O641