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標題: 前驅物植入方式合成中空ZnO暨中空Pt-Fe2O3複合殼層微球之研究
Synthesis of ZnO and Pt-Fe2O3 composite particles with hollow interiors by precursors implantation
作者: 郭旻鑫
Kuo, Min-Hsin
關鍵字: zinc oxide;氧化鋅;iron oxide;platinum;hollow sphere;氧化鐵;白金;空心球
出版社: 材料科學與工程學系所
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A facile process has been developed to fabricate hollow spheres with nanoporous shell structure. The process used metal chloride as a precursor and polymeric hard template as the starting materials, together with tetrachloroethylene (C2Cl4) as a solvent. The hollow spheres were obtained after removal of the polymeric template by thermal pyrolysis. The process involves implantation of the precursor into the template surface to become a core-shell structure, different from those reported in the literature. In this work, the experiment was divided into two parts. First, we prepared ZnO hollow spheres, proposed a model to explain the implantation mechanism, and examined effect of calcinations temperature on hollow structure. Second, Pt/Fe2O3 composite hollow spheres were synthesized. Effect of Pt loading on microstructure of the composite particles was examined

In the first part, ZnCl2 was used as the precursor. From ESCA/Auger depth analysis, Zn species penetrated to template surface for the implantation process. FTIR observed that -CH=CH2 absorption intensity becomes stronger but =CH2 absorption intensity gets weaker after the implantation. We inferred that the implantation maybe caused by tetrachloroethylene decomposition and Zn precursor recomposed to replace the original organic group on template surface. We also found that calcination temperature plays an important factor in synthesis of the hollow sphere shell. TG/DSC showed the template removal process. From SEM/TEM examination, the ZnO shell crystallized before the template had vanished, although high temperature seemed helpful to template core pyrolysis and formation of hollow spheres shell atructure. As temperature raised further to 700 oC would help the core removal, the spheres shell would collapse.

In the second section, we chose FeCl3 and H2PtCl6 as the precursor for the synthesis of Pt/Fe2O3 composite hollow spheres. The H2PtCl6 concentration was adjusted in order to study the effect of Pt loading on shell structure of the composite hollow spheres. From ICP-MS analysis, we found out that the precursors would compete for the implantation. FE-SEM, TEM, BET were also used to analyze the different Pt loadings on the composite hollow spheres. XRD revealed that the Fe2O3 grain size and crystallinity decrease as the Pt loading increased. Finally, composite hollow spheres with different Pt loadings were prepared into electrorheological fluids and subjected to alternating magnetic field. Result revealed that heat transform efficiency descended when the composite hollow spheres with a higher Pt loading.
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