MoS2修饰TiO2纳米管阵列光电化学性能研究

doi:10.15541/jim20160107

摘要/Abstract

摘要：

通过阳极氧化法在乙二醇电解液中制备TiO₂纳米管阵列, 以钼酸钠和硫脲作为钼源和硫源, 并添加半胱氨酸为辅助剂, 水热法制备纳米花状二硫化钼修饰的TiO₂纳米管阵列。用X射线衍射仪、扫描电子显微镜、能谱仪和拉曼光谱对复合材料的晶型、形貌、物相等进行分析, 通过电化学工作站测试复合材料的线性扫描伏安曲线、电化学阻抗谱和莫特-肖特基曲线。结果表明: MoS₂/TiO₂复合材料形貌比较规整均匀, MoS₂纳米花尺寸约为200 nm; MoS₂与TiO₂复合有利于形成异质结, 促进光生电子和空穴的分离; 当钼酸钠浓度为0.8 mmol/L时制备的复合材料光化学能转化率为纯氧化钛的2.89倍, 达到了1.65%, 而且复合材料的电荷转移电阻降低了约50%, 光生载流子浓度提高了24倍, 达到了3.38×10²³ cm^-3, 具有非常优异的光电化学性能。

关键词: 阳极氧化, TiO2纳米管阵列, 二硫化钼, 水热法

Abstract:

Well aligned TiO₂ nanotube arrays were grown by anodization method on Ti foils in ethylene glycol electrolyte. Flowers-like molybdenum disulfide composed with nanoflakes was synthesized by hydrothermal process on TiO₂ nanotube arrays, using sodium molybdate, thiourea and L-Cysteine as reactants. The obtained samples were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM) equipped with energy dispersive X-ray detector. Linear sweeps voltammetry, electrochemical impedance spectroscopy and Mott-Schottky plots of samples were analyzed by electrochemical workstation. The results showed that a flowers-like MoS₂ with diameter of c.a. 200 nm was synthesized, forming a heterojunction between TiO₂ nanotube arrays and MoS₂, which can effectively promote the separation of photogenerated charges, reduce the electron-hole recombination. Optimum concentration of sodium molybdate was obtained at 0.8 mmol/L, its corresponding photoconversion efficiency reached 1.65%, which was 2.89 times as high as that of pure TiO₂, and the charge transfer resistance decreased approximately 50%. The MoS₂/TiO₂ composite exhibited high carrier density of 3.38×10²³ cm^-3, which was about 24 times higher than that of pure TiO₂ nanotube arrays.

Key words: anodization, TiO2 nanotube arrays, molybdenum disulfide, hydrothermal method

中图分类号:

TQ174

于濂清, 黄承兴, 张亚萍, 董开拓, 郝兰众. MoS₂修饰TiO₂纳米管阵列光电化学性能研究[J]. 无机材料学报, 2016, 31(11): 1237-1241.

YU Lian-Qing, HUANG Cheng-Xing, ZHANG Ya-Ping, DONG Kai-Tuo, HAO Lan-Zhong. Photoelectrochemical Properties of MoS₂ Modified TiO₂ Nanotube Arrays[J]. Journal of Inorganic Materials, 2016, 31(11): 1237-1241.

图/表 6

图1 MoS2/TiO2样品的XRD图谱

Fig. 1 XRD patterns of MoS2/TiO2

图2 样品0.8-MT和1.5-MT拉曼图谱

Fig. 2 Raman spectra of samples 0.8-MT, 1.5-MT

图3 (a)纯TiO2, (b)样品 0.8-MT和(c)样品 1.5-MT的SEM图片, (d) 样品0.8-MT的EDS分析

Fig. 3 SEM images of (a) pure TiO2, (b) sample 0.8-MT, and (c) sample 1.5-MT, (d) EDS analysis of sample 0.8-MT

图4 MoS2/TiO2线性扫描伏安曲线(a)和光化学能转换率(b)

Fig. 4 (a) Linear sweep voltammograms and (b) photoconversion efficiency curves of MoS2/TiO2

图5 MoS2/TiO2的电化学抗谱(插图为等效电路图) (a)和莫特-肖特基曲线(b)

Fig. 5 (a) Nyquist plots (Insert: equivalent circuit fitting the EIS) and (b) Mott-Schottky plots of MoS2/TiO2

表1 MoS2/TiO2复合物各物理参数值

Table 1 Physics parameters of MoS2/TiO2

Sample	R_ct /(Ω·cm^-2)	V_fb/V (vs Ag/AgCl)	N_D /cm^-3
0.4-MT	507.6	-0.448	1.40×10²³
0.8-MT	407.4	-0.395	3.38×10²³
1.5-MT	375.6	-0.533	4.02×10²²
3-MT	322.5	-0.508	7.66×10²²
Pure TiO₂	594.8	-0.612	1.35×10²²

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MoS₂修饰TiO₂纳米管阵列光电化学性能研究

Photoelectrochemical Properties of MoS₂ Modified TiO₂ Nanotube Arrays

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