臺灣博碩士論文加值系統

奈米材料與技術在綠色化學領域上有廣泛應用的前景，所以本篇論文，希望製備出一種具有磁學性質和催化性質的核殼型磁性奈米粒子。本研究先是利用化學還原法製備出具有羧基(-COOH)、羥基(-OH)的FePt 奈米粒子；再利用溶膠凝膠法在低溫下製備出正方晶相的ZrO2 奈米粒子；最後結合化學還原法和溶膠凝膠法利用FePt表面的官能基與非晶相Zr(OH)4形成氫鍵，經熱退火處理後，製備出FePt/ZrO2之核殼型式奈米粒子，最後使用硫酸對粒子表面做修飾。最後將這些樣品分別以X光繞射儀、穿透式電子顯微鏡、傅立葉轉換紅外線光譜儀、振動試樣磁力計、高週波加熱器等儀器鑑定並分析其性質，實驗結果顯示：以三乙二醇所製備出來的FePt奈米粒子因表面有-OH、-COO-M和-CO-M的官能基訊號，可使FePt奈米粒子可溶於有機溶劑和水溶液中，且具有較大的飽和磁化量，為26.12 emu/g；在低溫下，初製備的非晶相Zr(OH)4，隨熱退火溫度增加至800 ℃出現正方晶相，經硫酸改質後成功的製備出ZrO2/SO42-；最後發現添加不同C12H28O4Zr前驅物比例時，可發現其飽和磁化量隨之增加而遞減，該奈米粒子具有磁學性質，且表面擁有SO42-官能基，希望此核殼奈式米粒子在未來可應用於磁性固體酸式催化劑。

The recent development of nanostructured materials and nanotechnologies led them to have potential applications in green chemical engineering. In this study, we aim at synthesizing magnetic and catalytic nanoparticles with core-shell structure. FePt/ZrO2 core-shell structured nanoparticles were successfully prepared by chemical reduction and sol gel method using FePt nanoparticles with carboxyl (-COOH), hydroxyl (-OH) functional groups and Zr(OH)4 as precursors, followed by an annealing procedure to obtain tetragonal phase zirconia (t-ZrO2). Sulfuric acid was employed for the surface modification of as-prepared nanoparticles. X-ray diffraction (XRD), Raman spectroscopy, high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), vibration sample magnetometer (VSM), and high frequency heater were utilized to investigate the properties of the FePt/ZrO2 nanoparticles. FTIR analysis demonstrated that the FePt nanoparticles synthesizing from tetraethylene glycol, possessed high amphiphilic property due to –OH, -COO-M, and –CO-M functional groups, and high saturation magnetization of 26.12 emu/g. XRD and Raman spectroscopy revealed that t-ZrO2 could be obtained from Zr(OH)4 by annealing at 800 oC. Also, the surface modification using sulfuric acid was found to contribute in formation of ZrO2/SO42-. The results show that high concentration of C12H28O4Zr as zirconium precursor, could significantly reduce the saturation magnetization of as-prepared nanoparticles. All the results open up an avenue for the applications of FePt/ZrO2 in magnetic solid acid catalyst.

目 錄
摘 要 ....................................................................................................................... i
Abstract .....................................................................................................................ii
誌 謝 .................................................................................................................... iii
目 錄 ...............................................................................................................iv
表目錄 ...................................................vii
圖目錄 ...................................................viii
第一章 緒論 .......................................................................................................... 1
1.1 前言........................................................................................................................... 1
1.2 研究動機 ................................................................................................................... 2
1.3 研究目的與範圍 ....................................................................................................... 3
第二章 文獻回顧與理論 ...................................................................................... 4
2.1 奈米材料 ............................................................................................................. 4
2.2 奈米粒子的基本特性 ......................................................................................... 4
2.2.1表面效應 ............................................................................................................. 4
2.2.2 量子尺寸效應 .................................................................................................... 5
2.2.3 小尺寸效應 ........................................................................................................ 6
2.2.4 量子穿隧效應 .................................................................................................... 7
2.2.5. 庫倫堵塞效應 ................................................................................................... 9
2.2.6. 奈米粒子的製備 ............................................................................................... 9
2.3 FePt磁性奈米粒子的特性 .................................................................................. 11
2.4 FePt奈米粒子的製備 .......................................................................................... 13
2.5 FePt奈米粒子在生物醫學上的應用 ................................................................... 15
2.6 ZrO2奈米粒子的特性 .......................................................................................... 17
2.7 ZrO2奈米粒子的製備 .......................................................................................... 20
2.8 ZrO2奈米粒子在化學工業上的應用 .................................................................. 25
v
2.9 FePt核殼型奈米複合材料在生醫上及其他應用 ............................................... 26
第三章 實驗方法及步驟 .................................................................................... 29
3.1 製備親水親油相FePt奈米粒子 ............................................................................ 30
3.1.1 實驗藥品 .......................................................................................................... 31
3.1.2 實驗設置 .......................................................................................................... 31
3.1.3 實驗步驟 .......................................................................................................... 32
3.2 製備Tetragonal ZrO2奈米粒子 ............................................................................. 34
3.2.1 實驗藥品 .......................................................................................................... 34
3.2.2 實驗設置 .......................................................................................................... 35
3.2.3 實驗步驟 .......................................................................................................... 36
3.2.4 熱退火處理 ...................................................................................................... 37
3.2.5 表面改質處理 .................................................................................................. 37
3.3 製備FePt@ZrO2核殼奈米粒子 ............................................................................ 38
3.3.1 實驗藥品 .......................................................................................................... 39
3.3.2 實驗步驟 .......................................................................................................... 40
3.4 儀器介紹 ................................................................................................................. 41
3.4.1 X-ray繞射晶體結構分析儀 .......................................................................... 41
3.4.2 穿透式電子顯微鏡 .......................................................................................... 42
3.4.3 傅立葉轉換紅外線光譜儀 .............................................................................. 43
3.4.4 振動試樣磁力計 .............................................................................................. 44
3.4.5 拉曼光譜儀 ...................................................................................................... 45
3.4.6 高週波加熱器 .................................................................................................. 46
第四章 實驗結果與討論 ...................................................................................... 49
4.1 FePt奈米粒子的實驗結果與討論 ................................................................... 49
4.1.1 FePt奈米粒子的晶體結構分析 ....................................................................... 50
4.1.2 FePt奈米粒子的粒徑、形貌和成份分析 ....................................................... 53
4.1.3 FePt奈米粒子的表面性質分析 ....................................................................... 56
vi
4.1.4 FePt奈米粒子的磁學分析 ............................................................................... 58
4.1.5 FePt奈米粒子的磁流體熱療檢測 ................................................................... 59
4.2 FePt奈米粒子在不同條件下的熱退火效應 ................................................... 62
4.2.1 FePt奈米粒子在大氣條件下熱退火 ............................................................... 62
4.2.2 FePt奈米粒子在真空條件下熱退火 ............................................................... 66
4.3 ZrO2奈米粒子的實驗結果與討論 ................................................................... 71
4.3.1 ZrO2奈米粒子的晶體結構分析 ....................................................................... 71
4.3.2 ZrO2奈米粒子的粒徑、形貌及成份分析 ....................................................... 74
4.3.3ZrO2奈米粒子的表面性質分析 ........................................................................ 76
4.4 FePt@ZrO2奈米粒子的實驗結果與討論 ........................................................ 78
4.4.1 FePt@ZrO2奈米粒子的晶體結構分析 ............................................................ 78
4.4.2 FePt@ZrO2奈米粒子的粒徑、形貌分析 ........................................................ 80
4.4.3 FePt@ZrO2奈米粒子的磁性質分析 ................................................................ 83
4.4.4 FePt@ZrO2奈米粒子的磁流體熱療檢測 ........................................................ 86
第五章 結論 ........................................................................................................ 90
第六章 未來展望 ................................................................................................ 92
參考文獻 ................................................................................................................ 93

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