本論文係有關金屬奈米粒子及核殼型複合奈米粒子之製備，前者主要在乙二醇系統和水相界面活性劑系統製備鎳及銅奈米粒子，探討製備變因及產品特性。後者在乙二醇系統中製備兼具有磁性及光學性質之鎳/金核殼型複合奈米粒子，並將其與藥物葉酸拮抗劑鍵結。
　　關於在乙二醇系統下製備鎳奈米粒子之研究，以聯胺為還原劑，在添加微量鹼的乙二醇溶液中，不需加入額外的惰性氣體及保護劑，即可製備出純鎳之金屬奈米粒子。由FTIR分析，得知乙二醇及其鎳催化分解產物在粒子表面形成保護層，可防止粒子的凝聚。由穿透式電子顯微鏡(TEM)、X射線繞射儀(XRD)、電子繞射、晶格影像、和超導量子干涉(SQUID)磁量儀分析得知，所得粒子為平均粒徑6~9nm、面心立方結構、且具超順磁特性之純鎳金屬奈米粒子。而隨著聯胺濃度的增加，粒徑隨著變小，當[N2H5OH]/[NiCl2]>20時，粒徑即維持不變。此外，所製得鎳奈米粒子對聯胺有催化分解成氫氣及氮氣的作用，在一大氣壓、25℃下其分解速率為3.1 nmol/h mg Ni。
　　關於在水相界面活性劑系統製備鎳奈米粒子之研究，以聯胺為還原劑，在添加微量鹼之CTAB水溶液中，不需通入額外的惰性氣體，即可製備出純鎳之金屬奈米粒子。由TGA分析，可推測CTAB以雙層結構被覆在鎳奈米粒子的表面，產生防止粒子凝聚的作用。由TEM、XRD、電子繞射、晶格影像、及SQUID磁量儀分析得知，所得粒子為平均粒徑10~14nm、面心立方結構、且具超順磁特性之純鎳金屬奈米粒子。而隨著聯胺濃度的增加，粒徑隨著變小，當[N2H5OH]/[NiCl2]> 20時，粒徑即維持不變。
　　關於在水相界面活性劑系統製備銅奈米粒子之研究，以聯胺為還原劑，並以氨水控制CTAB水溶液的pH值在10附近，不需通入額外的惰性氣體即可製備出純銅奈米粒子，銅離子濃度可高達0.2M。由TGA分析，可推測CTAB以雙層結構被覆在銅奈米粒子的表面，產生防止粒子凝聚的作用。由TEM、XRD、電子繞射、紫外光-可見光光譜、及化學分析電子光譜 (XPS)分析得知，所得粒子為平均粒徑5~15nm、面心立方結構之純銅金屬奈米粒子。而隨著聯胺濃度的增加，粒徑隨著變小，當[N2H5OH]/[NiCl2]> 40時，粒徑即維持不變。
　　關於在乙二醇系統中製備鎳/金核殼型複合奈米粒子及其與葉酸拮抗劑共價鍵結之研究，發現在無保護劑存在下，所製得之鎳/金核殼型複合奈米粒子有凝聚現象，但在有保護劑聚乙醯胺(PEI)存在下，即可製備出平均粒徑14.6nm、兼具磁性及光學性質、且分散均勻之鎳/金核殼型複合奈米粒子。XRD及電子繞射分析顯示所得之鎳/金核殼型複合奈米粒子為面心立方體結構。又鎳/金核殼型複合奈米粒子經表面修飾後，可與葉酸拮抗劑共價鍵結，平均一個鎳/金核殼型複合奈米粒子可鍵結高達3.63×104個葉酸拮抗劑分子。

　　This dissertation concerns the preparation of metal nanoparticles and core-shell composite nanoparticles. In the former, nickel and copper nanoparticles have been prepared in ethylene glycol and aqueous surfactant systems. The preparation conditions and product properties were investigated. In the latter, Ni@Au core-shell composites nanoparticles were prepared in ethylene glycol system and covalently bound with methotrexate (MTX).
　　In ethylene glycol system containing trace bases, Ni nanoparticles could be prepared by hydrazine reduction without the input of extra inert gases and the addition of protective agent. FTIR analysis revealed the formation of a protective layer from ethylene glycol and the Ni-catalyzed decomposition products, which prevented from the agglomeration of particles. The TEM, high-resolution TEM, XRD, electron diffraction pattern, magnetic analyses indicated the resultant particles were pure Ni nanoparticles with the mean diameter of 6-9 nm, fcc structure, and superparamagnetic property. With increasing N2H5OH concentration, The mean diameter decreased and approached a constant when [N2H5OH]/[NiCl2]>20. In addition, hydrazine was catalytically decomposed to hydrogen and nitrogen gases by the resultant Ni nanoparticles. The decomposition rate was 3.1 nmol/h mg Ni at 1 atm and 25℃.
　　In a pure aqueous CTAB solution containing trace bases, Ni nanoparticles could be prepared by hydrazine reduction without the input of extra inert gases. the synthesis of nickel nanoparticles without inert gases was studied. TGA study suggested the formation of a bi-layer structure on particle surface, which prevented from the agglomeration of particles. The TEM, high-resolution TEM, XRD, electron diffraction pattern, magnetic analyses indicated the resultant particles were pure Ni nanoparticles with mean diameters of 10-14 nm, fcc structure, and a superparamagnetic property. With increasing N2H5OH concentration, the mean diameter decreased and approached a constant when [N2H5OH]/[NiCl2]>20.
　　In a pure aqueous CTAB solution, Cu nanoparticles could be prepared by hydrazine reduction without the input of extra inert gases. The key point was the use of ammonia solution to adjust the solution pH up to 10. The concentration of Cu2+ ions allowable was as high as 0.2 M. TGA study suggested the formation of a bi-layer structure on particle surface, which prevented from the agglomeration of particles. The TEM, XRD, electron diffraction pattern, UV-VIS spectrum, and XPS analyses indicated the resultant particles were pure Cu nanoparticles with mean diameter of 5-15 nm and fcc structure. With increasing N2H5OH concentration, the mean diameter decreased and approached a constant when [N2H5OH]/[NiCl2]>40.
　　In ethylene glycol, Ni@Au core-shell composites nanoparticles were prepared. In the absence of protective agent, particle agglomeration was observed. In the presence of polyethyleneimine (PEI) as a protective agent, monodisperse Ni@Au composite nanoparticles with a mean diameter of 14.6 nm were obtained. After surface modification, Ni@Au composite nanoparticles were covalently bound with methotrexate (MTX). Averagely 3.63×104 MTX molecules could be bound on each Ni@Au composite nanoparticle.

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