溶剂热法合成In_2Se_3/CuSe复合粉及CuInSe_2薄膜的制备  

Synthesis of In_2Se_3/CuSe Composite Powders by Solvothermal Method and Preparation of CuInSe_2 Thin Film

作　　者：梁凤基[1] 龙飞[1] 莫淑一[1] 高耀[1] 邹正光[1] 

机构地区：[1]桂林理工大学材料科学与工程学院,桂林541004

出　　处：《人工晶体学报》2014年第7期1705-1712,共8页Journal of Synthetic Crystals

基　　金：国家高技术研究发展计划(863计划)(2012AA050704)

摘　　要：采用常压下两步溶剂热法合成了In2Se3/CuSe复合粉,并以其为原料,通过喷涂成膜后快速热处理制备了CuInSe2(CIS)薄膜。利用XRD、FE-SEM、EDS对In2Se3/CuSe复合粉的晶体结构和形貌进行分析表征,研究了溶剂热合成过程中的反应温度、表面活性剂对In2Se3/CuSe复合粉体物相及形貌的影响。结果表明:以InCl3·4H2O、Se粉为原料,聚乙二醇-400、水合肼、醋酸为溶剂于120℃下反应30 min可以成功合成出结晶性良好的纯相In2Se3纳米球,直径分布在50～100 nm之间;以In2Se3纳米粉作为中间产物,分散于乙二醇溶剂中,加入Se源溶液(水合肼溶解Se粉)及CuCl2·2H2O,90℃下反应30 min可获得In2Se3/CuSe复合粉,其中CuSe呈不规则团聚状均匀分布在In2Se3纳米球的周围,且当加入0.2 g CTAB时获得的In2Se3/CuSe复合粉分散性较好。采用FE-SEM、EDS、XRF和Raman光谱对预置膜和快速热处理后获得的CIS薄膜的形貌和成分进行表征。结果表明:将In2Se3/CuSe复合粉制备成"墨水"后涂覆在镀Mo玻璃基板上,快速升温至550℃可成功获得致密的CIS薄膜。The CuInSe2（CIS） thin film was obtained by spraying the In2Se3/CuSe composite powders ＂ink＂ and the following rapid thermal process based on the In2Se3/CuSe composite powders prepared by two-step solvothermal method under ambient pressure. The crystal structure and morphology of the In2Se3/CuSe composite powders were characterized by XRD,FE-SEM,EDS,and the effects of reaction temperature and the surfactant on phase and morphology of the In2Se3/CuSe composite powders were investigated. The results indicate that using the InCl3·4H2O and Se powders as the raw materials,the polyethylene glycol,hydrazine hydrate and acetic acid as the solvents,the good crystallinity and pure phase of In2Se3 nanospheres with the diameter of 50-100 nm could be successfully synthesized at 120 ℃for 30 min; then using the as-prepared In2Se3 powders as the intermediate products and dispersing them in the ethylene glycol,in which the Se source solution that the Se powders were dissolved in hydrazineand CuCl2·2H2O were added,the In2Se3/CuSe composite powders could be obtained at 90 ℃ for 30 min. Among that the obtained CuSe exhibited irregular agglomerates and well distributed around the In2Se3 nanospheres. Moreover,when adding 0. 2 g CTAB to the synthesis system,the dispersion of In2Se3/CuSe composite powders were better than the situation of without CTAB. The morphology and composition of the as-prepared thin film and the CIS thin film after rapid thermal process was characterized by FE-SEM,EDS,XRF and Raman spectroscopy. The result indicated that the CIS compact thin film was successfully acquired by spraying the In2Se3/CuSe composite powders ＂ ink＂ onto the Mo /glass substrate and the following RTP at 550 ℃.

关 键 词：溶剂热 In2Se3 CuSe复合粉 CIS薄膜 

分 类 号：TN304.2[电子电信—物理电子学]