以TEOS/乙醇/水三成份溶膠凝膠系統製備氧化矽薄膜

Silica Film Formation via TEOS/Ethanol/Water Tri-component Sol-Gel System

廖振生(Chen-Sheng Liao)

指導教授 ： 張幼珍

元智大學/工程學院/化學工程與材料科學學系/碩士(2008年)

摘要

本研究使用溶膠凝膠法評估成膜的可行性，系統為三成份系統的勻相系統(去離子水、四乙基矽酸鹽(Tetra Ethyl Ortho Silicate)、乙醇)加上催化劑(鹽酸或氨水)調整水的pH值，經過一定程度的水解與縮合後，塗佈於玻璃基板上，觀察酸鹼條件下，不同催化劑濃度以及不同水矽比(Water/Silicon ratio)成膜的可能性，同時分別以SEM以及FTIR觀察長時間下系統巨觀及微觀的變化，
實驗結果顯示，調整pH的去離子水在低pH值條件下以及水矽比1~4時，是可成膜的配方，在高水矽比的條件下則無法塗佈成膜。實驗結果驗證文獻的論述，即不同pH值(催化劑濃度)以及不同水矽比有不同的微觀縮合產物，而不同的微觀縮合產物將影響成膜的可能性。在去離子水pH2、水矽比1的條件下，FTIR分析結果驗證線性物質與環狀物質的存在，線性物質因形成環狀物質而逐漸減少。在高pH值水矽比逐漸增加的條件下，膜層表面微粒有增加的趨勢，與Stober method結果相符。最後實驗結果顯示，中間pH值的條件下可得到類似的膜層形貌和FTIR光譜。

關鍵字

TEOS ； 水解 ； 縮合 ； FTIR

並列摘要

This study employed the sol-gel method to evaluate film formation feasibility of the TEOS/ethanol/water tri-component system. The pH of water was adjusted by HCl or NH4OH. After the precursor (TEOS) was hydrolyzed and condensed to a certain extent, the formulation was applied onto glass substrate. The feasibility of film formation under acid and base condition with different water/silicon ratio was investigated. After the applied coating was dried, SEM was used to observe the morphology of surface of the glass substrate before and after curing. Besides, FTIR was used to observe the microscopic change of each liquid formulation for a period of time.
The result showed that the recipe was applicable under low pH value with the ratio of water/silicon ranging from 1 to 4. At high ratio of water/silicon, the formulation cannot spread out on the substrate. At high ratio of water/silicon, the recipe can not be applied. The FTIR results confirmed that different concentration of catalyst and water/silicon ratio resulted in different condensation product. Different condensation products affects the feasibility of film formation for each recipe. Under condition of pH2 and r=1, FTIR result indicated the existence of linear and cyclic species. Linear species were diminished due to their gradual cyclization into cyclic species with time. At high pH value, increasing water/silicon ratio, r, resulted in particle-based films. Finally, at intermediate pH value ranging from 4 to 7, FTIR results showed similar spectra, while the SEM result also showed similar film surface morphology.

並列關鍵字

TEOS ； hydrolysis ； condensation ； FTIR

參考文獻

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