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Improvement of functionality of sol-gel-derived silica glass thin films by tailoring their nanostructure at low heat-treatment temperature.

通过在低热处理温度下调整纳米结构来改善溶胶-凝胶衍生的二氧化硅玻璃薄膜的功能。

基本信息

批准号：
08555217
负责人：
KAMIYA Kanichi
金额：
$ 4.93万
依托单位：
Mie University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (A)
财政年份：
1996
资助国家：
日本
起止时间：
1996 至 1998
项目状态：
已结题

项目摘要

Establishment of technique to produce silica glass thin film coating on semiconductor, plastics and metal substrates at temperatures below 500ﾟC in low cost and without complicated processes is nowadays more and more strongly demanded.The sol-gel method has been developed for that purpose, but the heat-treatment at 600-800ﾟC is still required for transforming silica gel films to dense glass films, In the present study, we found through the examination of nano-structure change of the alkoxy-derived silica gels on heating by X-ray diffraction analysis method that 4-fold sioxane ring units are prevailing in the gels, and the heat-treatment at 600-800ﾟC is indispensable for changing gels to glasses. Then we invented the method by which silica gels consisting of 6-fold siloxane rings are obtainable. The glass coating films thus obtained, however, were still porous below 500ﾟC.Perhydropolysilazane (PHPS) gives dense silica glass coating film by the heat-treatment at 450ﾟC in the air. It was found in the present study that Si-H bonds remaining up to 450ﾟC make difficult the lowering of glassification temperature. Then novel PHPS from which Si-H bonds are easily removed on heating was synthesized to obtain silica glass films below 450ﾟC.However, the raw materials are still expensive.Finally we tried to combine above two methods. The combination, namely the preparation of silica glass coating by using the mixture of alkoxy-derived sioxane oligomers consisting of 6-fold rings and PHPS as raw materials in the ratio of 9 to 1 was found to be very prospective for making silica glass coatings below 450ﾟC in low cost and with ease.

如今，人们越来越强烈地需要建立在低于 500°C 的温度下、在半导体、塑料和金属基底上以低成本、无需复杂工艺生产二氧化硅玻璃薄膜涂层的技术。为此目的，开发了溶胶-凝胶法，但仍需要 600-800°C 的热处理才能将二氧化硅凝胶薄膜转变为致密的玻璃薄膜。在本研究中，我们通过研究发现通过X射线衍射分析方法观察烷氧基硅胶受热时纳米结构的变化，凝胶中普遍存在4重硅氧烷环单元，600-800℃的热处理是凝胶转变为玻璃所必需的。然后我们发明了获得由六重硅氧烷环组成的硅胶的方法。然而，如此获得的玻璃涂层膜在500℃以下仍然是多孔的。全氢聚硅氮烷(PHPS)通过在空气中450℃下的热处理得到致密的二氧化硅玻璃涂层膜。本研究发现，高达450℃时Si-H键的残留使得玻璃化温度难以降低。然后合成了新型PHPS，在加热时容易除去Si-H键，在450℃以下获得二氧化硅玻璃薄膜。但原材料仍然昂贵。最后我们尝试将上述两种方法结合起来。这种组合，即以六环烷氧基低聚物与PHPS按9:1的混合物为原料制备二氧化硅玻璃涂层，被发现对于低成本、容易地制备450℃以下的二氧化硅玻璃涂层是非常有前景的。