臺灣博碩士論文加值系統

本論文主要是以Stöber 法，先將二氧化矽包覆鐵氧化物以製備核殼結構之二氧化矽/鐵氧化物(SiO2/γ-Fe2O3)奈米複材，再以苯胺為單體利用原位聚合反應，合成具電磁特性之多層核殼型聚苯胺/二氧化矽包覆鐵氧化物(PANI/SiO2/γ-Fe2O3)奈米複材，同時藉由傅氏紅外線光譜儀、紫外光/可見光吸收光譜儀、廣角X-光繞射儀、穿透式電子顯微鏡、X-光電子光譜儀、阻抗分析儀、兩點式微歐姆計與超導量子干涉磁量儀等，系統化探討組成、結構與形態對核殼型SiO2/γ-Fe2O3 及多層核殼型PANI/SiO2/γ-Fe2O3 奈米複材導電與磁學特性之影響及其相互間關係。 結果顯示，利用化學共沉澱法可合成具奈米尺寸的磁赤鐵礦(γ-Fe2O3)，當γ-Fe2O3/四乙基矽氧烷(TEOS)重量比小於0.55時，可製備以γ-Fe2O3 為核，二氧化矽為殼之核殼型SiO2/γ-Fe2O3 奈米複材，其二氧化矽殼層厚度隨TEOS 添加量的增加而增加；PANI/SiO2/γ-Fe2O3 奈米複材之PANI包覆層則隨二氧化矽殼層厚度的增加而呈局部包覆形態。 磁量儀結果顯示，γ-Fe2O3、核殼型SiO2/γ-Fe2O3 及多層核殼型PANI/SiO2/γ-Fe2O3 奈米複材均具超順磁特性。 核殼型SiO2/γ-Fe2O3 奈米複材之導磁係數與飽和磁化量隨TEOS 添加量的增加而降低；多層核殼型PANI/SiO2 /γ-Fe2O3 奈米複材則隨二氧化矽殼層厚度的增加而降低。 於不同二氧化矽殼層厚度(10~55 nm)下，多層核殼型PANI/SiO2/γ-Fe2O3 奈米複材之摻雜程度隨二氧化矽殼層厚度的增加而降低，導致複材之導電度因而下降；當SiO2/γ-Fe2O3 奈米複材添加量從0.3 g 減少至0.1 g 時，多層核殼型複材之導電度將提昇至10-1 S/cm。

The purpose of this article is to carry out studies on synthesis and characterization of the multilayered polyaniline/silica-coated iron oxide nanocomposites. Two synthesis steps are involved in this work, first is about the preparation of core-shell silica-coated iron oxide nanoparticles. The core-shell structured nanoparticles can be prepared through the well known Stöber process. Second is concerning about the synthesis of multilayered core-shell structure of polyaniline/silica-coated iron oxide nanocomposites by in-situ polymerizing polyaniline on the surface of core-shell structured nanoparticles. As a result, a novel material comprising both leads magnetic and electric conductivity can be obtained. The structure, morphology and properties of samples are characterized by Fourier transform spectrometer (FT-IR), Ultraviolet-Visible spectroscopy (UV-Vis), wide angle X-ray diffraction (WAXD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), microhmeter, and superconductor quantum interference device (SQUID). The results showed that, as the weight ratio of γ-Fe2O3/TEOS is less than 0.55, the silica-coated maghemite (SiO2/γ-Fe2O3) particles with well-defined a core-shell structure can be conveniently prepared. Furthermore, the thickness of silica coating on the surface of γ-Fe2O3 nanoparticles increases gradually with increasing the TEOS content. For the room-temperature SQUID analysis, the magnetic properties of SiO2/γ-Fe2O3 nanocomposites are mainly dominated by γ-Fe2O3, and all SiO2/γ-Fe2O3 nanocomposites show superparamagnetic behavior. In addition, the saturation magnetization of the synthesized SiO2/γ-Fe2O3 nanocomposites decreases dramatically upon the increase of silica layer thickness. The magnetic properties and superparamagnetic behavior of multilayered core-shell PANI/SiO2/γ-Fe2O3 nanocomposites are found to be the same as the described above. As for microhmeter measurements, revealing the conductivity of nanocomposites increase with increasing the thickness of silica layer. As the amount of SiO2/γ-Fe2O3 nanocomposites is decreased, the doping level and the conductivity of multilayered core-shell PANI/SiO2/γ-Fe2O3 nanocomposites are significantly increased.

中文摘要……………………………………………………І
英文摘要……………………………………………………И
致謝…………………………………………………………Ш
目錄…………………………………………………………IV
表目錄.....................................Ⅵ
圖目錄.....................................Ⅶ
第一章 緒論....................................................1
1-1前言.......................................................1
1-2研究動機....................................................2
第二章 文獻回顧.................................................3
2-1 導電高分子...................................................3
2-1-1 聚苯胺簡介..............................................................6
2-1-2 聚苯胺之合成機構..............................................................8
2-1-3 聚苯胺之摻雜.............................................................11
2-1-4 聚苯胺的導電機構.............................................................13
2-2 鐵氧體.............................................................14
2-2-1 軟磁材料.............................................................15
2-2-2 磁赤鐵礦.............................................................15
2-2-3 磁學簡介.............................................................17
2-2-3-1 磁滯曲線.............................................................17
2-2-3-2 磁性與粒徑的關係.............................................................19
2-2-3-3 磁性與溫度的關係.............................................................21
2-3奈米粒子的化學特性.............................................................25
2-3-1奈米粒子表面被覆.............................................................25
2-3-1-1 溶膠-凝膠法.............................................................27
2-3-2 核殼型奈米粒子.............................................................28
第三章 實驗程序.............................................................30
3-1 實驗材料與藥品.............................................................30
3-2 儀器設備..............................................................32
3-3 實驗步驟..............................................................35
3-3-1 奈米級γ-Fe2O3之合成..............................................................35
3-3-2 核殼型SiO2/γ-Fe2O3 之製備..............................................................37

3-3-3 核殼型PANI/SiO2/γ-Fe2O3奈米複材之製備..........................38
3-4 性質測定.................................................................39
3-5 樣品代號之說明.................................................................44
第四章 結果與討論.................................................................45
4-1 奈米級γ-Fe2O3.............................................................45
4-1-1 合成γ-Fe2O3結構之鑑定............................................................45
4-1-2 合成γ-Fe2O3之磁性質................................................................51
4-2 核殼型SiO2/γ-Fe2O3奈米複材................................................................57
4-2-1不同TEOS添加量的核殼型SiO2/γ-Fe2O3奈米複材結構之鑑定................................................................57
4-2-2 不同TEOS添加量的核殼型SiO2/γ-Fe2O3 奈米複材之磁學特性................................................................65
4-3 多層核殼型PANI/SiO2/γ-Fe2O3 奈米複材................................................................72
4-3-1不同二氧化矽殼層厚度的多層核殼型PANI/SiO2/γ-Fe2O3 奈米複材結構之鑑定................................................................72
4-3-2不同二氧化矽殼層厚度下多層核殼型PANI/SiO2/γ-Fe2O3 奈米複材之磁學特性................................................................88
第五章 結論................................................................94
第六章 參考文獻................................................................95

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