Structure/property behavior of inorganic/organic sol-gel derived hybrid materials
Brennan, Anthony Bartholomew
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A novel class of inorganic/ organic hybrid materials referred to as CERAMERs have been successfully prepared by a sol-gel process using a polymeric acid catalyst, poly(styrene sulfonic acid), to form a network from tetraethylorthosilicate (TEOS) and triethoxysilane end capped oligomers of poly( tetramethylene oxide) (PTMO). The structure-property relationships were determined for these hybrid networks from their dynamic mechanical behavior, mechanical properties, and SAXS behavior. Thermal gravimetric data coupled with FfIR analysis were used to obtain a qualitative measure of the extent of conversion of the metal alkoxides as a function of acid catalyst. Another new class of CERAMERs was successfully developed by the sol-gel processing of three different metal alkoxides in conjuction with the triethoxy silane end capped PTMO oligomers. The first novel hybrid is based upon complexes of aluminum tri-n-butoxide with ethyl acetoacetonate or titanium tetra-iso-propoxide with ethyl acetoacetate reacted with the triethoxysilane end capped PTMO. The hybrid networks were optically clear and could be easily formed as relatively large monoliths. A novel method of preparation of stable sols without the use of ethyl acetoacetate, developed by Dr. Bing Wang in this laboratory, led to more stable CERAMERS of titanium tetra-iso-propoxide (TiOPr) reacted with the functionalized P'TMO as well as a fourth inorganic/organic hybrid material based upon zirconium tetra-n-propoxide and PTMO. Indeed, the mechanical properties of the TiOPr/P'TMO CERAMERs and ZrOPr/P'TMO CERAMERs were significantly enhanced over the TEOS/PTMO CERAMERs in terms of both Young's modulus and stress at break. The structure-property relationships of these materials were adequately described by the morphological model originally developed for the CERAMERs based upon TEOS/PTMO.
- Doctoral Dissertations