水热法制备掺Fe~(3+)纳米TiO_2粉体及其光学行为研究
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摘要
以钛酸丁酯为前驱体,冰乙酸和无水乙醇为溶剂,以Fe(NO_3)·9H_2O为掺杂剂,采用水热法制备出Fe掺杂纳米二氧化钛粉体。通过X射线衍射仪(XRD)、透射电子显微镜(TEM)和紫外-可见分光光度计(UV-Vis)对样品的晶型结构、微观形貌和光学行为等进行表征,研究水热反应温度、时间、Fe~(3+)的掺杂量对TiO_2粉体的影响。结果表明:随着水热处理时间、温度和Fe~(3+)掺杂量的变化,所得粉体均为锐钛矿相TiO_2纳米粉体,没有出现其他杂相。通过掺杂,XRD射线衍射峰强度有所降低,TiO_2晶粒生长受到抑制,晶粒平均粒径为10 nm左右。Fe~(3+)掺杂量为摩尔分数1%时,纳米TiO_2光吸收强度最强。
Using tetrabutyl titanate as the titanium source,the glacial acetic acid and absolute ethanol as solvent,and the Fe(NO_3)·9 H_2O as the dopant,the Fe doped TiO_2 nano powders were prepared by the hydrothermal method.The crystal structure,microstructure of the samples were analyzed by X-ray diffraction(XRD) and transmission electron microscopy(TEM),respectively.The optical properties of the samples were measured by ultraviolet visible spectrophotometer(UV-Vis),to study the influence of hydrothermal reaction temperature,time and doping amount of Fe~(3+) on TiO_2 powders.The results indicate that with the change of heat treatment time,temperature and Fe~(3+ )doping amount,the powders are all anatase TiO_(2 )nano powder,and there is no other heterozygous phases.Through doping,the peak intensity of X-ray diffraction is decreased and the grain size of TiO_2 is inhibited.The obtained grain size of the grain is about 10 nm.When Fe~(3+) doping amount is 1%(mole fraction),the intensity of TiO_2 absorption is the strongest.
Using tetrabutyl titanate as the titanium source,the glacial acetic acid and absolute ethanol as solvent,and the Fe(NO_3)·9 H_2O as the dopant,the Fe doped TiO_2 nano powders were prepared by the hydrothermal method.The crystal structure,microstructure of the samples were analyzed by X-ray diffraction(XRD) and transmission electron microscopy(TEM),respectively.The optical properties of the samples were measured by ultraviolet visible spectrophotometer(UV-Vis),to study the influence of hydrothermal reaction temperature,time and doping amount of Fe~(3+) on TiO_2 powders.The results indicate that with the change of heat treatment time,temperature and Fe~(3+ )doping amount,the powders are all anatase TiO_(2 )nano powder,and there is no other heterozygous phases.Through doping,the peak intensity of X-ray diffraction is decreased and the grain size of TiO_2 is inhibited.The obtained grain size of the grain is about 10 nm.When Fe~(3+) doping amount is 1%(mole fraction),the intensity of TiO_2 absorption is the strongest.
引文
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[3]田琳琳,姚兰芳,许瑞清,等.铋铁共掺纳米TiO2复合薄膜的制备及光催化性能 [J].稀有金属材料与工程,2012,40(s3):710-715.
[4]You X F,Chen F,Zhang J L.Effects of calcination on the physical and photocatalytic properties of TiO2 powders prepared by sol-gel template method [J].Journal of Sol-Gel Science and Technology,2005,34(2):181-187.
[5]王勇,陈桂华,李李泉,等.可见光响应氮掺杂TiO2制备与性能表征 [J].人工晶体学报,2012,41(4):1053-1058.
[6]李秀艳,杨贤锋,黄松涛,等.水热合成纳米二氧化钛及其光催化性能研究 [J].无机盐工业,2010,42(4):21-24.
[7]贾陈忠,刘松,张彩香,等.光催化氧化降解垃圾渗滤液中溶解性有机物 [J].环境工程学报,2013,7(2):451-456.
[8]张晶,张亚萍,于濂清,等.纳米二氧化钛的水热制备及光催化研究进展 [J].无机盐工业,2010,42(9):6-9.
[9]肖逸帆,柳松.纳米二氧化钛的水热法制备及光催化研究进展 [J].硅酸盐通报,2007,26(3):523-528.
[10]申乾宏,杨辉,高基伟,等.锐钛矿型多孔TiO2薄膜的溶解法制备及性能表征 [J].无机化学学报,2007,23(7):1159-1164.
[11]任学昌,史载锋,孔令仁.TiO2薄膜的Ag改性及光催化活性 [J].催化学报,2006,27(9):815-822.
[12]Linsebigler A L,Lu G,Yates J T.Photo catalysis on TiO2 surfaces:principles,mechanisms,and selected results [J].Chemical Reviews,1995,95(3):735-758.
[13]Wang M,Ioccozia J,Sun L,et al.Inorganic-modified semiconductor TiO2 nanotube arrays for photocatalysis [J].Energy and Environmental Science,2014,7(7):2182-2187.
[14]Choi W,Termin A,Hoffmann M R.The role of metal ion dopants in quantum-sized TiO2:correlation between photoreactivity and charge carrier recombination dynamics [J].The Journal of Physical Chemistry,1994,98(51):13669-13679.
[15]陈建刚,郭常新,张琳丽,等.一步溶液法制备ZnO亚微米晶体棒及其发光性能 [J].发光学报,2006,27(1):59-65.
[16]苗鸿雁,李永强,罗宏杰,等.掺铁二氧化钛纳米粉体的水热法制备与表征 [J].中国陶瓷工业,2003,10(5):1-5.
[17]闫鹏飞,周德瑞,王建强,等.水热法制备掺杂铁离子的TiO2纳米粒子及其光催化反应研究 [J].高等学校化学学报,2002,23(12):2317-2321.
[16]Cui Z K,Li S L,Zhou J Q,et al.Preparation and optical properties of spherical Bi2S3 nanoparticles by in situ thermal sulfuration method [J].Nano,2015,10(2):1550021.
[19]Liu X Y,Zheng H W,Zhang Z L,et al.Effect of energy level matching on the enhancement of photovoltaic response about oxide/Zn2SnO4 composites [J].Journal of Materials Chemistry,2011,21(12):4108-4116.