水熱法利用雙乙醯丙酮螯合鈦為前驅物製備奈米二氧化鈦及性質 分析

Preparation and Characterization of Ethoxy Iso-Propoxy Titanium Acetylacetonate Catalyst of a precursor for Titanium Dioxide by Hydrothermal Method

彭惠美(Hui-Mei Peng)

指導教授 ： 蘇昭瑾

國立臺北科技大學/工程學院/有機高分子研究所/碩士(2006年)

摘要

二氧化鈦(Titanium dioxide)為運用在纖維半光化、聚烯及工程塑膠等改質用途等方面最有潛力的材料之一，而每年繼續將有高達5~10%的成長率。除此之外，運用在纖維上的光觸媒更是不餘於力。在光觸媒的運用上，與二氧化鈦粉體的顆粒大小及結晶的相態都有密切的關連，所以製備奈米級的二氧化鈦粉體是目前發展的一重要課題。傳統二氧化鈦合成是利用含鈦的金屬烷氧化物或含鈦的金屬鹽類為前驅體，加以水解及熱處理。而部分報告指出加入螯合劑可以控制二氧化鈦的顆粒大小、均勻性及結晶性。本研究嘗試利用乙醯丙酮合成的螯合錯化物(Ethoxy iso-propoxy titanium acetylacetonate)作為前驅物，使用水熱法及高溫煅燒製備出結構穩定且粒子均勻的奈米二氧化鈦，再經由XRD分析粉體的結晶相、結晶強度。初步結果顯示，乙醯丙酮螯合鈦成功製得奈米二氧化鈦。水熱反應後，經低溫150 oC烘乾時，其相態均為銳鈦礦相(Anatase phase)；而煅燒溫度在700 oC以上時，發現相態由銳鈦礦相(Anatase phase)些相轉變成金紅石相(Rutile phase)，並在TEM看到顆粒聚集的現象。本研究以此為開端提供乙醯丙酮螯合鈦方式的前驅物進而製備更不同的結晶奈米二氧化鈦和形態的研究空間。製備所得二氧化鈦對亞甲基藍有光催化分解效果。

關鍵字

二氧化鈦 ； 螯合鈦前驅體 ； 水熱法 ； 銳鈦礦 ； 金紅石 ； 板鈦礦

並列摘要

Titanium dioxide is one of the most potential materials for semi-light fibre, polyene and engineering plastic , etc. application. Every year continue being up to 5~10% of the rate of increase. In addition, the photocatalytic application of the fibre. The photocatalytic application of TiO2 shows strong correlation with its particle size and crystal property. Therefore, the investigation of preparation on the TiO2 synthesis as well as the crystal phase evolution of the TiO2 product becomes very important. In general, TiO2 synthesis used precursors for the titanium alkoxide or titanium metal salt which are hydrolyzed and thermal treatment to obtain TiO2 crystals. Some report indicated that adding catalytic agent can control the particle size, homogeneity and crystallize for TiO2. To study, we applied new type of a precursor : ethoxy iso-propoxy titanium acetylacetonate, as initial compound for TiO2 synthesis that used hydrothermal method and high temperature calcination. prepared for TiO2 crystals . The crystal structure of the product was by X-ray diffraction(XRD) and the particle dimension. For ethoxy iso-propoxy titanium acetylacetonate, the preliminary results show that the anatase TiO2 was successfully obtained at hydrothermal temperature as low as 150 ºC. TiO2 was obtained at hydrothermal temperature as high as 700 ºC of anatase phase change from rutile phase. The TiO2 particles became aggregated by transmission electron microscopy (TEM). Further study for the optimized condition in preparing the TiO2 is currently under the investigation. In the photocatalytic experimental,the degradation of methylene blue was selected as a test-reaction to confer the photocatalytic activity.

並列關鍵字

titanium dioxide ； precursor ； hydrothermal method ； anatase phase ； rutile phase ； brookite phase

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