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研究生： 林長弘
Lin, Chang-Hung
論文名稱： 利用溶膠凝膠法製備摻雜氧化錫薄膜與氫氣感測特性之研究
Growth and Characterization of Pure and Doped SnO2 Films for H2 Gas Detection
指導教授： 齊孝定
Qi, Xiao-Ding
共同指導教授: 李世欽
Lee, Shih-Chin
學位類別： 碩士
Master
系所名稱： 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年： 2011
畢業學年度： 99
語文別： 中文
論文頁數： 100
中文關鍵詞： 溶膠凝膠法 、二氧化錫 、氣體感測 、氫氣
外文關鍵詞： sol-gel, tin oxide, gas sensor, H2
相關次數： 點閱：81  下載：3 
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    • 本實驗利用溶膠凝膠法(sol-gel)製備SnO2以及SnO2:M, M=Pd, Mn, W, Y。摻雜後，對此些混合金屬氧化物材料的表徵和化學成分進行了廣泛的特性分析，摻雜後晶粒變為比未摻雜之二氧化錫小，同樣的SEM觀察到的叢集物也相對變小，相對比表面積增加，有利於氣體感測應用。
    實驗結果針對不同摻雜與純氧化錫薄膜對於氣體偵測500 ppm氫氣做比較，純氧化錫有最高靈敏度時的最佳溫度是250 ℃，氣體敏感因子S=3.9，回復時間t=84 sec，相對的以250 ℃為操作溫度，摻雜5 at%W的薄膜對500 ppm氫氣擁有最高的靈敏度S=25.8，其回復時間亦有所減短(t=72 sec)。摻雜5 at%Pd的薄膜具備最短的回復時間(t=60sec)，但靈敏度僅少許改善S=4.4，而錳摻雜之氧化錫不但氣體靈敏性低，並且熱穩定性也不佳。實驗最後發現摻雜5 at%W及5 at%Y氧化錫薄膜在50~500 ppm氫氣間的靈敏度對氫氣濃度有良好的正比線性關係，可用於定量測量。在50 ppm氫氣情形下，5 at%W-SnO2薄膜仍有高達S=3.35的靈敏度。

    Pure and doped SnO2:M (M=Pd, Mn, W,Y) films were prepared by the sol-gel method. The surface morphology and microstructure of the grown films were characterized by a wide range of techniques. Generally, various doping resulted in a reduction of the grain size, as well as a smaller size of various surface features.
    The films were tested for the gas sensing applications. In the 500 ppm H2 gas, the optimum operating temperature for the pure SnO2 films was 250 oC, which showed a sensitivity of S=3.9 and a recovery time of 84 s. Doping of 5 at% W increased the sensitivity significantly (S=25.8) at the same operating temperature, while the recovery time was reduced to 72 s. For the 5 at% Pd doped SnO2 films, the sensitivity was only slightly improved (S=4.4), however they showed the quickest recovery time of 60 s. Doping of Mn did not improve the H2 sensing sensitivity and the doped films showed a poor thermal stability at the elevated temperatures. The sensitivity of 5 at% W and 5 at%Y doped SnO2 in 50-500 ppm H2 showed a linear increase with the gas concentration and therefore, they can be used for the quantitative sensing. In the 50 ppm H2 gas, 5 at% W doped SnO2 films still showed a fairly good sensitivity of S=3.35.

    摘要 I Abstract II 誌謝 IV 總目錄 VI 圖目錄 IX 表目錄 XIV 第一章 緒論 1 1-1研究背景 1 1-2研究動機與目的 3 第二章 文獻回顧 6 2-1二氧化錫結構與特性 6 2-2溶膠凝膠法基礎理論 8 2-3旋轉塗佈法的原理 11 2-4二氧化錫之氣體偵測性及其應用 13 2-5氣體偵測器工作原理 14 2-5-1氣體之吸附機制 14 2-5-2二氧化錫對氣體偵測原理 16 2-6 催化劑在金屬氧化物中的作用 19 2-7 儀器原理 21 2-7- 1掃瞄式電子顯微鏡原理 21 2-7-2 X光能量散佈分析儀原理 22 2-7-3低掠角X光繞射儀原理 23 2-7-4歐傑電子能譜儀原理 25 第三章 實驗方法及步驟 37 3-1實驗流程 37 3-2實驗藥品及儀器 38 3-3基材前處理與薄膜的製備 40 3-3-1基材前處理 40 3-3-2溶膠凝膠的配製 40 3-3-3旋轉塗佈法 41 3-3-4退火熱處理 42 3-4薄膜性質量測 43 3-4-1表面形貌及成分分析 43 3-4-2晶體結構分析 43 3-5氣體偵測性質分析 45 3-5-1 氣體偵測系統 45 3-5-2 氣體偵測試片製備 45 3-5-3 氣體偵測能力分析流程 45 第四章 結果與討論 50 4-1 SnO2試片表面分析 50 4-1-1 SnO2薄膜SEM斷面分析 50 4-1-2表面形貌分析 50 4-1-3 EDS表面成分分析 52 4-1-4 AES表面成分分析 52 4-1-5 X-ray繞射分析 53 4-2薄膜氣體感測性質分析 56 4-2-1二氧化錫薄膜在不同溫度之氫氣靈敏度 56 4-2-2摻雜對二氧化錫薄膜氫氣靈敏度及回復時間之影響 57 4-2-3摻雜後薄膜對低濃度氫氣之靈敏度 59 第五章 結論 92 參考文獻 93

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