溶胶—凝胶水热法结合电泳技术（EPD）制备FeS_2薄膜的研究
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摘要
本论文首先综述了国内外光伏电池的研究进展，对太阳能电池的原理、结构和效率进行了阐述，并对FeS_2 光伏薄膜的的功能性质、发展情况、制备技术和应用前景进行了比较和概述。溶胶-凝胶水热法广泛地用于材料制备、化学反应和处理，是一个十分活跃的研究领域。本论文根据有关文献资料及在实验工作中我对水热法的研究实践，从基本理论、工艺设备、技术手段三个层次，简述了水热法的应用与发展。同时介绍了样品结构、光学及电学性质的分析测试方法和相关仪器的测试原理。
本论文总结了我在做毕业论文期间涉及的研究工作，主要分为两个阶段：第一阶段：采用溶胶-凝胶水热法，成功地合成了结晶良好的黄铁矿型FeS_2粉晶。定性地讨论了反应物的组成和配比、水热反应温度及反应时间等因素对FeS_2粉晶的结构特征及结晶形貌的影响，并定量地确定了合适的反应物配比，水热反应温度及反应时间范围。用XRD，FT-IR和SEM等分析手段对FeS_2粉晶进行了表征，这为其它黄铁矿结构的硫化物的合成开拓了一条新的途径。此外，借助简化的数学模型及相变理论讨论了溶胶-凝胶水热过程中FeS_2晶体的生长过程。第二阶段：将前期工作合成的FeS_2粉晶采用电泳沉积（EPD）技术制备出了FeS_2 光伏薄膜。并讨论了电泳沉积过程中沉积时间、沉积电流、FeS_2 粉体的加入量等工艺参数对薄膜结构、形貌及厚度变化的影响。制备出的FeS_2 (pyrite)薄膜的光学和电学性质表明了这种凝胶-溶胶水热法结合EPD沉积技术制备FeS_2 (pyrite)薄膜方法的优越性。
An overview is given on development of photovoltaic materials at home and abroad, and set forth the principle、structure and efficiency of solar cell. We have also overviewed functional properties, recent development and preparation techniques of FeS_2 thin film based on solar cells material. Sol-gel hydrothermal method can find a wide application in the field of material synthesis, chemical reaction and processing. In this thesis, we have systematically described elementary principle and technical equipment of this method. Analysis instruments relating structure、electric and optical properties have also been introduced.
The thesis is a summarization concerning research work during my graduate experience. During the first period, iron pyrite (FeS_2) crystalline particles was prepared using sol-gel hydrothermal method, which was characterized via XRD, FT-IR and SEM. It was found that reaction temperature and time, and sulfur pressure provided by some amount of sulfur could produce an impressive effect on controlling the formation of single-phase pyrite crystals, and the desirable reaction conditions was also concluded. A simplified mathematics model was established to analyze the crystal growth process. In the course of the second period, electrophoretic deposition (EPD) technique was used to deposit the as-prepared pyrite crystalline particles in an ethanol suspension. Furthermore, we have discussed the effects of deposit time, current density and deposit weight on structure, thickness and morphology of the pyrite films during the EPD process. Optical and electrical properties of the pyrite films prepared in this way indicate the superiority of this combined method.
本论文总结了我在做毕业论文期间涉及的研究工作，主要分为两个阶段：第一阶段：采用溶胶-凝胶水热法，成功地合成了结晶良好的黄铁矿型FeS_2粉晶。定性地讨论了反应物的组成和配比、水热反应温度及反应时间等因素对FeS_2粉晶的结构特征及结晶形貌的影响，并定量地确定了合适的反应物配比，水热反应温度及反应时间范围。用XRD，FT-IR和SEM等分析手段对FeS_2粉晶进行了表征，这为其它黄铁矿结构的硫化物的合成开拓了一条新的途径。此外，借助简化的数学模型及相变理论讨论了溶胶-凝胶水热过程中FeS_2晶体的生长过程。第二阶段：将前期工作合成的FeS_2粉晶采用电泳沉积（EPD）技术制备出了FeS_2 光伏薄膜。并讨论了电泳沉积过程中沉积时间、沉积电流、FeS_2 粉体的加入量等工艺参数对薄膜结构、形貌及厚度变化的影响。制备出的FeS_2 (pyrite)薄膜的光学和电学性质表明了这种凝胶-溶胶水热法结合EPD沉积技术制备FeS_2 (pyrite)薄膜方法的优越性。
An overview is given on development of photovoltaic materials at home and abroad, and set forth the principle、structure and efficiency of solar cell. We have also overviewed functional properties, recent development and preparation techniques of FeS_2 thin film based on solar cells material. Sol-gel hydrothermal method can find a wide application in the field of material synthesis, chemical reaction and processing. In this thesis, we have systematically described elementary principle and technical equipment of this method. Analysis instruments relating structure、electric and optical properties have also been introduced.
The thesis is a summarization concerning research work during my graduate experience. During the first period, iron pyrite (FeS_2) crystalline particles was prepared using sol-gel hydrothermal method, which was characterized via XRD, FT-IR and SEM. It was found that reaction temperature and time, and sulfur pressure provided by some amount of sulfur could produce an impressive effect on controlling the formation of single-phase pyrite crystals, and the desirable reaction conditions was also concluded. A simplified mathematics model was established to analyze the crystal growth process. In the course of the second period, electrophoretic deposition (EPD) technique was used to deposit the as-prepared pyrite crystalline particles in an ethanol suspension. Furthermore, we have discussed the effects of deposit time, current density and deposit weight on structure, thickness and morphology of the pyrite films during the EPD process. Optical and electrical properties of the pyrite films prepared in this way indicate the superiority of this combined method.
引文
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[7] Ennaoui A, Fiechter S, Jaegermann W, et al. J Electrochem Soc, Photoelectro-chemistry of highly quantum
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[9] Ferrer I J, Sanchez C. 1991, J Appl Phys, 70 (5): 2641
[10] Smestad G, Ennaoui A, et al. 1990, Solar Energy Materials, 20(3): 149
[11] Alonso2Vante N, Chatzitheodorou G, et al. 1988, Solar Energy Materials, 18 (1): 9
[2] A. Shah, et al., 6th Photovoltaic Specialists Conference, 1997, 569
[3] Staebler D l, Wroskicr, et al . 1977, Appl Phys Lett, 31: 292
[4] 刘世友. 铜铟硒太阳电池的生产与发展[J], 1999, 太阳能, 2: 1
[5] H. Takakura, et al., International Solar Energy Society, 1997 Solar World Conference, 11
[6] Ennaoui A, Tributsch H, 1984 Solar Cells, 1
[7] Ennaoui A, Fiechter S, Jaegermann W, et al. J Electrochem Soc, Photoelectro-chemistry of highly quantum
[8] Fiechter S, Mai J ,Ennaoui A. 1986, Journal of Crystal Growth, 78 (3): 438
[9] Ferrer I J, Sanchez C. 1991, J Appl Phys, 70 (5): 2641
[10] Smestad G, Ennaoui A, et al. 1990, Solar Energy Materials, 20(3): 149
[11] Alonso2Vante N, Chatzitheodorou G, et al. 1988, Solar Energy Materials, 18 (1): 9
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