以TiO_2和ZnO为基体的复合催化剂的制备、表征及其光催化性能的研究
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摘要
以氮化钛二氧化钛氟化铵为原料,采用球磨法制备异质结型光催化剂TiN/F-TiO_2;以BN和TiO_2二氧化钛为原料,采用球磨法制备异质结型光催化剂BN/TiO_2;以硝酸铜为原料,采用热分解的方法制备CuO,然后再把CuO、TiO_2和NH_4F为原料,采用球磨法制备异质结型光催化剂CuO/F-TiO_2;以硝酸钙和硝酸锌为原料,采用热分解的方法制备CaCO_3/ZnO。采用UV-Vis、XRD、XPS、SEM、TEM、PL、等仪器对光催化剂进行分析与表征。通过氧化亚甲基蓝、罗丹明B和还原Cr~(6+)来研究其在紫外光催化氧化和还原活性。结果表明,TiN/F-TiO_2中TiN的最佳量为0.2 wt%,最佳球磨时间为12小时;球磨法制备的BN/TiO_2中的光催化氧化性高于纯的TiO_2,BN最佳量为0.5%,最佳球磨时间为0.5小时;球磨法制备异质结型光催化剂CuO/F-TiO_2光催化氧化和还原性能优于纯的TiO_2,CuO最佳掺杂量为1.0wt.%;以硝酸锌硝酸钙为原料,采用共沉淀出前驱物后再用热分解的方法制备CaCO_3/ZnO。同时讨论热处理条件对其光催化活性的影响。复合型光催化剂较单一的光催化剂,光催化活性有一定的提高。
TiN/F-TiO_2 was prepared by ball milling and using TiO_2, TiN and NH4F as the raw materials. BN/TiO_2 was prepared by ball milling and using TiO_2 and BN as the raw materials. CuO was synthesized by heat decomposition of Cu(NO_3)_2.3H_2O, then CuO/F-TiO_2 was prepared by ball milling and using CuO, TiN and NH4F as the raw materials. CaCO_3/ZnO photocatalyst was prepared by decomposition of zinc nitrate at different heat treatment temperatures and time. The photocatalysts were characterized by UV–Vis diffuse reflection spectrum, X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fluorescence spectra (FL), and Scanning electron microscopy (SEM), ransmission electron microscopy (TEM). The photocatalytic activity of the photocatalyst was evaluated by photocatalytic reduction of Cr_2O_7~(2-) and photocatalytic oxidation of methylene blue (MB) and rhodamine B (RhB). The results show that the optimum percentage of doped TiN is 0.2 wt% in the TiN/F-TiO_2 and the optimum ball milling time is 12 h. The optimum percentage of doped BN of BN/TiO_2 is 0.5 wt% and the optimum ball milling time is 0.5 h. When the doped amount CuO was 1.0 wt. % and the CuO/ F-TiO_2 show the optimal activity.The photocatalytic activity of the CaCO_3/ZnO was higher than that of ZnO.
TiN/F-TiO_2 was prepared by ball milling and using TiO_2, TiN and NH4F as the raw materials. BN/TiO_2 was prepared by ball milling and using TiO_2 and BN as the raw materials. CuO was synthesized by heat decomposition of Cu(NO_3)_2.3H_2O, then CuO/F-TiO_2 was prepared by ball milling and using CuO, TiN and NH4F as the raw materials. CaCO_3/ZnO photocatalyst was prepared by decomposition of zinc nitrate at different heat treatment temperatures and time. The photocatalysts were characterized by UV–Vis diffuse reflection spectrum, X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fluorescence spectra (FL), and Scanning electron microscopy (SEM), ransmission electron microscopy (TEM). The photocatalytic activity of the photocatalyst was evaluated by photocatalytic reduction of Cr_2O_7~(2-) and photocatalytic oxidation of methylene blue (MB) and rhodamine B (RhB). The results show that the optimum percentage of doped TiN is 0.2 wt% in the TiN/F-TiO_2 and the optimum ball milling time is 12 h. The optimum percentage of doped BN of BN/TiO_2 is 0.5 wt% and the optimum ball milling time is 0.5 h. When the doped amount CuO was 1.0 wt. % and the CuO/ F-TiO_2 show the optimal activity.The photocatalytic activity of the CaCO_3/ZnO was higher than that of ZnO.
引文
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[15] J. Lin, J. Lin, and Y.F. Zhu, Controlled synthesis of the ZnWO4 nanostructure and effects on the photocatalytic performance, Inorg. Chem. 46 (2007) 8372–8378.
[16] B. Doggett, S. Chakrabarti, R. O’Haire, A. Meaney, E. McGlynn, M.O. Henry, and J.P. Mosnier, Electrical characterisation of phosphorus-doped ZnO thin films grown by pulsed laser deposition, Superlattices. Microstruct. 42 (2007) 74-78.
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[11] R.Y. Hong, S.Z. Zhang, G.Q. Di, H.Z. Li, Y. Zheng, J. Ding, D.G. Wei, Preparation, characterization and application of Fe3O4/ZnO core/shell magnetic nanoparticles, Mater. Res. Bull. 43 (2008) 2457–2468.
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[14] S. Moribe, T. Ikoma, K. Akiyama, Q.W. Zhang, F. Saito, and S.T. Kubota , EPR study on paramagnetic species in nitrogen-doped ZnO powders prepared by a mechanochemical method, Chem. Phys. Lett. 436 (2007) 4-6.
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[19] W.Liu, S.F. Chen, S.J. Zhang, W. Zhao, H.Y. Zhang, X.L. Yu, Preparation and characterization of p–n heterojunction photocatalyst p-CuBi2O4/n-TiO_2 with high photocatalytic activity under visible and UV light irradiation,J. Nanopart. Res. 12 (2010) 1355–1366.
[20] S.F. Chen, W. Zhao, W. Liu, and S.J. Zhang, Preparation, characterization and activity evaluation of p–n junction photocatalyst p-ZnO/n-TiO_2, Appl. Surf. Sci. 255 (2008) 2478–2484.
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[1] X.Q. Qiu, L.P. Li, J. Zheng, J.J. Liu, X.F. Sun, and G.S. Li, Origin of the enhanced photocatalytic activities of semiconductors: A case study of ZnO doped with Mg2+, J. Phys. Chem. C 112 (2008), pp.12242–12248.
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[6] Y.H. Zheng, C.Q. Chen, Y.Y. Zhan, X.Y. Lin, Q. Zheng, K. Wei, and J.F. Zhu, Photocatalytic activity of Ag/ZnO heterostructure nanocatalyst: correlation between structure and property, J. Phys. Chem. C 112 (2008), pp. 10773–10777.
[7] H. Tang, J.C. Chang, Y.Y. Shan, and S.T. Lee, Surfactant-assisted alignment of ZnO nanocrystals to superstructures, J. Phys. Chem. B 112 (2008), pp. 4016–4021.
[8] Z.H. Wen, G. Wang, W. Lu, Q. Wang, Q. Zhang, and J.H. Li, Enhanced photocatalytic properties of mesoporous SnO2 induced by low concentration ZnO doping,Cryst. Growth Des. 7 (2007), pp. 1722–1725.
[9] R.Y. Hong, S.Z. Zhang, G.Q. Di, H.Z. Li, Y. Zheng, J. Ding, and D.G. Wei, Preparation, characterization and application of Fe3O4/ZnO core/shell magnetic nanoparticles, Mater. Res. Bull. 43 (2008), pp.2457–2468.
[10] C.K.S.J. Doh, S.G. Lee, S.J. Lee, and H.Y. Kim, Visible-light absorptivity of a zincoxysulfide (ZnO_xS_(1-x)) composite semiconductor and its photocatalytic activities for degradation of organic pollutants under visible-light irradiation, Applied Catalysis A. 330 (2007), pp. 127-133.
[11] X. Wang, P. Hu, Y.F. Li, and L.J. Yu,Preparation and characterization of ZnO hollow spheres and ZnO-Carbon composite materials using colloidal carbon spheres as templates,J. Phys. Chem. C 111 (2007), pp. 6706–6712.
[12] S. Moribe, T. Ikoma, K. Akiyama, Q.W. Zhang, F. Saito, and S.T. Kubota , EPR study on paramagnetic species in nitrogen-doped ZnO powders prepared by a mechanochemical method, Chem. Phys. Lett. 436 (2007), pp. 4-6.
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