本論文以微波輔助非水溶液合成法合成二氧化錫及貴金屬鈀修飾二氧化錫奈米材料，並應用於一氧化碳氣體感測。在合成過程中，我們探討合成溶劑與添加物對合成反應速率與晶面配位的影響，嘗試調控二氧化錫晶粒大小與形貌；此外，添加貴金屬鈀前驅物，微波合成貴金屬鈀修飾二氧化錫奈米材料。進一步以PXRD、SEM/TEM以及ICP-OES分析合成的奈米材料結構、晶粒大小與成分組成比例，以XPS、NMR分析奈米材料元素狀態與副產物組成，探討其合成機制。以苯甲醇作為溶劑與氧源能合成高產率與均勻晶粒大小的二氧化錫奈米材料。而以二次微波合成貴金屬鈀修飾二氧化錫奈米材料對於二氧化錫結構與晶粒大小無影響，隨著鈀含量的提高至2 wt%時會產生較大粒徑鈀。在一氧化碳氣體感測應用研究中我們發現在相同工作溫度下，鈀修飾二氧化錫之反應性明顯優於純二氧化錫奈米材料，且具有較低的工作溫度，以1 wt%鈀修飾二氧化錫具有最佳感測效果。在長時間壽命實驗中，發現鈀修飾二氧化錫奈米材料氣體感測反應性會受環境水氣影響，但在熱處理後能回復氣體感測反應性。

In the thesis, tin oxide and palladium decorated tin oxide nanocrystals were synthesized by microwave-assisted non-aqueous synthetic method and applied in carbon monoxide gas sensing. Different solvents and capping agents were used to control the morphology of the tin oxide nanostructures, and palladium decorated tin oxide nanostructures were prepared with addition of the palladium precursor in the microwave synthetic process. The obtained materials were characterized by PXRD, electron microscopy, ICP-OES, XPS and 13C-NMR for analysis of material structure and reaction mechanism. The analytical results indicated that tin oxide nanostructures were successfully synthesized in benzyl alcohol with high yield and uniform crystal sizes；however, capping agents might affect the synthesis of tin oxide and limit the growth of tin oxide nanostructures. For palladium decorated tin oxide nanostructures, the addition of palladium did not affect the size and morphology of tin oxide nanostructures. As the palladium ratio increased to 2 wt%, palladium with large particle size formed. Results of carbon monoxide gas sensing indicated that palladium decorated tin oxide nanostructures showed better response than tin oxide nanostructures at the same working temperature. In addition, palladium decorated tin oxide nanostructures also showed long-term stability at lower working temperature. For long-term stability test, sensing response of palladium decorated tin oxide decreaseed because of the influence of humidity. After heat treatment, the sensing response could be recovered.

第一章 緒論 1
1-1 危害氣體感測與環境安全 1
1-2 金屬氧化物半導體型氣體感測器 5
1-2-1 半導體型氣體感測器感測原理 6
1-2-2 二氧化錫材料特性 9
1-3 優化氣體感測因素與機制 11
1-3-1 感測材料形貌與顆粒大小 11
1-3-2 附載催化金屬 18
1-4 感測材料合成與製備 20
1-4-1 濺鍍法 20
1-4-2 化學氣相層積法 21
1-4-3 水熱法 22
1-4-4 非水溶液合成法 23
1-4-5 微波合成化學 29
1-5 研究動機 32
第二章 實驗部分 34
2-1 實驗藥品 34
2-2 感測材料合成 34
2-2-1合成二氧化錫奈米材料 35
2-2-1-1 合成二氧化錫奈米材料 35
2-2-1-2 溶劑對二氧化錫奈米材料合成影響 36
2-2-1-3 添加物對二氧化錫奈米材料合成影響 37
2-2-2 貴金屬修飾二氧化錫奈米材料合成 38
2-2-2-1 一次微波合成鈀修飾二氧化錫奈米材料 38
2-2-2-2 二次微波合成鈀修飾二氧化錫奈米材料 39
2-3 一氧化碳氣體感測實驗 41
2-3-1感測晶片製備 41
2-3-1-1 感測晶片規格與感測電路設計 41
2-3-1-2 晶片製備與前處理 43
2-3-2 一氧化碳氣體感測 43
2-3-2-1 感測系統設計 43
2-3-2-2 氣體感測流程 45
2-4 實驗鑑定與儀器 46
2-4-1 X光粉末繞射儀 46
2-4-2 掃描式電子顯微鏡 47
2-4-3 穿透式電子顯微鏡 49
2-4-4 X光光電子能譜 51
2-4-5 氮氣物理吸脫附 52
2-4-6 核磁共振光譜 59
2-4-7 感應耦合電漿放射光譜儀 60
第三章 結果與討論 62
3-1 感測材料合成與鑑定 62
3-1-1 合成二氧化錫奈米材料 62
3-1-1-1 溶劑影響 70
3-1-1-2 添加物影響 72
3-1-2 合成貴金屬修飾二氧化錫奈米材料 77
3-2 一氧化碳氣體感測結果 87
3-2-1 不同工作溫度對一氧化碳感測反應性比較 87
3-2-2 不同感測材料濃度對一氧化碳感測反應性比較 93
3-2-3 不同含量鈀修飾二氧化錫對一氧化碳感測反應性比較 97
3-2-5 感測晶片壽命測試 98
3-2-6 附件 102
第四章 結論 110
第五章 參考文獻 112

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