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共缩聚法制备形貌可控的介孔氧化硅MCM-41

The Morphology Control of Mesoporous Silica MCM-41through Co-condensation Method

【作者】 陈曦

【导师】 蔡强;

【作者基本信息】 清华大学 , 材料科学与工程, 2012, 硕士

【摘要】 本论文以介孔氧化硅MCM-41的形貌控制为研究对象,通过共缩聚法分别合成出棒状形貌、纤维状形貌的介孔氧化硅MCM-41。对于棒状形貌的介孔氧化硅(MSNR:mesoporous silica nanorods)的制备,以表面活性剂十六烷基三甲基溴化铵(CTAB)作为模板剂,正硅酸乙酯(TEOS)、双[3-(三乙氧基硅)丙基]四硫化物(TESPT)为硅源物种,在极稀碱水溶液体系下进行共缩聚反应。对合成样品的微观形貌和内部介孔孔道结构进行了的表征和分析,讨论了溶剂量、共缩聚反应时间以及两种硅源的滴加方式对MSNR合成及棒状形貌的影响。同时探索了MSNR在离子吸附方面的应用,实验表明MSNR具有良好的重金属离子(Ag+、Cd2+)吸附能力。同样以十六烷基三甲基溴化铵作为模板剂,正硅酸乙酯、γ-巯丙基三甲氧基硅烷(MPTMS)为硅源,在单相水溶剂体系中通过共缩聚反应得到了纤维状形貌的介孔氧化硅(MSNF:mesoporous silica nanofibers)。同样对样品的微观形貌和内部孔道结构进行了全面的表征和分析,深入讨论了模板剂种类、硅源MPTMS、反应时间以及水溶剂用量对MSNF合成及纤维状形貌的影响,摸索出MSNF的最佳合成条件。另外,以正硅酸乙酯、双[3-(三乙氧基硅)丙基]四硫化物、γ-巯丙基三甲氧基硅烷三种有机物为硅源前驱体,通过共缩聚法制备出形貌不规整的介孔氧化硅颗粒。本论文中合成的多种不同形貌的介孔氧化硅材料在纳米尺寸下形貌规整、大小均一,内部介孔孔道排列高度有序,具有典型MCM-41介孔结构特征。因此在生物医药、光学器件、分离催化等应用领域具有广泛的实用价值。

【Abstract】 In this thesis we focus on the morphology control of mesoporous silica MCM-41through a base co-condensation method, in which two organoalkoxysilanes were used assilica precursors simultaneously. Rod-like and fiber-like mesoporous silica MCM-41were obtained.Using with hexadecyl trimethyl ammonium bromide (CTAB) as template,tetraethoxylsilane (TEOS) and bis[3-(triethoxysilyl)propyl]tetrasulfide (TESPT) as thesilica precursors, we had successfully prepared thiol-functionalized mesoporous silicananorods (MSNR). By scanning electron microscopy, transmission electron microscopy,small angle X-ray diffraction and nitrogen sorption measurements, the MSNR materialswere characterized as nanometer-sized MCM-41rods. We discussed the amount ofsolvent, the co-condensation time and the adding sequence of silica precursors on themorphology of MSNR. Such functional inner surface and its sorption character of heavymetal (Ag+、Cd2+) ions make the rod-like mesoporous silica suitable as promisingadsorbents for environmental application.Novel mesoporous silica nanofibers (MSNF) have been synthesized throughco-condensation method, in which two organoalkoxysilanes, TEOS and3-mercaptopropyl trimethoxysilane (MPTMS), were used as silica precursors. Themicrostructure as well as porous character of the MSNF had been characterized bymeans of scanning electron microscopy, transmission electron microscopy, small angleX-ray diffraction and nitrogen sorption measurements. We discussed the template,MPTMS, reaction time and the amount of solvent on the morphology of MSNF.TEOS, TESPT and MPTMS serving as the silica precursors simultaneously,however, no regular morphology of mesoporous silica nanomaterials were not obtained.Various mesoporous silica MCM-41with regular morphology and highly orderedinner mesostructure were obtained. They could be used widely in biomedicine, opticaldevice, separation and catalysis fields.

  • 【网络出版投稿人】 清华大学
  • 【网络出版年期】2013年 07期
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