滴涂法制备石墨烯/碳纳米管复合薄膜及其表征

doi:10.15541/jim20160299

摘要/Abstract

摘要：

以化学气相沉积(CVD)法制备的石墨烯和碳纳米管的邻二氯苯分散液为原料, 采用滴涂法制备石墨烯/碳纳米管复合薄膜, 用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、拉曼光谱(Raman)和X射线光电子能谱(XPS)对其形貌和结构进行表征。实验发现随着碳纳米管分散液浓度的增大, 复合薄膜结构中碳纳米管的面密度线性增大。利用紫外-可见光谱仪和四探针测试仪表征了不同碳纳米管浓度下复合薄膜的透光率及其薄层电阻, 结果表明: 随着碳纳米管浓度的增大, 复合薄膜的透光率及其薄层电阻都将减小, 当碳纳米管浓度为0.1 mg/mL时, 复合薄膜的透光率(550 nm)及其薄层电阻分别为92.18%和0.998 kΩ/□。实验通过调节碳纳米管浓度制备得到不同性能的石墨烯/碳纳米管复合薄膜, 该复合薄膜在透明电极、场效应晶体管和激光锁模等方面具有潜在应用。

关键词: 石墨烯, 碳纳米管, 复合薄膜, 滴涂法

Abstract:

Hybrid thin films were prepared via a drop-coating method by using graphene prepared by chemical vapor deposition(CVD) and carbon nanotube dispersed in 1, 2-dichlorobenzene as crude materials. The structure and morphology of hybrid thin films were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It was found that surface density of carbon nanotube in the hybrid thin films increased linearly with the increase of dispersion concentration. Furthermore, the transmittance and sheet resistance of the hybrid thin films, which were characterized by UV-visible spectroscope and four-point probe analyzer, respectively, both significant decreased when concentration of the dispersed carbon nanotube increased. The two parameters, to be specific, were found to be 92.18% (at 550 nm) and 0.998 kΩ/□, respectively as the concentration of the dispersed carbon nanotube reaching 0.1 mg/mL. In other words, the performances of the hybrid thin films can be improved by regulating concentration of carbon nanotube in the dispersion, showing the films potential applications in the fields of transparent electrodes, field effect transistors and laser mode-locking.

Key words: graphene, carbon nanotube, hybrid thin films, drop-coating

中图分类号:

TB332

黄维, 朱家艺, 李浩, 杨曦, 王朝阳, 付志兵. 滴涂法制备石墨烯/碳纳米管复合薄膜及其表征[J]. 无机材料学报, 2017, 32(2): 203-209.

HUANG Wei, ZHU Jia-Yi, LI Hao, YANG Xi, WANG Chao-Yang, FU Zhi-Bing. Preparation and Characterization of Graphene/Carbon Nanotube Hybrid Thin Films by Drop-coating[J]. Journal of Inorganic Materials, 2017, 32(2): 203-209.

图/表 7

图1 未处理(a)和硝酸预处理(b)退火后的铜箔的SEM照片, 石墨烯/铜箔的高倍(c)和低倍(d)SEM照片

Fig. 1 SEM images of the pristine copper foil (a) and nitric acid pre-cleaned copper foil (b) after annealing, high- (c) and low- (d) magnification SEM images of graphene/Cu

图2 (a)不同碳纳米管分散体系的照片, (b)分散的碳纳米管SEM照片和(c)石墨烯薄膜与不同分散液接触角测量的照片

Fig. 2 (a) Photo of carbon nanotube dispersed in different dispersion system, (b) SEM image of dispersive carbon nanotube, and (c) schematic pictures of contact angle measurement of graphene films with different dispersion

图3 不同碳纳米管浓度下复合薄膜的SEM照片(a~e), 碳纳米管面密度随分散液浓度的变化曲线(f)

Fig. 3 SEM images of hybrid thin films with different concentration of carbon nanotube (a-e), and curve of surface density of carbon nanotube vs concentration changes of dispersion (f) Carbon nanotube concentration (a-e): 0.02, 0.04, 0.06, 0.08, 0.1 mg/mL

图4 石墨烯的高倍TEM照片(a)和电子衍射谱(b), 石墨烯/碳纳米管复合薄膜的低倍(c)和高倍(d)TEM照片

Fig. 4 High-magnification TEM image (a) and electron diffraction pattern (b) of graphene, and low-magnification (c) and high-magnification (d) TEM images of hybrid thin films

图5 碳纳米管/石墨烯/ SiO2的XPS图谱

Fig. 5 XPS spectrum of carbon nanotube/graphene/SiO2

图6 石墨烯(a,c)和石墨烯/碳纳米管复合薄膜(b,d)的拉曼光谱图

Fig. 6 Raman spectra of graphene films (a,c) and graphene/carbon nanotube hybrid films (b,d)(a and b) RBM of graphene and graphene/ carbon nanotube hybrid films, respectively

图7 转移至K9玻璃上的复合薄膜的照片(a), 不同碳纳米管浓度下复合薄膜的透光性曲线(b)及复合薄膜的透光率和薄层电阻随碳纳米管浓度的变化曲线(c)

Fig. 7 Image of hybrid film transferred on K9 glass (a), transmittance curve of hybrid thin films with different concentrations of carbon nanotube (b), and curve of transmittance and sheet resistance of hybrid films vs concentration changes of carbon nanotube (c)

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