硫属化合物复合薄膜的制备及光电性质研究
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摘要
金属硫属化物(如硫化物、硒化物和碲化物等)纳米材料具有独特的光电性质,在太阳能电池等方面有广泛的应用前景。将金属硫属化物与TiO2复合,可以提高材料的光电转换效率,是光电材料领域的研究热点之
本论文首先应用聚乙二醇(PEG)作为造孔剂,制备了多孔Ti02薄膜,然后将Ag2Se、PbSe、SnS等金属硫属化合物沉积其表面,制备复合薄膜。采用扫描电镜(SEM)、X射线衍射(XRD)、紫外—可见光谱(UV-vis)等测试技术对所得薄膜进行了表征,探讨了所得薄膜的形成过程及影响因素,并以氙灯作为光源,研究了各种薄膜的光电转换性质。
主要研究内容如下：
1.Ag2Se／Ti02纳米复合薄膜的制备及其光电性质研究
在Ti02溶胶中加入PEG,采用浸渍提拉法首先在导电玻璃上制备多孔Ti02薄膜,然后利用界面反应将Ag2Se沉积到Ti02薄膜上,制备Ag2Se／Ti02复合薄膜。采用XRD、SEM、UV-vis等测试技术对所得薄膜进行表征。以氙灯作为光源,用电化学工作站测试各种薄膜的光电转换性质,探讨溶胶中PEG的加入量对薄膜光电转换性质的影响。结果表明：Ag2Se／Ti02复合薄膜的光电性质优于纯Ti02薄膜,当PEG加入量为10%时其光电流最大。
2.PbSe／BaTiO3／Ti02纳米复合薄膜的制备及其光电性质的研究
首先以浸渍提拉的方式在导电玻璃上制备多孔Ti02薄膜,然后将溶胶-凝胶法制备的BaTi03复合在TiO2薄膜表面,最后采用界面反应将PbSe沉积到BaTi03／Ti02薄膜上,制备出PbSe／BaTi03／Ti02复合薄膜。用XRD和SEM方法对各种薄膜和纳米粒子进行表征,利用UV-vis测定其光学性质。以氙灯作为光源,用电化学工作站测试各种薄膜的光电流和开路电压,探讨其光电转换性质。结果表明：由于BaTi03的引入,减少了空穴与载流子的无效复合,使所得PbSe／BaTiO3／Ti02复合薄膜能产生大的光电流。
3.SnS／TiO2纳米复合薄膜的制备及其光电性质研究
首先采用浸渍提拉法在导电玻璃上制备多孔TiO2薄膜,然后在常温下用界面反应将SnS沉积到TiO2薄膜上。用XRD、SEM、UV-vis等测试技术对各种薄膜进行表征。用氙灯作为光源,采用电化学工作站测试各种薄膜的光电流和开路电压,探讨其光电转换性质。结果表明：合成薄膜表面的SnS粒径为几十纳米,由于其在可见光区有强的吸收,拓宽了薄膜的光电响应范围,因而使所得SnS／Ti02复合薄膜能产生大的光电流和开路电压。
Metal chalcogenide (such as selenide, sulfide and telluride) nano-materials have special photoelectric properties, and wide potential applications in solar cell and others. The efficiency of photo-electric transformation would be heightened by complexing metal chalcogenide with TiO2, which is a hot field in photoelectric materials.
In this paper, the porous TiO2 thin film was first prepared by adding PEG in the TiO2 sol. Then, the composite films were constructed by depositing Ag2Se, PbSe and SnS on the surface TiO2 thin film. The films as-abtained were characterized by Scanning Electron Microscope (SEM), X-ray Diffraction (XRD), Ultraviolet-visible Spectrophotometer (UV-vis). The formation mechanism and the influence factors for the films were exploited. With the xenon lamp light as source, the photoelectric conversion performance of the films was examined.
Main work as follows:
1. The preparation and photoelectric performance of Ag2Se/TiO2 interface composite film
First, the porous TiO2 film was prepared with conduct glass plate by dipping-lifting process in the sol mixing PEG. Then, the Ag2Se/TiO2 composite film was made through the interfacial reaction of Ag2Se. The films as-obtained were characterized by SEM, XRD, and UV-vis. The photoelectric conversion performance of the films was examined by electeochemical workstation with xenon lamp light source. The effect of the amount of the PEG in the sol on the photoelectric conversion was studied. The results show that the photoelectric conversion efficiency of the Ag2Se/TiO2 composite film is higher than that of the pure TiO2 film. The largest photocurrent was obtained by the Ag2Se/TiO2 composite film prepared with the amount of the 10% PEG in the sol.
2. The preparation and photoelectric performance of PbSe/BaTiO3/ TiO2 interface composite film
First, the TiO2 film on the conduct glass plate was prepared by dipping-lifting process with sol-gel solution. Then, the BaTiO3 was deposited on the surface of the TiO2 film by sol-gel method. Finally, the PbSe/BaTiO3/TiO2 composite film was prepared by the interfacial reaction of PbSe. The films as-obtained were characterized by SEM, XRD and UV-vis. The photoelectric conversion performance of the films was examined by electeochemical workstation with xenon lamp light source. The results show that the large photocurrent can be obtained with the PbSe/ BaTiO3/TiO2 composite film since the useless recombination of the hole and electron was decreased in the presence of BaTiO3.
3. The preparation and photoelectric performance of SnS/TiO2 interface composite film
First, the TiO2 film on the conduct glass plate was prepared by dipping-lifting process with sol-gel solution. Then, the SnS/TiO2 composite film was made by depositing SnS on the surface of the TiO2 film at room temperature. The films as-obtained were characterized by SEM, XRD and UV-vis. Using the xenon lamp light as source, the photoelectric conversion performance of the films were examined by electeochemical workstation. The results show that the large photocurrent and open circuit voltage can be obtained with the SnS/TiO2 composite film, since the SnS has strong absorption in visible light district, which broadens the scope of its optical response.
本论文首先应用聚乙二醇(PEG)作为造孔剂,制备了多孔Ti02薄膜,然后将Ag2Se、PbSe、SnS等金属硫属化合物沉积其表面,制备复合薄膜。采用扫描电镜(SEM)、X射线衍射(XRD)、紫外—可见光谱(UV-vis)等测试技术对所得薄膜进行了表征,探讨了所得薄膜的形成过程及影响因素,并以氙灯作为光源,研究了各种薄膜的光电转换性质。
主要研究内容如下：
1.Ag2Se／Ti02纳米复合薄膜的制备及其光电性质研究
在Ti02溶胶中加入PEG,采用浸渍提拉法首先在导电玻璃上制备多孔Ti02薄膜,然后利用界面反应将Ag2Se沉积到Ti02薄膜上,制备Ag2Se／Ti02复合薄膜。采用XRD、SEM、UV-vis等测试技术对所得薄膜进行表征。以氙灯作为光源,用电化学工作站测试各种薄膜的光电转换性质,探讨溶胶中PEG的加入量对薄膜光电转换性质的影响。结果表明：Ag2Se／Ti02复合薄膜的光电性质优于纯Ti02薄膜,当PEG加入量为10%时其光电流最大。
2.PbSe／BaTiO3／Ti02纳米复合薄膜的制备及其光电性质的研究
首先以浸渍提拉的方式在导电玻璃上制备多孔Ti02薄膜,然后将溶胶-凝胶法制备的BaTi03复合在TiO2薄膜表面,最后采用界面反应将PbSe沉积到BaTi03／Ti02薄膜上,制备出PbSe／BaTi03／Ti02复合薄膜。用XRD和SEM方法对各种薄膜和纳米粒子进行表征,利用UV-vis测定其光学性质。以氙灯作为光源,用电化学工作站测试各种薄膜的光电流和开路电压,探讨其光电转换性质。结果表明：由于BaTi03的引入,减少了空穴与载流子的无效复合,使所得PbSe／BaTiO3／Ti02复合薄膜能产生大的光电流。
3.SnS／TiO2纳米复合薄膜的制备及其光电性质研究
首先采用浸渍提拉法在导电玻璃上制备多孔TiO2薄膜,然后在常温下用界面反应将SnS沉积到TiO2薄膜上。用XRD、SEM、UV-vis等测试技术对各种薄膜进行表征。用氙灯作为光源,采用电化学工作站测试各种薄膜的光电流和开路电压,探讨其光电转换性质。结果表明：合成薄膜表面的SnS粒径为几十纳米,由于其在可见光区有强的吸收,拓宽了薄膜的光电响应范围,因而使所得SnS／Ti02复合薄膜能产生大的光电流和开路电压。
Metal chalcogenide (such as selenide, sulfide and telluride) nano-materials have special photoelectric properties, and wide potential applications in solar cell and others. The efficiency of photo-electric transformation would be heightened by complexing metal chalcogenide with TiO2, which is a hot field in photoelectric materials.
In this paper, the porous TiO2 thin film was first prepared by adding PEG in the TiO2 sol. Then, the composite films were constructed by depositing Ag2Se, PbSe and SnS on the surface TiO2 thin film. The films as-abtained were characterized by Scanning Electron Microscope (SEM), X-ray Diffraction (XRD), Ultraviolet-visible Spectrophotometer (UV-vis). The formation mechanism and the influence factors for the films were exploited. With the xenon lamp light as source, the photoelectric conversion performance of the films was examined.
Main work as follows:
1. The preparation and photoelectric performance of Ag2Se/TiO2 interface composite film
First, the porous TiO2 film was prepared with conduct glass plate by dipping-lifting process in the sol mixing PEG. Then, the Ag2Se/TiO2 composite film was made through the interfacial reaction of Ag2Se. The films as-obtained were characterized by SEM, XRD, and UV-vis. The photoelectric conversion performance of the films was examined by electeochemical workstation with xenon lamp light source. The effect of the amount of the PEG in the sol on the photoelectric conversion was studied. The results show that the photoelectric conversion efficiency of the Ag2Se/TiO2 composite film is higher than that of the pure TiO2 film. The largest photocurrent was obtained by the Ag2Se/TiO2 composite film prepared with the amount of the 10% PEG in the sol.
2. The preparation and photoelectric performance of PbSe/BaTiO3/ TiO2 interface composite film
First, the TiO2 film on the conduct glass plate was prepared by dipping-lifting process with sol-gel solution. Then, the BaTiO3 was deposited on the surface of the TiO2 film by sol-gel method. Finally, the PbSe/BaTiO3/TiO2 composite film was prepared by the interfacial reaction of PbSe. The films as-obtained were characterized by SEM, XRD and UV-vis. The photoelectric conversion performance of the films was examined by electeochemical workstation with xenon lamp light source. The results show that the large photocurrent can be obtained with the PbSe/ BaTiO3/TiO2 composite film since the useless recombination of the hole and electron was decreased in the presence of BaTiO3.
3. The preparation and photoelectric performance of SnS/TiO2 interface composite film
First, the TiO2 film on the conduct glass plate was prepared by dipping-lifting process with sol-gel solution. Then, the SnS/TiO2 composite film was made by depositing SnS on the surface of the TiO2 film at room temperature. The films as-obtained were characterized by SEM, XRD and UV-vis. Using the xenon lamp light as source, the photoelectric conversion performance of the films were examined by electeochemical workstation. The results show that the large photocurrent and open circuit voltage can be obtained with the SnS/TiO2 composite film, since the SnS has strong absorption in visible light district, which broadens the scope of its optical response.
引文
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[14]G. Beck, J. Janek. Negative and linear positive magnetoresistance effect in silver-rich silver selenide [J]. Solid State Sciences,2008,10 (6):776-789.
[15]Yong Cui, Gang Chen. Solvothermal syntheses of β-Ag2Se crystals with novel morphologies [J]. Journal of Solid State Chemistry,2003,172 (1):17-21.
[16]Z. Y. Jiang, R. B. Huang. Synthesis of Silver Selenide Bicomponent Nanoparticles by a Novel Technique:Laser' Solid' Liquid Ablation [J]. Journal of Solid State Chemistry,2001,160(2):430-434.
[17]Robel I, Subramanian V,Kuno M. Quantum dot solar cells. Har-vesting light energy with CdSe nanocrystals molecularly linked to mesoscopic TiO2 films[J]. J Am Chem Soc,2006,128:2385-2393.
[18]Gerischer H, Luebke M. A particle size effect in the sensitization of TiO2 electrodes by a CdS deposit[J]. J Electroanal Chem,1986,204:225-227.
[1]王冬至,刘福田.多孔纳米二氧化钦薄膜的制备及其光催化活性[J].陶瓷学报,2006,27(4)：397-401.
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[4]Xiang Dong, Jie Tao. Enhanced photoelectrochemical properties of F-containing TiO2 sphere thin film induced by its novel hierarchical structure[J]. Applied Surface Science,2009,255 (16) 7183-7187.
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[6]OliviaNiitsool,ShaibalK.Sarkar. Chemical bath deposited CdS/CdSe-sensitized porous TiO2 solar cells [J]. Journal of Photochemistry and Photobiology A: Chemistry,2006,181 (2-3):306-313.
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[8]P. Sudhagar, June Hyuk Jung, Suil Park, R. Sathyamoorthy. Self-assembled CdS quantum dots-sensitized TiO2 nanospheroidal solar cells:Structural and charge transport analysis [J]. Electrochimica Acta,2009,55 (1):113-117.
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[12]Daqin Yun, WeiFeng, HongcaiWu. Efficient conjugated polymer-ZnSe and-PbSe nanocrystals hybrid photovoltaic cells through full solar spectrum utilization[J]. Solar Energy Materials and Solar Cells,2009,93 (8):1208-1213.
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[15]Ki-Deuk Min,Jongwon Lee. Influences of particle size upon room temperature structure of BaTiO3 thin films onp-Si substrates[J]. J Mater Sci:Mater Electron, 2008,19(1):85-90.
[16]Bo Li,Shuren Zhang. Preparation of BaTiO3-based ceramics by nanocomposite doping process[J]. J Mater Sci,2007,42(6):2090-2096.
[17]L.Gomathi Devi, G.Krishnamurthy. TiO2/BaTiO3-assisted photocatalytic mineralization of diclofop-methyl on UV-light irradiation in the presence of oxidizing agents[J]. Journal of Hazardous Materials,2009,162 (2-3):899-905.
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[19]I. Robel, V. Subramanian, M. Kuno. Harvesting Light Energy with CdSe Nanocrystals Molecularly Linked to Mesoscopic TiO2 Films[J]. J.Am. Chem. Soc,2006,128(7):2385-2393.
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[1]LI Qian, ZHANG Xiu lian. Synthesis of TiO2 Nano structured Film Composed of Needle Shaped Particles[J]. Chemical Research,2006,17(1):20-23.
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[1]王冬至,刘福田.多孔纳米二氧化钦薄膜的制备及其光催化活性[J].陶瓷学报,2006,27(4)：397-401.
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[3]Jirapat Ananpattarachai, Puangrat Kajitvichyanukul. Visible light absorption ability and photocatalytic oxidation activity of various interstitial N-doped TiO2 prepared from different nitrogen dopants[J]. Journal of Hazardous Materials,2009, 168(1):253-261.
[4]Xiang Dong, Jie Tao. Enhanced photoelectrochemical properties of F-containing TiO2 sphere thin film induced by its novel hierarchical structure[J]. Applied Surface Science,2009,255 (16) 7183-7187.
[5]Chuen-Shii Chou, Ru-Yuan Yang. Preparation of TiO2/Nano-metal composite particles and their applications in dye-sensitized solar cells[J]. Powder Technology,2009,194 (1-2):95-105.
[6]OliviaNiitsool,ShaibalK.Sarkar. Chemical bath deposited CdS/CdSe-sensitized porous TiO2 solar cells [J]. Journal of Photochemistry and Photobiology A: Chemistry,2006,181 (2-3):306-313.
[7]R.S. Singh, V.K. Rangari, S. Sanagapalli. Nano-structured CdTe, CdS and TiO2 for thin film solar cell applications[J]. Solar Energy Materials and Solar Cells, 2004,82 (1-2):315-330.
[8]P. Sudhagar, June Hyuk Jung, Suil Park, R. Sathyamoorthy. Self-assembled CdS quantum dots-sensitized TiO2 nanospheroidal solar cells:Structural and charge transport analysis [J]. Electrochimica Acta,2009,55 (1):113-117.
[9]A. Munoz,J. Melendez,M.C. Torquemada. PbSe photodetector arrays for IR sensors [J]. Thin Solid Films,1998,317(1-2):425-428.
[10]V. Sholin, A.J.Breeze, I.E.Anderson, Y.Sahoo. All-inorganic CdSe/PbSe nanoparticle solar cells[J]. Solar Energy Materials & Solar Cells,
2008,92(18):1706-1711.
[11]Seiki Kitada, Einosuke Kikuchi, Akira Ohno. Effect of diamine treatment on the conversion efficiency of PbSe colloidal quantum dot solar cells[J]. Solid State Communications,2009,149 (41-42):1853-1855.
[12]Daqin Yun, WeiFeng, HongcaiWu. Efficient conjugated polymer-ZnSe and-PbSe nanocrystals hybrid photovoltaic cells through full solar spectrum utilization[J]. Solar Energy Materials and Solar Cells,2009,93 (8):1208-1213.
[13]Hugh W. Hillhouse, Matthew C. Beard. Solar cells from colloidal nanocrystals: Fundamentals, materials, devices, and economics[J]. Current Opinion in Colloid and Interface Science,2009,14 (4):245-259.
[14]曹鸣,操卫忠,杨新华.钛酸钡晶体压电性能的分子动力学模拟[J].压电与光,2009,31(2)：289-295.
[15]Ki-Deuk Min,Jongwon Lee. Influences of particle size upon room temperature structure of BaTiO3 thin films onp-Si substrates[J]. J Mater Sci:Mater Electron, 2008,19(1):85-90.
[16]Bo Li,Shuren Zhang. Preparation of BaTiO3-based ceramics by nanocomposite doping process[J]. J Mater Sci,2007,42(6):2090-2096.
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