我們使用具有3D立體且互相連通孔道的中孔洞二氧化矽MCM-48當作模板，我們嘗試使用”初溼含浸法”來使金屬前驅物流入MCM-48的孔道內，經過高溫下氫氣的還原後，可以獲得Pd/MCM-48複合物，經過氫氟酸處理後，可得到鈀金屬的奈米線網路。
我們嘗試將中孔洞鈀奈米粒子應用在α-methylstyrene及p-bromoacetophenone當反應物的Heck反應上，我們發現了的確與文獻上的催化劑有不同的效果，且在反應結束後，E/Z的產物比例會發生改變，未來可以嘗試將中孔洞鈀奈米粒子應用在攜帶儲存小分子上面。
我們使用了TEM (穿透式電子顯微鏡)、SEM (掃描式電子顯微鏡)、XRD (X光繞射儀)及BET氮氣吸託付實驗來鑑定MCM-48、Pd/MCM-48及中孔洞鈀奈米粒子，另外也使用了NMR (核磁共振儀)及GC (氣相層析儀)來追蹤Heck反應進而與文獻所使用的催化劑去比較其催化效果。

In our study, 3D interconnection channels of mesoporous silica MCM-48 was used as template. We try to fill the channels with the metal precussor by “incipient wetness” technique. After the reduction with H2, the composites containning metal Pd and MCM-48 could be obtained. Then, Pd nanowire network was obtained through HF etching.
The mesoporous palladium nanoparticles are obtained and we try to use it as the catalyst in the Heck coupling reaction of α-methylstyrene and p-bromoacetophenone. We find that our catalyst have different effect in this Heck reaction. The terminal and internal (E/Z form) isomer ratio variated in the reaction. In the future, we will attempt to apply our mesoporous Palladium nanoparticles as organic molecule storage.
The MCM-48 and mesoporous Palladium nanoparticles were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution nitrogen adsorption.We used NMR and GC to trace the reaction. Heck reaction was performed as a test reaction to compare catalytic performances of the meosoporous Palladium nanoparticles and the catalyst of refrence.

目錄
謝誌
中文摘要
英文摘要
第一章
緒論
1-1
中孔洞氧化矽(mesoporous silica)材料簡介.........................................1
1-1-1
歷史...............................................................................................1
1-1-2
MCM-48簡介…………………………………………………...5
1-2
中孔洞氧化矽材料的應用.....................................................................8
1-2-1 中孔洞氧化矽當模板合成中孔洞碳材………………………….10
1-2-2 中孔洞氧化矽當模板合成奈米金屬…………………………….13
1-3
鈀的催化.................................................................................................23
1-3-1 Heck reaction.................................................................................24
1-3-2 Heck reaction之反應機構.............................................................27
1-3-3 Heck反應之文獻探討..................................................................29
1-4
實驗目標.................................................................................................30
第二章
實驗部份......................................................................................................31
2-1
藥品…………………………………………………………………….31
2-2
儀器與性質測量.....................................................................................33
2-2-1 解析型掃描穿透式電子顯微鏡(analytical scanning transmission
electron microscope，TEM)………………………………………………33
2-2-2 掃描式電子顯微鏡(Scanning Electron Microscope，SEM).........33
2-2-3 高解析度X光繞射儀(high resolution X-ray diffractometer).......34
2-2-4 氮氣等溫吸附/脫附測量(N2 adsorption/desorption isotherm).....34
2-2-5 X-射線單晶繞射儀 ( X-ray Diffractometer )..............................35
2-2-6 GC/MS，氣相層析質譜儀……………………………………...38
2-2-7 核磁共振光譜(NMR)測定………………………………………38
2-3
前驅物及中孔鈀奈米粒子的合成與Heck reaction…………………..39
2-3-1
MCM-48的合成……………………………………………… ..39
2-3-2
中孔洞鈀奈米粒子的合成……………………………………...40
2-3-3
將中孔洞鈀奈米粒子應用於Heck反應之催化……………….42
第三章
結果與討論..................................................................................................48
3-1
MCM-48的鑑定...................................................................................48
3-2
Pd/MCM-48複合物的鑑定..................................................................52
3-2-1
條件A的TEM圖討論...................................................................52
3-2-2
條件B的TEM圖討論…………………………………………...53
3-2-3
條件C的TEM圖討論…………………………………………..54
3-2-4
使用最佳化條件所作之Pd/MCM-48的性質鑑定……………...56
3-3
多孔鈀奈米粒子的TEM鑑定……………………………………….61
3-4
中孔洞鈀奈米粒子應用在Heck反應上…………………………….64
3-4-1
以4-bromoacetophenone及α-methylstyrene當反應物之反 應產物的鑑定……………………………………………………..65
3-4-2
多孔性Pd奈米粒子隨反應時間的變化…………………………77
3-4-3
1 mol%催化劑所作以4-bromoacetophenone與α-methylstyrene
當反應物之Heck reaction………………………………………...80
3-4-4
0.1 mol%催化劑所作4-bromoacetophenone與α-methylstyrene
反應之Heck reaction……………………………………………...82
3-4-5
純產物有加Pd與沒加Pd反應之變化…………………………..84
3-4-6
1 mol%催化劑所作以bromobenzene與α-methylstyrene
當反應物之Heck reaction………………………………………...86
3-4-7
催化效果比較……………………………………………………..88
第四
章 結論..............................................................................................................91
第五章
未來展望......................................................................................................92
第六章
參考文獻......................................................................................................93
第七章 附錄..............................................................................................................96

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