立方相WO3薄膜的制备及表征

doi:10.3724/SP.J.1077.2010.01318

无机材料学报 ›› 2010, Vol. 25 ›› Issue (12): 1318-1324.DOI: 10.3724/SP.J.1077.2010.01318 CSTR: 32189.14.SP.J.1077.2010.01318

立方相WO₃薄膜的制备及表征

李文章¹, 李洁¹, 王旋^{1, 2}, 肖娟¹, 陈启元¹

(1. 中南大学化学化工学院, 有色金属资源化学教育部重点实验室, 长沙 410083; 2. 沈阳铝镁设计研究院, 沈阳 110001)

收稿日期:2010-03-20 修回日期:2010-05-16 出版日期:2010-12-20 网络出版日期:2010-11-24
基金资助:
国家863项目(2007A06Z129); 湖南省重大科技计划项目( 2008SK1001)

Preparation and Characterization of Cubic WO₃ Films

LI Wen-Zhang¹, LI Jie¹, WANG Xuan^{1, 2}, XIAO Juan¹, CHEN Qi-Yuan¹

(1. Key Laboratory of Resources Chemistry of Nonferrous Metals, Ministry of Education, Central South University, Changsha 410083, China; 2. Shenyang Aluminum & Magnesium Engineering & Research Institute, Shenyang 110001, China)

Received:2010-03-20 Revised:2010-05-16 Published:2010-12-20 Online:2010-11-24
Supported by:
863 Program (2007A06Z129); Key Science and Technology Project of Hunan Province (2008SK1001)

摘要/Abstract

摘要： 以偏钨酸铵(NH₄)₆W₇O₂₄× 6H₂O为钨源, 聚乙二醇(PEG)为配位聚合物, 采用聚合物前驱体法制备了立方晶相WO₃ (c-WO₃)薄膜, 利用X射线衍射、扫描电镜、能谱分析及高分辨透射电镜等手段对结构进行了表征, 并考察了煅烧温度、溶液pH值及镀膜衬底对WO₃薄膜晶体结构与形貌的影响. 结果表明, 以FTO导电玻璃为衬底, 450℃热处理3 h的样品为c-WO₃, 薄膜光滑平整, 均匀良好, 表面颗粒粒径为60 nm, 厚度为2.9 μm, 晶体生长有序度较高; 热处理温度在400~550℃和不同pH值条件下制得的薄膜均为立方晶体结构; 样品的颗粒粒径随前驱体溶胶pH值升高而减小; 以石英玻璃和石墨衬底镀膜得到的样品均为单斜晶体结构, 表明衬底对WO₃薄膜晶体结构具有明显的影响.

关键词: 立方相WO₃, 纳米薄膜, 聚合物前驱体法

Abstract: Cubic WO₃ films were prepared by the polymeric precursor method using ammonium metatungstate as precursor and polyethylene glycol as structure-directing agent. The obtained materials were characterized by means of X-ray diffraction (XRD), scanning electron microscope (SEM), energy disperse spectroscope (EDS) and high-resolution transmission electron microscope (HRTEM). The influence of calcination temperature, pH value and substrates on the structure and morphology of films was investigated. The results indicate that the surface morphology of the resulting film on FTO glass has particle of 60 nm in size as cubic WO₃ calcined at 450℃, and the films are smooth and glossy with an uniform thickness of 2.9 μm. The structures of all samples on FTO glass annealed at 450-550℃ or prepared at the different pH values are cubic WO₃. The particle size of the films decreases with the increase of the pH values. Monoclinic WO₃ is formed when the films are prepared on quartz glass and graphite substrate, indicating that the substrates have apparent influence on the crystal structure of WO₃ thin films.

Key words: cubic WO₃, nano-structured film, polymeric precursor method

中图分类号:

O614
TB383

李文章, 李洁, 王旋, 肖娟, 陈启元. 立方相WO₃薄膜的制备及表征[J]. 无机材料学报, 2010, 25(12): 1318-1324.

LI Wen-Zhang, LI Jie, WANG Xuan, XIAO Juan, CHEN Qi-Yuan. Preparation and Characterization of Cubic WO₃ Films[J]. Journal of Inorganic Materials, 2010, 25(12): 1318-1324.

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立方相WO₃薄膜的制备及表征

Preparation and Characterization of Cubic WO₃ Films

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