后浩,代文,孙红岩,赵文杰,林正得,周红洋.快速电化学剥离天然脉石墨制备石墨烯用于透明导电薄膜的研究[J].表面技术,2018,47(9):49-56.
HOU Hao,DAI Wen,SUN Hong-yan,ZHAO Wen-jie,LIN Zheng-de,ZHOU Hong-yang.Transparent Conductive Film Fabricated with Graphene from Fast Electrochemical Exfoliation of Natural Vein Graphite[J].Surface Technology,2018,47(9):49-56
快速电化学剥离天然脉石墨制备石墨烯用于透明导电薄膜的研究
Transparent Conductive Film Fabricated with Graphene from Fast Electrochemical Exfoliation of Natural Vein Graphite
投稿时间:2018-03-15  修订日期:2018-09-20
DOI:10.16490/j.cnki.issn.1001-3660.2018.09.007
中文关键词:  电化学剥离  天然脉石墨  石墨烯  自组装  透明导电薄膜  方阻
英文关键词:electrochemical exfoliation  natural vein graphite  graphene  self-assembly  transparent conductive film  sheet resistance
基金项目:浙江省重点研发计划(2015C0101006);中国科学院战略性先导科技专项(XDA13040601);宁波市自然科学基金(2017A610049)
作者单位
后浩 1.合肥工业大学宣城校区 化工与食品加工系,安徽 宣城 242000;2.中国科学院宁波材料技术与工程研究所 a.中国科学院海洋新材料与应用技术重点实验室,b.浙江省海洋与防护重点实验室,浙江 宁波 315201 
代文 2.中国科学院宁波材料技术与工程研究所 a.中国科学院海洋新材料与应用技术重点实验室,b.浙江省海洋与防护重点实验室,浙江 宁波 315201 
孙红岩 2.中国科学院宁波材料技术与工程研究所 a.中国科学院海洋新材料与应用技术重点实验室,b.浙江省海洋与防护重点实验室,浙江 宁波 315201 
赵文杰 2.中国科学院宁波材料技术与工程研究所 a.中国科学院海洋新材料与应用技术重点实验室,b.浙江省海洋与防护重点实验室,浙江 宁波 315201 
林正得 2.中国科学院宁波材料技术与工程研究所 a.中国科学院海洋新材料与应用技术重点实验室,b.浙江省海洋与防护重点实验室,浙江 宁波 315201 
周红洋 1.合肥工业大学宣城校区 化工与食品加工系,安徽 宣城 242000 
AuthorInstitution
HOU Hao 1.Department of Chemical Engineering and Food Processing, Hefei University of Technology, Xuancheng Campus,Xuancheng 242000, China;2. a. Key Laboratory of New Marine Materials and Application Technologies,b.Key Laboratory of Marine and Protection of Zhejiang, Ningbo Institute of Materials Technology and Engineering (NIMTE), Chinese Academy of Sciences, Ningbo 315201, China 
DAI Wen 2. a. Key Laboratory of New Marine Materials and Application Technologies,b.Key Laboratory of Marine and Protection of Zhejiang, Ningbo Institute of Materials Technology and Engineering (NIMTE), Chinese Academy of Sciences, Ningbo 315201, China 
SUN Hong-yan 2. a. Key Laboratory of New Marine Materials and Application Technologies,b.Key Laboratory of Marine and Protection of Zhejiang, Ningbo Institute of Materials Technology and Engineering (NIMTE), Chinese Academy of Sciences, Ningbo 315201, China 
ZHAO Wen-jie 2. a. Key Laboratory of New Marine Materials and Application Technologies,b.Key Laboratory of Marine and Protection of Zhejiang, Ningbo Institute of Materials Technology and Engineering (NIMTE), Chinese Academy of Sciences, Ningbo 315201, China 
LIN Zheng-de 2. a. Key Laboratory of New Marine Materials and Application Technologies,b.Key Laboratory of Marine and Protection of Zhejiang, Ningbo Institute of Materials Technology and Engineering (NIMTE), Chinese Academy of Sciences, Ningbo 315201, China 
ZHOU Hong-yang 1.Department of Chemical Engineering and Food Processing, Hefei University of Technology, Xuancheng Campus,Xuancheng 242000, China 
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中文摘要:
      目的 开发一种基于电化学剥离天然脉石墨的石墨烯量产制备工艺,并研究其剥离石墨烯的品质,最后验证以该量产石墨烯作为原料制备透明导电薄膜的可行性。方法 以相同的电化学工艺剥离天然脉石墨、高定向热解石墨以及人工石墨制备石墨烯,然后用共聚焦光学显微镜(OM)、扫描探针显微镜(AFM)、拉曼光谱仪(Raman)和X-射线光电子能谱仪(XPS)考察天然脉石墨剥离的石墨烯尺寸和品质,并将其与另外两种石墨烯及基于文献报道的热/化学还原氧化石墨烯进行对比,最后以天然脉石墨剥离的石墨烯制备成透明导电膜并测量其电导率和透光率。结果 以天然脉石墨通过电化学剥离得到的石墨烯主要以1—3层石墨烯为主,平均横向尺寸和厚度分别为5.9 μm和2.4 nm。Raman及XPS分析表明,该石墨烯的品质可与电化学剥离高定向热解石墨得到的石墨烯相媲美,并且优于人工石墨烯和基于热/化学还原的氧化石墨烯的品质。最后以天然脉石墨烯为原料,通过界面自组装及后续的转移工艺于石英基板上制备了透明的石墨烯导电薄膜,在83.1%的透光率下,该薄膜的方阻低至13 kΩ/□,相对于以人工石墨经电化学剥离得到的石墨烯为原料所制备的导电薄膜有较大的提升。结论 以天然脉石墨作为原料并通过电化学剥离得到的石墨烯的尺寸较大、缺陷少、官能化程度低,可应用于透明导电膜的制备,这主要归因于天然脉石墨的致密结晶性及高含碳量。
英文摘要:
      Graphene has been considered as a promising candidate to replace the traditional metallic oxide to prepare transparent conductive film based on its superior electrical conductivity and high visible light transmittance. However, so far no appropriate method is found to prepare high-quality and low-cost graphene in a large quantity. Therefore, the work aims to develop a technology to prepare the graphene based on fast electrochemical exfoliation of natural vein graphite and study the performance to exfoliate natural vein graphite and finally verify the feasibility to prepare the transparent conductive film by the graphene in volume production. The same electrochemical technology was used to exfoliate natural vein graphite and highly oriented pyrolytic graphiteand artificial graphite was used to prepare the graphene. The size and quality of the graphene exfoliated from natural vein graphite were investigated by OM, AFM, Raman and XPS. Then, the graphene exfoliated from natural vein graphite was compared with other two kinds of graphene and the graphene based on thermal/chemical reduction-oxidation reported in the literature. The transparent conductive film was prepared by the graphene exfoliated from natural vein graphite and its conductivity and light transmittance were measured. The graphene based on fast electrochemical exfoliation of natural vein graphite was mainly composed of 1—3 layers and the average horizontal size and thickness were respectively 5.9 μm and 2.4 nm. Through Raman and XPS analysis, the quality of such graphene could be compared favourably with that from highly oriented pyrolytic graphite by electrochemical exfoliation and better than that of artificial graphite and graphene based on thermal/chemical reduction-oxidation. Such graphene was used as raw materials to prepare the transparent graphene conductive film on the quartz by the interface self-assembly andthe subsequent transferring. At the light transmittance of 83.1%, the sheet resistance of the film decreased to 13kΩ/□, but improved greatly when compared with that of conductive film prepared by the graphene based on electrochemical exfoliation. The graphene prepared by electrochemical exfoliation with natural vein graphite as raw materials has large size, few defects and low degree of functionalization and can be used to prepare the transparent conductive film due to dense crystallization and high carbon contents of natural vein graphite.
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