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.

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