Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/10175
標題: 藉由有機修飾二氧化矽表面合成無機複合與多孔氧化物陶瓷之研究
Effect of Organics Modified Silicon Oxide on Synthesis of Inorganic Hybrids and Porous Oxide Ceramics
作者: 郭軒甫
Kuo, Hsiuan-Fu
關鍵字: silicon oxide;二氧化矽;3-trimethoxysilyl propyl methacrylate (MPS);butyl methacrylate (BMA);core/shell;organic/inorganic compound;三甲氧矽烷丙基甲基丙烯酸(MPS);甲基丙烯酸丁酯(BMA);核殼結構;有機/無機複合
出版社: 材料科學與工程學系所
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摘要: 
本研究合成之次微米二氧化矽非晶之粒徑以動態光散射介面電位與粒徑分析儀(DLS)鑑定後,其平均粒徑為0.3±0.15 μm,吾人以此二氧化矽為核,先以三甲氧矽烷丙基甲基丙烯酸(MPS)修飾二氧化矽表面,再與高分子單體甲基丙烯酸丁酯(BMA)聚合,製得有機/無機複合粒子(簡稱SMB)。由傅立葉轉換紅外線光譜儀(FT-IR)、固態核磁共振質譜儀(SSNMR)以及熱重與熱差分析儀(TG/DTA)分析得知,二氧化矽表面之MPS修飾量最多為22%,而BMA與MPS的接枝率最高為67%。進一步將SMB作為模板,無水氯化鋁作為鋁前驅物,在SSNMR與化學分析電子儀(ESCA)的分析結果發現,模板SMB與無水氯化鋁改質後,於固態27Al-NMR圖譜發現兩個峰值,分別位於-0.7與12.7 ppm,顯示粒子中含有鋁的成分且鋁是以六配位與五配位的離子形式存在;由ESCA全能譜圖分析,得知有機/無機複合模板上有Al元素之訊號,於Al2p之窄能譜圖得知Al元素鍵結屬於Al2O3鍵。綜合以上兩組分析,顯示吾人自製之有機/無機複合粒子經無水氯化鋁改質後存在鋁離子之鍵結。將此鋁改質模板於空氣氣氛以1000 oC煅燒兩小時,以場發射掃描式電子顯微鏡(SEM)與能量散射光譜儀(EDS)分析,顯示獲得二氧化矽/氧化鋁核殼結構複合粒子,若進一步以氫氟酸移除二氧化矽核,由穿透式電子顯微鏡(TEM)、擇區繞射(SAD) 與X光繞射分析儀(XRD)觀察,吾人獲得γ-氧化鋁中空結構。藉由比表面積及孔徑分析儀(BET)分析,氧化鋁中空結構之BET比表面積為78.6 m2/g,以Horvath-Kawazoe孔徑分佈模型,氧化鋁多孔結構同時具有微孔(1.35 nm)與介孔(2.23 nm)洞。

Submicrometer silica (SiO2) particles with an average diameter of 0.3±0.15 μm determined from the dynamic light-scattering technique (DLS) were grafted by 3-trimethoxysilyl propyl methacrylate (MPS) to form silica/MPS, hereafter termed SM, followed then by polymerization of butyl methacrylate (BMA) to form silica/MPS/BMA, hereafter termed SMB, hybrid particles. The highest MPS and BMA grafting degrees are 22% and 67%, respectively, determined by Fourier-transform infrared spectrometry (FTIR), solid-state nuclear magnetic resonance spectrometry (SSNMR), and thermogravimetric/differential thermal analysis (TG/DTA).
When the SMB hybrid particles were used as a template, anhydrous aluminum chloride as a precursor for alumina (Al2O3), and tetrachloroethylene as a reactive solvent, the SMB particles showed existence of 5- and 6-coordinated aluminum peaks by SSNMR. The aluminum signals were also confirmed by the electron spectroscopy for chemical analysis (ESCA).
Field-emission scanning electron microscopy (FE-SEM) and Energy Dispersive Spectrometry (EDS) showed that SiO2@Al2O3 structure is obtained after calcination at 1000 oC in air atmosphere from the silica/MPS/BMA/Al hybrid particles. Removal of the SiO2 core via acid etching showed hollow Al2O3 structure from transmission electron microscopy (TEM), selective area diffraction (SAD), and X-ray diffraction (XRD). The hollow Al2O3 structure showed a B.E.T. specific surface area of 78.6 m2/g and a mixture of micro- and meso-pores by the Horvath-Kawazoe model.
URI: http://hdl.handle.net/11455/10175
其他識別: U0005-1707201115564900
Appears in Collections:材料科學與工程學系

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