石墨烯薄膜的制备和结构表征

引用本文: 杨勇辉, 孙红娟, 彭同江, 黄桥. 石墨烯薄膜的制备和结构表征[J]. 物理化学学报, 2011, 27(03): 736-742. doi: 10.3866/PKU.WHXB20110320 shu

Citation: YANG Yong-Hui, SUN Hong-Juan, PENG Tong-Jiang, HUANG Qiao. Synthesis and Structural Characterization of Graphene-Based Membranes[J]. Acta Physico-Chimica Sinica, 2011, 27(03): 736-742. doi: 10.3866/PKU.WHXB20110320 shu

石墨烯薄膜的制备和结构表征

基金项目:
西南科技大学研究生创新基金(10ycjj21)资助项目 (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, I_D/I_G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:

English

Synthesis and Structural Characterization of Graphene-Based Membranes

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 Date: 30 September 2010
Available Online: 03 March 2011
Fund Project:
西南科技大学研究生创新基金(10ycjj21)资助项目

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, I_D/I_G 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:

1. [1]
  
  (1) Novoselov, K. S.; Geim, A. K.; Morozov, S. V.; Jiang, D.; Zhang, Y.; Dubonos, S. V.; Gri rieva, I. V.; Firsov, A. A. Science 2004, 306, 666.
  (1) Novoselov, K. S.; Geim, A. K.; Morozov, S. V.; Jiang, D.; Zhang, Y.; Dubonos, S. V.; Gri rieva, I. V.; Firsov, A. A. Science 2004, 306, 666.
2. [2]
  (2) Yang, Q. H.; Lü, W.; Yang, Y. G.; Wang, M. Z. New Carbon Materials 2008, 23, 97.(2) Yang, Q. H.; Lü, W.; Yang, Y. G.; Wang, M. Z. New Carbon Materials 2008, 23, 97.
3. [3]
  [杨全红, 吕伟, 杨永岗, 王茂章. 新型炭材料, 2008, 23, 97.][杨全红, 吕伟, 杨永岗, 王茂章. 新型炭材料, 2008, 23, 97.]
4. [4]
  (3) Gu, Z. B.; Ji, G. H.; Lu, M. H. Journal of Nanjing University of Technology (Natural Science) 2010, 32, 105.(3) Gu, Z. B.; Ji, G. H.; Lu, M. H. Journal of Nanjing University of Technology (Natural Science) 2010, 32, 105.
5. [5]
  [顾正彬, 季根华, 卢明辉. 南京工业大学学报: 自然科学版, 2010, 32, 105.][顾正彬, 季根华, 卢明辉. 南京工业大学学报: 自然科学版, 2010, 32, 105.]
6. [6]
  (4) Zhang, W. N.; He, W.; Zhang, X. L. New Chemical Materials 2010, 38, 15.(4) Zhang, W. N.; He, W.; Zhang, X. L. New Chemical Materials 2010, 38, 15.
7. [7]
  [张伟娜, 何伟, 张新荔. 化工新型材料, 2010, 38, 15.][张伟娜, 何伟, 张新荔. 化工新型材料, 2010, 38, 15.]
8. [8]
  (5) Meyer, J. C.; Geim, A. K.; Katsnelson, M. I.; Novoselov, K. S.; Booth, T. J.; Roth, S. Nature 2007, 446, 60.(5) Meyer, J. C.; Geim, A. K.; Katsnelson, M. I.; Novoselov, K. S.; Booth, T. J.; Roth, S. Nature 2007, 446, 60.
9. [9]
  (6) Geim, A. K.; Novoselov, K. S. Nature Mater. 2007, 6, 183.(6) Geim, A. K.; Novoselov, K. S. Nature Mater. 2007, 6, 183.
10. [10]
  (7) Kim, S. K.; Zhao, Y.; Jang, H.; Lee, Y. S.; Kim, M. J.; Ahn, H. J.; Kim, P.; Choi, Y. J.; Hong, H. B. Nature, 2009, 457, 706.(7) Kim, S. K.; Zhao, Y.; Jang, H.; Lee, Y. S.; Kim, M. J.; Ahn, H. J.; Kim, P.; Choi, Y. J.; Hong, H. B. Nature, 2009, 457, 706.
11. [11]
  (8) Obraztsov, N. A. Nat. Nanotech. 2009, 4, 212.(8) Obraztsov, N. A. Nat. Nanotech. 2009, 4, 212.
12. [12]
  (9) Tung, C. V.; Allen, J. M.; Yang, Y.; Kaner, B. R. Nat. Nanotech. 2009, 4, 25.(9) Tung, C. V.; Allen, J. M.; Yang, Y.; Kaner, B. R. Nat. Nanotech. 2009, 4, 25.
13. [13]
  (10) Li, D.; Muller, M. B.; Gilje, S.; Kaner, B. R.; Wallace, G. G. Nat. Nanotech. 2008, 3, 101.(10) Li, D.; Muller, M. B.; Gilje, S.; Kaner, B. R.; Wallace, G. G. Nat. Nanotech. 2008, 3, 101.
14. [14]
  (11) Hernandez, Y.; Nicolosi, V.; Lotya, M.; Blighe, F.; Sun, Z.; De, S.; Mc vern, I. T.; Holland, B.; Byrne, M.; Gunko, Y.; Boland, J.; Niraj, P.; Duesberg, G.; Krishnamurti, S.; odhue, R.; Hutchison, J.; Scardaci, V.; Ferrari, A. C.; Coleman, J. N. Nat. Nanotech. 2008, 3, 563.(11) Hernandez, Y.; Nicolosi, V.; Lotya, M.; Blighe, F.; Sun, Z.; De, S.; Mc vern, I. T.; Holland, B.; Byrne, M.; Gunko, Y.; Boland, J.; Niraj, P.; Duesberg, G.; Krishnamurti, S.; odhue, R.; Hutchison, J.; Scardaci, V.; Ferrari, A. C.; Coleman, J. N. Nat. Nanotech. 2008, 3, 563.
15. [15]
  (12) Hamilton, C. E.; Lomeda; J. R.; Sun, Z. Z.; Tour, M. J.; Barron, R. D. Nano Lett. 2009, 9, 3460.(12) Hamilton, C. E.; Lomeda; J. R.; Sun, Z. Z.; Tour, M. J.; Barron, R. D. Nano Lett. 2009, 9, 3460.
16. [16]
  (13) Choucair, M.; Thordarson, P.; Stride, J. A. Nat. Nanotech. 2009, 4, 30.(13) Choucair, M.; Thordarson, P.; Stride, J. A. Nat. Nanotech. 2009, 4, 30.
17. [17]
  (14) Wang, H. L.; Robinson, J. T.; Li, X. L.; Dai, H. J. J. Am. Chem. Soc. 2009, 131, 9910.(14) Wang, H. L.; Robinson, J. T.; Li, X. L.; Dai, H. J. J. Am. Chem. Soc. 2009, 131, 9910.
18. [18]
  (15) Ramesh, P.; Bhagyalakshmi, S.; Sampath, S. J. Colloid Interface Sci. 2004, 274, 95.(15) Ramesh, P.; Bhagyalakshmi, S.; Sampath, S. J. Colloid Interface Sci. 2004, 274, 95.
19. [19]
  (16) Stankovich, S.; Dikin, A. D.; Piner, D. R.; Kohlhaas, A. K.; Kleinhammes, A.; Jia, Y. Y.; Wu, Y.; Nguyen, T. S.; Ruoff, S. R. Carbon 2007, 45, 1558.(16) Stankovich, S.; Dikin, A. D.; Piner, D. R.; Kohlhaas, A. K.; Kleinhammes, A.; Jia, Y. Y.; Wu, Y.; Nguyen, T. S.; Ruoff, S. R. Carbon 2007, 45, 1558.
20. [20]
  (17) Yang, Y. H.; Sun, H. J.; Peng, T. J. Chin. J. Inorg. Chem. 2010, 26, 2083.(17) Yang, Y. H.; Sun, H. J.; Peng, T. J. Chin. J. Inorg. Chem. 2010, 26, 2083.
21. [21]
  [杨勇辉, 孙红娟, 彭同江. 无机化学学报, 2010, 26, 2083.][杨勇辉, 孙红娟, 彭同江. 无机化学学报, 2010, 26, 2083.]
22. [22]
  (18) Stankovich, S.; Piner, D. R.; Chen, X. Q.; Wu, N. Q.; Nguyen, T. S.; Ruoff, S. R. J. Mater. Chem. 2006, 16, 155.(18) Stankovich, S.; Piner, D. R.; Chen, X. Q.; Wu, N. Q.; Nguyen, T. S.; Ruoff, S. R. J. Mater. Chem. 2006, 16, 155.
23. [23]
  (19) Yang, D. X.; Velamakanni, A.; Bozoklu, G.; Park, S.; Stoller, M.; Piner, D. R.; Stankovich, S.; Jung, I.; Field, A. D.; Ventrice, A. C.; Ruoff, S. R. Carbon 2009, 47, 145.(19) Yang, D. X.; Velamakanni, A.; Bozoklu, G.; Park, S.; Stoller, M.; Piner, D. R.; Stankovich, S.; Jung, I.; Field, A. D.; Ventrice, A. C.; Ruoff, S. R. Carbon 2009, 47, 145.
24. [24]
  (20) Hu, W. B.; Peng, C.; Luo, W. J.; Lv, M.; Li, X. M.; Li, D.; Huang, Q.; Fan, C. H. ACS Nano 2010, 4, 4317.(20) Hu, W. B.; Peng, C.; Luo, W. J.; Lv, M.; Li, X. M.; Li, D.; Huang, Q.; Fan, C. H. ACS Nano 2010, 4, 4317.
25. [25]
  (21) Dikin, D. A.; Stankovich, S.; Zimney, E. J.; Piner, D. R.; Dommett, H. B.; Guennadi, E.; Nguyen, T. S.; Ruoff, S. R. Nature 2007, 448, 457.(21) Dikin, D. A.; Stankovich, S.; Zimney, E. J.; Piner, D. R.; Dommett, H. B.; Guennadi, E.; Nguyen, T. S.; Ruoff, S. R. Nature 2007, 448, 457.
26. [26]
  (22) Chen, C. M.; Yang, Y. G.; Wen, Y. F.; Yang, Q. H.; Wang, M. Z. New Carbon Materials 2008, 24, 345.(22) Chen, C. M.; Yang, Y. G.; Wen, Y. F.; Yang, Q. H.; Wang, M. Z. New Carbon Materials 2008, 24, 345.
27. [27]
  [陈成猛, 杨永岗, 温月芳, 杨金红, 王茂章. 新型炭材料, 2008, 24, 345.][陈成猛, 杨永岗, 温月芳, 杨金红, 王茂章. 新型炭材料, 2008, 24, 345.]
28. [28]
  (23) Hummers, W. S.; Offeman, R. E. J. Am. Chem. Soc. 1958, 80, 1339.(23) Hummers, W. S.; Offeman, R. E. J. Am. Chem. Soc. 1958, 80, 1339.
29. [29]
  (24) He, H. Y.; Klinowski, J.; Forster, M.; Lerf, A. Chem. Phys. Lett. 1998, 287, 53.(24) He, H. Y.; Klinowski, J.; Forster, M.; Lerf, A. Chem. Phys. Lett. 1998, 287, 53.
30. [30]
  (25) Pan, Z. L.; Wan, P. Application Mineralogy; Wuhan University of Technology Press: Wuhan, 1993; pp 209-211.(25) Pan, Z. L.; Wan, P. Application Mineralogy; Wuhan University of Technology Press: Wuhan, 1993; pp 209-211.
31. [31]
  [潘兆橹, 万朴. 应用矿物学. 武汉: 武汉工业大学出版社, 1993: 209-211.][潘兆橹, 万朴. 应用矿物学. 武汉: 武汉工业大学出版社, 1993: 209-211.]
32. [32]
  (26) Titelman, G. I.; Gelman, V.; Bron, S.; Khalfin, R. L.; Cohen, Y.; Bianco-Peled, H. Carbon 2005, 43, 641.(26) Titelman, G. I.; Gelman, V.; Bron, S.; Khalfin, R. L.; Cohen, Y.; Bianco-Peled, H. Carbon 2005, 43, 641.
33. [33]
  (27) Mermoux, M.; Chabre, Y.; Rousseau, A. Carbon 1991, 29, 469.(27) Mermoux, M.; Chabre, Y.; Rousseau, A. Carbon 1991, 29, 469.
34. [34]
  (28) Singh, V. K.; Patra,M. K.; Manoth, M.; wd, G. S.; Vadera, S. R.; Kumar, N. New Carbon Materials 2009, 24, 147.(28) Singh, V. K.; Patra,M. K.; Manoth, M.; wd, G. S.; Vadera, S. R.; Kumar, N. New Carbon Materials 2009, 24, 147.
35. [35]
  (29) Ferrari, C. A.; Robertson, J. Raman Spectroscopy in Carbons: from Nanotubes to Diamond; Chemical Industry Press: Beijing, 2007; pp 193-204; translated by Tan, P. H., Li, F., Cheng, H. M.(29) Ferrari, C. A.; Robertson, J. Raman Spectroscopy in Carbons: from Nanotubes to Diamond; Chemical Industry Press: Beijing, 2007; pp 193-204; translated by Tan, P. H., Li, F., Cheng, H. M.
36. [36]
  [Ferrari, C. A.; Robertson, J. 碳材料的拉曼光谱—从纳米管到金刚石. 谭平恒, 李峰, 成会明, 译. 北京: 化学工业出版社, 2007: 193-204.][Ferrari, C. A.; Robertson, J. 碳材料的拉曼光谱—从纳米管到金刚石. 谭平恒, 李峰, 成会明, 译. 北京: 化学工业出版社, 2007: 193-204.]
37. [37]
  (30) Ferrari, A. C.; Robertson, J. Phys. Rev. B 2000, 61, 14095.(30) Ferrari, A. C.; Robertson, J. Phys. Rev. B 2000, 61, 14095.
38. [38]
  (31) Yang, X. G.; Wu, Q. L. Raman Spectroscopy Analysis and Application; National Defense Industry Press: Beijing, 2008; pp 210-220.(31) Yang, X. G.; Wu, Q. L. Raman Spectroscopy Analysis and Application; National Defense Industry Press: Beijing, 2008; pp 210-220.
39. [39]
  [杨序纲, 吴琪琳. 拉曼光谱的分析与应用. 北京: 国防工业出版社, 2008: 210-220.]
  [杨序纲, 吴琪琳. 拉曼光谱的分析与应用. 北京: 国防工业出版社, 2008: 210-220.]

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

石墨烯薄膜的制备和结构表征

English

Synthesis and Structural Characterization of Graphene-Based Membranes

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

石墨烯薄膜的制备和结构表征

English

Synthesis and Structural Characterization of Graphene-Based Membranes

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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