本研究利用中孔洞二氧化矽作為模板，以含浸法將金屬鹽與金氯酸填入孔道，藉由陰陽離子間電荷作用力，並使用氫氣還原，可製備出高含量金奈米結構於中孔洞二氧化矽。第一部分我們選擇不同種類的金屬鹽與金氯酸共含浸於SBA-15薄片，以X光粉末繞射、掃描式電子顯微鏡、穿透式電子顯微術與X光吸收光譜證實具高電荷密度的金屬陽離子 (例如：Fe3+、Ga3+等) 可協助金氯酸進入孔道內，且於氫氣反應後仍可侷限還原態金於孔洞內。此外，藉由調控帶正電金屬鹽與金氯酸之比例與含量，可製備出高含量且高分散的金奈米顆粒或金奈米棒於SBA-15薄片，改善以往合成金奈米結構於中孔洞二氧化矽時需引入表面特定官能基 (例如：胺基或巰基) 等步驟。第二部分我們使用相同製備法於不同結構與孔徑之中孔洞二氧化矽 (MCM-41、MMT-1與MCM-48)，研究此法的適用性，以及不同中孔洞材料所對應的金奈米顆粒之形貌與結構。

We utilized electrostatic interactions between metal salts and chloroauric acid to fabricate high gold loading nanostructure in mesoporous silica. In the first part of the thesis, we incorporated different kinds of metal salts and chloroauric acid into SBA-15 platelet via impregnation. We postulated that metal cations with high charge density (e.g. Fe3+, Ga3+ ) could confine chloroauric acid in the channel during hydrogen reduction, and prevent sintering of gold nanostructures. The idea is evidenced by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and X-ray absorption spectroscopy. Moreover, we could obtain high loading and high dispersion gold nanoparticles and gold nanorods in SBA-15 platelet by altering the ratio of metal salts to chloroauric acid or the quantity of metal species. This strategy is superior to the conventional one, which requires the modification of mesoporous silica with the specific functional group (e.g. –NH2, -SH) prior to loading gold precursor onto silica support. In the second part of the thesis, we extend this idea to mesoporous silica nanoparticles with different mesopore topologies (e.g. MCM-41, MMT-1, MCM-48).

謝誌 I
摘要 III
目錄 VI
圖目錄 IX
表目錄 XIII
第一章 緒論 1
1-1金奈米結構製備方法 1
1-1-1 直接合成法 2
1-1-2 模板合成法 4
1-2 金奈米結構性質與應用 7
1-2-1 表面電漿共振效應 8
1-2-2 奈米金觸媒 13
1-3 中孔洞二氧化矽材料簡介 15
1-4 研究動機 28
第二章 實驗部分 30
2-1 實驗藥品 30
2-2 樣品製備 32
2-2-1 中孔洞二氧化矽之製備 32
2-2-1-1 SBA-15 platelet的合成92 32
2-2-1-2 MCM-41及MMT-1的合成77 32
2-2-1-3 MCM-48的合成93 33
2-2-2 以中孔洞二氧化矽為模板製備金奈米結構 34
2-3 樣品命名 34
2-4 材料鑑定分析技術簡介 37
2-4-1 結構分析技術 37
2-4-1-1 X光粉末繞射 37
2-4-1-2 X光吸收光譜 40
2-4-2 成分分析技術 44
2-4-2-1 能量散射光譜 44
2-4-3 電子顯微術 46
2-4-3-1 掃描式電子顯微術 46
2-4-3-2 穿透式電子微術 47
2-4-4 氮氣物理吸附 48
第三章 結果與討論 54
3-1中孔洞二氧化矽之分析與鑑定 54
3-1-1 SBA-15 platelet 54
3-1-2 MCM-41 56
3-1-3 MMT-1 57
3-1-4 MCM-48 59
3-2 以 SBA-15 為模板製備之金奈米結構 61
3-2-1 金屬硝酸鹽種類的影響 61
3-2-2 鐵價數與陰離子種類的影響 67
3-2-3 X光吸收光譜鑑定 70
3-2-4 後處理方式的影響 77
3-2-5 金屬含量的影響 83
3-3 以 MCM-41 為模板製備之金奈米結構 89
3-4 以 MMT-1 為模板製備之金奈米結構 90
3-5 以 MCM-48 為模板製備之金奈米結構 91
第四章 結論及未來展望 93
第五章 參考文獻 94

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