CIESC Journal ›› 2018, Vol. 69 ›› Issue (7): 3263-3269.DOI: 10.11949/j.issn.0438-1157.20171582

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Hydrothermal synthesis of reduced graphene oxide with tunable conductivity

WENG Chengjie1, SHI Yexun1, HE Dafang1,2,3, SHEN Liming1, BAO Ningzhong1,2,3   

  1. 1 College of Chemical Engineering, State Key Laboratory of Material-Oriented Chemical Engineering, Nanjing Tech University, Nanjing 210009, Jiangsu, China;
    2 Jiangsu Industrial Technology Research Institute, Graphene Material Research Institute, Changzhou 213100, Jiangsu, China;
    3 Jiangnan Graphene Research Institute, Changzhou 213149, Jiangsu, China
  • Received:2017-11-30 Revised:2018-02-01 Online:2018-07-05 Published:2018-07-05
  • Supported by:

    supported by the National Natural Science Foundation of China (51425202, 51772150), the Natural Science Foundation of Jiangsu Province (BK20160093, BK20171012), the Industrial Support Program of Changzhou (CE20150054) and the Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions(PAPD).

水热法制备还原氧化石墨烯及其导电性调控

翁程杰1, 史叶勋1, 何大方1,2,3, 沈丽明1, 暴宁钟1,2,3   

  1. 1 南京工业大学化工学院, 材料化学工程国家重点实验室, 江苏 南京 210009;
    2 江苏省产业技术研究院石墨烯材料研究所, 江苏 常州 213100;
    3 江南石墨烯研究院, 江苏 常州 213149
  • 通讯作者: 沈丽明, 暴宁钟
  • 基金资助:

    国家自然科学基金项目(51425202,51772150);江苏省自然科学基金项目(BK20160093,BK20171012);常州市科技支撑计划项目(CE20150054);江苏高校优势学科建设工程资助项目。

Abstract:

Reduced graphene oxide (rGO) with tunable conductivity has great promise for potential applications in the fields of advanced structural-functional composites, new chemical materials and so on. In this research, environment-friendly hydrothermal method was applied to prepare rGO. The conductivity of the synthesized rGO can be controlled from 10-4 to 1 S·cm-1 by changing the hydrothermal reaction temperature and time. Various characterization techniques such as UV-vis, FT-IR, XPS, SEM, XRD, and Raman spectroscopy were used to analyze the composition and structure change of the rGO. The results showed that the oxygen contained functional groups on the rGO surface decomposed rapidly at ≥ 120℃, and the content of oxygen contained functional groups decreased drastically at ≥ 140℃. Meanwhile, the carbon sp2 region of the rGO was recovered gradually, which caused the conductivity increased to 1 S·cm-1 and the interlayer spacing decreased from 8.2 Å to 3.6 Å. Compared with thermal reduction method, hydrothermal method avoids the aggregation and stacking of the rGO, which has great significance in large-scale production of the rGO with tunable conductivity.

Key words: reduced graphene oxide, dispersion, preparation, nanomaterials, microstructure, conductivity

摘要:

导电性可调控的还原氧化石墨烯(rGO)在结构功能材料和化工新材料等领域具有重要的应用前景。本文利用水热还原法实现了rGO的绿色制备,并通过调控反应温度和时间,获得了电导率可控的rGO产品,其电导率范围为10-4~1 S·cm-1。采用UV-vis、FT-IR、XPS、SEM、XRD和Raman等表征方法系统研究了rGO还原过程中结构与组成的变化。发现GO还原过程中,其含氧官能团于120℃时开始明显分解,高于140℃后含量显著降低,GO片层sp2区域逐渐恢复,电导率逐渐增大到1 S·cm-1,同时层间距从8.2 Å减少到3.6 Å(1 Å=0.1 nm)。对比热还原法,水热法有效避免了rGO片层的堆叠,产物分散性较好,有望规模化制备导电性可控的rGO产品。本研究成果对rGO生产和应用具有重要意义。

关键词: 还原氧化石墨烯, 分散液, 制备, 纳米材料, 显微结构, 电导率

CLC Number: