物理化学学报 >> 2010, Vol. 26 >> Issue (07): 2044-2048.doi: 10.3866/PKU.WHXB20100714

材料物理化学 上一篇    下一篇

高度b取向Silicalite-1分子筛膜的制备

王周翔, 闫文付, 田大勇, 曹学静, 于吉红, 徐如人   

  1. 吉林大学无机合成与制备化学国家重点实验室, 长春 130012
  • 收稿日期:2010-01-29 修回日期:2010-05-10 发布日期:2010-07-02
  • 通讯作者: 闫文付, 徐如人 E-mail:yanw@jlu.edu.cn; jihong@jlu.edu.cn

Preparation of Highly b-Oriented Silicalite-1 Films

WANG Zhou-Xiang, YAN Wen-Fu, TIAN Da-Yong, CAO Xue-Jing, YU Ji-Hong, Xu Ru-Ren   

  1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130012, P. R. China
  • Received:2010-01-29 Revised:2010-05-10 Published:2010-07-02
  • Contact: YAN Wen-Fu, YU Ji-Hong E-mail:yanw@jlu.edu.cn; jihong@jlu.edu.cn

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摘要：

以正硅酸乙酯(TEOS)为硅源, 四丙基氢氧化铵(TPAOH)为模板剂, 通过调变合成silicalite-1分子筛溶胶组成及反应时间等合成参数, 用原位水热晶化法在玻璃基底上制备了表面平整、连续性好且高度b取向的silicalite-1分子筛膜. 研究了溶胶组成及基底表面粗糙度与分子筛膜中晶体取向的关系, 讨论了晶化条件对分子筛膜厚度及膜中微晶尺寸及分布的影响, 实现了silicalite-1 沸石分子筛在基底表面的高度取向生长和膜中晶体大小及膜层微结构的调控. 本文描述的制备方法简单且重复性好. 此外, 还利用扫描电子显微镜(SEM)和X射线衍射(XRD)等分析方法对样品进行了表征.

关键词: 分子筛, Silicalite-1, 膜, 原位水热晶化, b取向

Abstract:

Using tetraethylorthosilicate (TEOS) as a silicon source and tetrapropylammonium hydroxide (TPAOH) as a structure-directing agent, we prepared highly b-oriented silicalite-1 thin films with smooth surfaces and excellent continuity by optimizing the preparation parameters such as the gel composition and reaction time. The influence of gel composition and substrate surface roughness on the orientation, size, and distribution of the microcrystals in the silicalite-1 thin films were investigated. We achieved highly orientated silicalite-1 crystal growth on the substrates as well as excellent control of crystal size and filmmicrostructure. The preparation procedure reported here is feasible and has excellent reproducibility. In addition, the thin films were further characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD).

Key words: Zeolite, Silicalite-1, Film, In situ hydrothermal crystallization, b-Orientation