负载有立方相p-型半导体Cu1.8S颗粒的TiO2纳米带制备与表征

doi:10.3724/SP.J.1077.2012.00038

摘要/Abstract

摘要：

采用Cu₂O自牺牲模板法, 以负载有立方相p-型半导体Cu₂O颗粒的TiO₂纳米带作为前驱物, 在水热条件下与硫脲进行反应, 制得了负载有立方相p-型半导体Cu_1.8S颗粒的TiO₂纳米带. 测试结果表明, 反应温度、反应时间和硫脲浓度对Cu_1.8S纯度和形貌皆有影响. 若反应在较低温度(如120℃)进行, 即使反应时间达到25 h, 产物中除了生成Cu_1.8S还存在未反应Cu₂O; 若水热温度控制在160℃反应25 h, 当硫脲浓度为0.25 mol/L时, 负载物基本上是Cu_1.8S且分散较好, 当硫脲浓度升到0.5 mol/L时, 负载物团聚严重. 对罗丹明B的光催化降解活性测试结果表明, 与纯TiO₂纳米带相比, 在负载有Cu₂O或Cu_1.8S后光催化活性显著降低.

关键词: 复合材料, 立方相Cu_1.8S, TiO₂纳米带, 光催化, p-n异质结

Abstract:

TiO₂ nanobelts deposited with cubic p-type semiconductor Cu_1.8S particles were prepared using Cu₂O-deposited TiO₂ nanobelts and thiourea as precursors under hydrothermal condition by Cu₂O sacrificial template process. The measurement results show that the reaction temperature, reaction time and thiourea concentration have strong influence on the purity and morphology of Cu_1.8S particles. A mixture phases of Cu_1.8S and Cu₂O on TiO₂ nanobelts were obtained at 120℃ for 25 h within 0.5 mol/L of thiourea concentration. While reaction temperature was raised to 160℃, the Cu_1.8S particles with high purity exhibited obvious aggregation, whereas the Cu_1.8S particles with high purity and well dispersion were prepared under 0.25 mol/L of thiourea concentration. The photocatalytic activities in degradation of Rhodamine B solution demonstrate that the Cu_1.8S or Cu₂O-loading catalysts show lower photodegradation activities as compared with that of pure TiO₂ nanobelts.

Key words: composite, cubic Cu_1.8S, TiO₂nanobelts, photocatalytic activity, p-n heterojunction

中图分类号:

TB381

李丽, 雷静果, 嵇天浩, 张希鹏. 负载有立方相p-型半导体Cu_1.8S颗粒的TiO₂纳米带制备与表征[J]. 无机材料学报, 2012, 27(1): 38-44.

LI Li, LEI Jing-Guo, JI Tian-Hao, ZHANG Xi-Peng. Synthesis and Characterization of Cubic P-type Semiconductor Cu_1.8S-deposited TiO₂Nanobelts[J]. Journal of Inorganic Materials, 2012, 27(1): 38-44.

图/表 8

Table 1 Preparation condition of the cubic Cu1.8S-loaded TiO2 nanobelts

Sample	Cu₂O-TiO₂/g	C/(mol·L^-1)	T/℃	t/h
CT-1	3	0.25	160	5
CT-2	3	0.25	160	15
CT-3	3	0.25	160	25
CT-4	3	0.50	120	25
CT-5	3	0.50	160	5
CT-6	3	0.50	160	15
CT-7	3	0.50	160	25

图1 Cu2O-TiO2纳米带(a)、CT-1 (b)、CT-2 (c)、CT-3 (d)、CT-5 (e)、CT-6 (f)和CT-7 (g)的XRD图谱

Fig. 1 XRD patterns of Cu2O-TiO2 nanobelts (a), CT-1 (b), CT-2 (c), CT-3 (d), CT-5 (e), CT-6 (f) and CT-7(g)

图2 CT-3 (a)和纯TiO2纳米带(b)的拉曼光谱

Fig. 2 Raman spectra of CT-3 (a) and TiO2 nanobelts (b)

图3 前驱物Cu2O-TiO2纳米带(a)、CT-3 (b)、CT-4 (c)和CT-7 (d)的SEM及CT-3 的TEM照片 (e,f)

Fig. 3 SEM images of Cu2O-TiO2 nanobelts (a), CT-3 (b), CT-4 (c) and CT-7 (d) as well as TEM images of CT-3 (e,f)

图4 紫外-可见漫反射吸收光谱

Fig. 4 UV-Vis DRS of the products

图5 (a) Cu2O-TiO2纳米带; (b) CT-3; (c) CT-4; (d) CT-7产物的N2吸附/脱附曲线

Fig. 5 N2 adsorption/desorption isotherms of (a) Cu2O-TiO2 nanobelts; (b) CT-3; (c) CT-4; (d) CT-7

图6 H-CT-3、CT-3、CT-4和CT-7对罗丹明B的可见光光催化降解活性

Fig. 6 Visible-light photodegradation of Rhodamine B on H-CT-3, CT-3, CT-4 and CT-7 H-CT-3 is made from CT-3 dipping in dilute HCl solution for short time

图7 在CT-3光催化作用下罗丹明B的吸收光谱

Fig. 7 Absorption spectra of Rhodamine B solution at different reaction time with the catalysis of CT-3

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负载有立方相p-型半导体Cu_1.8S颗粒的TiO₂纳米带制备与表征

Synthesis and Characterization of Cubic P-type Semiconductor Cu_1.8S-deposited TiO₂Nanobelts

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