Synthesis of water-soluble silicon oxide material by sol-gel reaction in tetraalkoxysilane-aminoalkyltrialkoxysilane bin
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Nobuo Iyi Advanced Materials Laboratory, National Institute for Materials Science (NIMS), Tsukuba, Ibaraki 305-0044, Japan
Taki Matsumoto and Hisanao Usami Department of Fine Materials Engineering, Faculty of Textile Science and Technology, Shinshu University, Ueda 386-8567, Japan (Received 16 February 2005; accepted 2 May 2005)
A series of water-soluble silicon oxide materials was synthesized by the sol-gel reaction of tetramethoxysilane (TMOS)/3-aminopropyltrimethoxysilane (APTMOS) mixtures catalyzed by hydrochloric acid with varying TMOS/APTMOS ratios. Increase in TMOS composition made the products less water-soluble, and the richest TMOS composition for the water-soluble silicon oxide materials was found to be TMOS/APTMOS ⳱ 7/3 (mol/mol). Ultraviolet-visible spectroscopy of a 10 wt% aqueous solution of the product with TMOS/APTMOS ⳱ 7/3 showed a high transmittance in the visible region. Its infrared spectrum showed an absorption band attributable to the Si–O bond, and the 29Si dipole decoupled/magic angle spinning–nuclear magnetic resonance spectrum exhibited signals in the regions of T3, Q3, and Q4, indicating a dense siloxane network structure. A peak due to an ordered structure with a 1.76 nm periodicity was observed in the x-ray diffraction profile, and a stripe pattern was observed in the transmission electron microscopy image. These results indicate that the rodlike silicon oxide macromolecules with a 1–2-nm diameter stack parallel. Thus a silicon oxide material with nano-ordered structure was successfully formed and such a structure produced the water solubility.
I. INTRODUCTION
Preparation of hybrid materials (nanocomposites) by the combination of silicon oxide materials and various functional organic compounds has been extensively studied because the performance of organic compounds is expected to be improved due to the advantageous properties of the inorganic silicon oxide component (thermal and chemical stabilities, mechanical strength, transparency, etc.). Among silicon oxide materials, clay minerals have been widely applied as reinforcing agents in an organic polymer-matrix.1–5 In addition, the intercalation of photofunctional organic molecules into layered clay minerals has attracted much attention because the durability of these photofunctional molecules was
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Address all correspondence to this author. e-mail: [email protected] DOI: 10.1557/JMR.2005.0274 J. Mater. Res., Vol. 20, No. 8, Aug 2005
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improved.6,7 As another attractive example for preparing hybrid materials using silicon oxide materials, the surface modification of mesoporous silicas with various organic functional molecules has been reported.8–11 These materials can be used as specific adsorbents, e.g., removers of toxic metal ions. Furthermore, the preparation of hybrid materials using other silicon oxide materials, such as glass fibers12,13 and silica gels,14 has also been conducted. Generally, the hybridization of these silicon oxide materials with organic m
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