臺灣博碩士論文加值系統

本論文在水相溶液系統中，利用共沈澱法在不同Fe2+與Fe3+濃度比與添加不同界面活性劑濃度下，製備鐵氧化物，將鐵氧化物分散於溶液中，再利用還原法將Au製備至鐵氧化物上。文中利用XRD分析其晶粒大小、AEM觀察其顆粒大小、氧化還原滴定分析鐵氧化物中Fe2+的含量、AAS分析核殼式奈米粒子的組成比例，並利用SQUID測量其磁性質。在本文中亦探討製備所得之鐵氧化物與鐵氧化物@金奈米粒子之磁熱效應。
在不同莫耳濃度比(Fe2+/Fe3+)下所製備之鐵氧化物，其粒徑大小隨著比值下降而減小，所獲得顆粒的型態與大小皆不均勻。當Fe2+ / Fe3+濃度比為2 M / 1 M、1 M / 2 M與1 M / 2.5M時，其平均粒徑分別為26、17與15 nm。而當添加固定濃度之界面活性劑SB12 (N-dodecyl-N,N-dimethyl-3-ammonio-1-propane-sulfonate)時，在反應物Fe2+與Fe3+總濃度較低時，製備所得之顆粒大小及其型態受界面活性劑的影響較大，當Fe2+與Fe3+之濃度控制在0.5 M與0.25 M，製備所得之鐵氧化物顆粒大小，隨界面活性劑之濃度SB12由1.656增加至6.620 mM時，其粒徑分別由17 nm降為13 nm。製備所得之鐵氧化物的飽和磁化量隨粒徑減小而下降。在水相中，當鐵氧化物與黃金的莫耳比為1/1、1/2與1/3時，製備所得之鐵氧化物＠金顆粒大小分佈為11-30, 12-30 與 15-40 nm。鐵氧化物＠金奈米粒子的飽和磁化量較鐵氧化物低。
利用Fe2+與Fe3+之濃度比為1 M：2 M製備所得之鐵氧化物進行磁熱效應分析，由結果發現磁熱效應之溫度上升量與磁場強度、頻率以及磁性物質之含量皆成正比關係。改變反應前驅物的濃度比例(Fe2+/Fe3+)1 M / 2 M、1 M / 2.5 M與1M / 3 M製備所得之鐵氧化物，其飽和磁化量分別為68.5、49.68與16.11 emu g-1，磁熱效應中施加65 Hz及電壓150 V所獲得之溫度上升量為1.1、0.85與0.6 ℃，其溫度上升量隨所獲得之飽和磁化量上升而增加。核殼式鐵氧化物＠金奈米粒子，在磁熱效應中溫度上升量隨著Au前驅物濃度增加而遞減，其原因為其飽和磁化量與磁滯區面積減小。

The iron oxides nano-particles were prepared by using the coprecipitation with various Fe2+/Fe3+ ratios, the kinds and concentrations of surfactants. Then, the iron oxides@Au nano-particles were prepared by the reduction of Au3+ on the iron oxides. The grain size, particle size, surface morphology, compositions of iron oxides and iron oxides@Au nano-particles were analyzed by XRD, AEM, FE-SEM, oxidation/reduction titration, and AAS, respectively. The magnetic properties of iron oxides were measured by SQUID. The magneto-caloric effect of the iron oxides and iron oxides@Au nanoparticles were also investigated in this thesis.
The particle sizes of iron oxides with non-uniform morphology and size distribution decreased by the decrease in the molar ratio of Fe2+/Fe3+. The average particle sizes of iron oxides were obtained to be 26, 17, and 15 nm for Fe2+/Fe3+ ratio of 2M/1M, 1M/2M, and 1M/2.5M, respectively. The morphology and particle size was affected by surfactant at a relative lower concentration of Fe2+ and Fe3+. The particle size of iron oxides decreased from 17 to 13 nm with increasing the concentration of SB12 (N-dodecyl-N,N-dimethyl-3-ammonio-1-propane-sulfonate) surfactant from 1.656 to 6.62 mM for preparing iron oxides at the Fe2+/Fe3+ ratio of 0.5M/0.25M. The saturation magnetization of iron oxides decreased with decreasing the particle size. The particle sizes of iron oxides@Au prepared in the aqueous solution were obtained to be 11-30, 12-30 and 15-40 nm for the iron oxides/Au molar ratios of 1/1, 1/2 and 1/3, respectively. The saturation magnetization of iron oxides@Au was lower than that of iron oxides.
The increase in the temperature was increased with the strength and frequency of applied magnetic field, and the amount of magnetic material in the magneto-caloric effect analysis. The saturation magnetization and the increase in the temperature in the magneto-caloric analysis were found to be 68.5, 49.68 and 16.11 emu g-1 , and 1.1, 0.85 and 0.6 oC for the iron oxides prepared at the Fe2+/Fe3+ ration of 1M/2M, 1M/2.5M, 1M/3M, respectively. The increase in the temperature of iron oxides@Au nano-paritcles in the magneto-caloric analysis decreased with increasing Au precursor for preparation due to the decrease in the saturation magnetization and the magnetic hysteresis area.

中文摘要 III
英文摘要 V
誌謝 VII
目錄 IX
表目錄 XIV
圖目錄 XVII
第一章 緒論 1
1-1 奈米材料與奈米科技之簡介 1
1-1-1 奈米材料之特性 2
1-1-1-1 量子尺寸效應 2
1-1-1-2 小尺寸效應 2
1-1-1-3 表面效應 4
1-1-2 奈米粒子之製備與應用 7
1-2 磁性理論之簡介 16
1-2-1 磁性單位 16
1-2-2 磁性的種類 16
1-2-3 磁滯曲線(hysteresis loop) 24
1-3 磁性奈米材料 27
1-3-1 磁性奈米材料鐵氧化物之製備與性質 32
1-3-2 磁性奈米材料應用 40
1-4 核殼式奈米粒子之製備與應用 44
1-5 研究動機與目的 61
第二章 實驗設備與程序 66
2-1 實驗儀器 66
2-2 實驗藥品 68
2-3 實驗程序 70
2-3-1 鐵氧化物之奈米顆粒製備 70
2-3-2 鐵氧化物＠Au奈米複合材料之製備 72
2-4 奈米顆粒及複合材料之鑑定與分析 73
2-4-1 XRD晶相分析 73
2-4-2 AEM分析 73
2-4-3 FE-SEM分析 74
2-4-4 組成分析 74
2-4-4-1 氧化還原滴定 74
2-4-4-2 AAS分析 76
2-4-5 磁性測量 76
2-4-5-1 SQUID分析 76
2-4-6 磁熱效應之量測 76
第三章 結果與討論 80
3-1 鐵氧化物奈米顆粒之性質分析 80
3-1-1 AEM、SEM鑑定分析 80
3-1-1-1 未添加界面活性劑之鐵氧化物奈米粒子 80
3-1-1-2 添加界面活性劑之鐵氧化物奈米粒子 91
3-1-1-2-1 微胞的形成 91
3-1-1-2-2 兩性離子型界面活性劑SB12的影響 93
3-1-1-2-3 陽離子型之界面活性劑CTAB的影響 109
3-1-2 製備所得鐵氧化物的晶相分析 116
3-1-2-1 未添加界面活性劑下，Fe2+與Fe3+濃度比之影響 117
3-1-2-2 界面活性劑SB12濃度之影響 120
3-1-2-3 界面活性劑CTAB濃度之影響 128
3-1-3 製備所得鐵氧化物之組成分析 132
3-1-3-1 界面活性劑不存在下製備所得鐵氧化物奈米粒子組成分析 133
3-1-3-2 兩性離子型界面活性劑SB12添加濃度對鐵氧化物組成之影響 137
3-1-3-3 陽離子型界面活性劑CTAB添加濃度對鐵氧化物組成之影響 139
3-1-4 製備所得鐵氧化物之磁性質量測 143
3-1-4-1 未添加界面活性劑所製備之鐵氧化物磁性質分析 143
3-1-4-2 添加界面活性劑所製備之鐵氧化物之磁性質分析 153
3-2 鐵氧化物@Au奈米粒子之性質分析 157
3-2-1 AEM鑑定分析 157
3-2-2 晶相分析 164
3-2-3 組成分析 169
3-2-4 磁性質之量測 170
3-3 鐵氧化物及鐵氧化物@Au奈米粒子之磁熱效應 174
3-3-1 鐵氧化物重量與水體積比的影響 174
3-3-2 磁場強度之影響 178
3-3-3 頻率的影響 181
3-3-4 不同製備條件所得之鐵氧化物及鐵氧化物@Au奈米粒子之磁熱效應及其影響因素 183
3-4 綜合討論 194
3-4-1 鐵氧化物之反應途徑 194
3-4-2 不同製備條件對鐵氧化物顆粒大小與型態之影響 197
3-4-3 添加界面活性劑對鐵氧化物的顆粒大小與型態影響之機制 202
3-4-4 磁性奈米粒子之磁性質與磁熱效應 208
第四章 結論與建議 212
參考文獻 216

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