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????? 二氧化钛及其掺Fe材料的制备和电子顺磁共振谱的研究? 神干,殷春浩,朱姗姗,李富强,侯磊田**|1|神干|SHEN Gan|中国矿业大学理学院|College of Science,China University of Mining and Technology|神干(1987-),男,在读硕士,主要研究晶体材料方向.

|江苏省徐州市中国矿业大学理学院A101|221116|[email protected]|15062195190|15062195190|2|殷春浩|YIN Chunhao|中国矿业大学理学院|College of Science,China University of Mining and Technology|||||||3|朱姗姗|ZHU Shanshan|中国矿业大学理学院|College of Science,China University of Mining and Technology|||||||4|李富强|LI Fuqiang|中国矿业大学理学院|College of Science,China University of Mining and Technology|||||||5|侯磊田|HOU Leitian|中国矿业大学理学院|College of Science,China University of Mining and Technology||||||二氧化钛及其掺Fe材料的制备和电子顺磁共振谱的研究?|Study on Preparation and EPR Spectra of Titanium Dioxide and Fe-doped Titanium Dioxide Materilals| (中国矿业大学理学院) 摘要:以钛酸四丁酯、无水乙醇、冰醋酸为原料,在室温下用溶胶-凝胶法制备得到二氧化钛及其掺Fe样品的湿凝胶,室温放置两天后,100 °C干燥得到干凝胶,在500°C下焙烧得到二氧化钛及其掺Fe的粉末状样品.利用X射线衍射、电子顺磁共振等测试手段对样品进行分析,结果显示所得样品均为锐钛矿,Fe被引入了二氧化钛晶格中,Ti3+氧化中心信号强度随Fe掺杂量的增加而增强,峰值向磁场减小方向小幅偏移.在不同测试温度下,含Fe量为0.1%的Fe-TiO2样品中Ti3+氧化中心信号强度随温度升高而增强,峰值也向磁场减小方向小幅偏移.根据电子顺磁共振理论以及二氧化钛在空气中与O2的反应解释了这些现象. 关键词: 溶胶-凝胶法 二氧化钛 电子顺磁共振 中图分类号:O4 Study on Preparation and EPR Spectra of Titanium Dioxide and Fe-doped Titanium Dioxide Materilals SHEN Gan, YIN Chunhao, ZHU Shanshan, LI Fuqiang, HOU Leitian (College of Science,China University of Mining and Technology) Abstract: In this paper, we got TiO2 samples and samples of TiO2 doped with Fe by sol-gel method with tetrabutyl titanate, absolute ethyl, alcoholglacial acetic acid at room temperature. After two days under room temperature, dry it at

100 °C, then we got xerogel. The TiO2 and Fe-doper powder samples were got at

500 °C. The sampels were analyzed by X-ray diffraction and EPR spectrum. The results show that all the samples made in this way were anatase, and Fe was doped in theTiO2 crystal lattice. The signal intensity of Ti3+ oxidation center enhanced with Fe doped increase, and its peak moved to the magnetic reducing direction. Under the different test temperatures, the signal intensity of Ti3+ oxidation center in Fe-doped 0.1% of Fe-TiO2 samples enhanced with test temperatures, and its peak also moved to the magnetic reducing direction. This phenomena was explaned according to the theory of EPR and the reaction of TiO2 and O2. Key words: sol-gel method;

titanium dioxide;

EPR 引言 Fujishima等[1]在1972报道了在光电池中受辐射的的二氧化钛可发生持续的水氧化还原反应而产生氢气,1977年Frank和Bard首次检验到能过使用二氧化钛分解水中的氰化物以来,TiO2作为光催化材料得到了广泛的研究,半导体多相光催化反应方面的研究得到了深入而广泛的开展[2-4].但是由于锐钛矿相的TiO2的禁带宽度为3.23eV,只有在紫外光的激发下才能显示出其催化活性,而太阳光中的紫外光能量仅占4%,这就对TiO2光催化的应用规模和范围产生了极大的限制.因此,如何能有效地利用可见光是决定TiO2光催化性能的关键.二氧化钛纳米材料的制备方法有许多,大体可以分为气相法、液相法.[5]而在液相法中则以溶胶-凝胶法[6]为典型代表.近年来掺Al[7]、Ge[8]等元素的TiO2材料研究层出不穷,很好地改善了TiO2的催化性能.本文即采用溶胶-凝胶法制备TiO2及其掺Fe材料并通过XRD和EPR手段对其进行了表征.Fe掺杂有利于提高TiO2催化活性,但有饱和掺杂浓度0.1%,温度提高也可以提高材料Ti3+离子含量. 实验部分 Fe掺杂TiO2材料的制备 利用钛酸四丁酯作为钛源,无水乙醇为溶剂,冰醋酸为水解抑制剂,制备过程中使用的试剂均为分析纯.首先量取10ml的钛酸四丁酯置于分液漏斗中,并缓慢地滴入到30ml无水乙醇中,10分钟滴完,在滴定过程中用磁力搅拌仪不停地搅拌,得到a溶液;