Crepaldi Eduardo L, Soler-Illia Galo J de A A, Grosso David, Cagnol Florence, Ribot François, Sanchez Clément
Laboratoire de Chimie de la Matière Condensée, Université Pierre et Marie Curie - CNRS UMR 7574, Paris, France.
J Am Chem Soc. 2003 Aug 13;125(32):9770-86. doi: 10.1021/ja030070g.
In this paper, we report the complete synthesis and characterization procedures to generate highly organized and oriented mesoporous titania thin films, using poly(ethylene oxide) (PEO)-based templates. Controlled conditions in the deposition, postsynthesis, and thermal treatment steps allow one to tailor the final mesostructure (2D hexagonal, p6m, or 3D cubic, Im3m). Various techniques were used to determine the time evolution of the mesostructure. Spectroscopic techniques (UV/vis, (17)O NMR) and EXAFS/XANES have been used to follow the chemical changes in the Ti(IV) environment. Crossing these techniques spanning all ranges permits a complete description of the chemistry all the way from solution to the mesostructured metal oxide. A critical discussion on all important chemical and processing parameters is provided; the understanding of these features is essential for a rational design and the reproducible construction of mesoporous materials.
在本文中,我们报告了使用基于聚环氧乙烷(PEO)的模板生成高度有序且取向的介孔二氧化钛薄膜的完整合成及表征程序。沉积、合成后处理和热处理步骤中的可控条件使人们能够定制最终的介观结构(二维六方,p6m,或三维立方,Im3m)。我们使用了各种技术来确定介观结构随时间的演变。光谱技术(紫外/可见光谱、¹⁷O核磁共振)以及扩展X射线吸收精细结构/ X射线吸收近边结构已被用于追踪Ti(IV)环境中的化学变化。综合运用涵盖所有范围的这些技术,可以对从溶液到介观结构金属氧化物的整个化学过程进行完整描述。本文对所有重要的化学和加工参数进行了批判性讨论;理解这些特性对于介孔材料的合理设计和可重复构建至关重要。