溶胶-凝胶法制备S掺杂TiO_2纳米粉体的光催化性能
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摘要
本研究采用溶胶-凝胶法制备了S掺杂TiO_2纳米粉体。采用X射线衍射(XRD)、热重差热(TG-DTA)、傅里叶变换红外光谱(FT-IR)、透射电子显微镜(TEM)、能量弥散X射线能谱(EDS)及X射线光电子能谱(XPS)等测试手段对其进行了表征,以亚甲基蓝为模拟污染物,评价了不同热处理条件下的粉体在可见光下的光催化活性。结果表明:S掺杂对TiO_2由锐钛矿型向金红石型的转变有抑制作用,但对其微观形貌没有影响;部分S进入TiO_2晶格间隙形成Ti-O-S键,部分S以SO_4~(2-)的形式吸附于TiO_2表面,S含量约为0.3at%;S掺杂TiO_2纳米粉体具有较高的可见光催化活性,当硫酸钠加入量为10%,550℃煅烧1 h的S/TiO_2样品的光催化活性最佳,在可见光下对亚甲基蓝的2 h降解率由未掺杂的74.12%提高至86.15%。
S-doped TiO_2nano-powders were prepared by a sol-gel method. The powders were characterized by XRD,TG-DTA,FT-IR,TEM,EDS and XPS. The photocatalytic activities of the powders prepared under different heat treatment conditions were evaluated according to their photodegradation behavior to methylene blue in visible light. The results indicated that S doping had no obvious effect on the surface morphology of TiO_2,but inhibited the growth of TiO_2grains and the transformation of TiO_2from anatase to rutile. Parts of S was incorporated into the TiO_2lattice interstitial sites to form Ti-O-S bond,parts adsorbed on the surface of TiO_2as SO_4~(2-),the sulphur content was about 0. 3 at%. In addition,the S-doped TiO_2powders had a good visible photocatalytic activity. The S-doped TiO_2calcined at 550 ℃ with an optimal photocatalytic activity were fabricated with the Na2 SO_4 concentration of 0. 6 wt%. The photocatalytic degradation rate of MB in 2 h increased from 74. 12% for TiO_2to 86. 15% for S/TiO_2.
S-doped TiO_2nano-powders were prepared by a sol-gel method. The powders were characterized by XRD,TG-DTA,FT-IR,TEM,EDS and XPS. The photocatalytic activities of the powders prepared under different heat treatment conditions were evaluated according to their photodegradation behavior to methylene blue in visible light. The results indicated that S doping had no obvious effect on the surface morphology of TiO_2,but inhibited the growth of TiO_2grains and the transformation of TiO_2from anatase to rutile. Parts of S was incorporated into the TiO_2lattice interstitial sites to form Ti-O-S bond,parts adsorbed on the surface of TiO_2as SO_4~(2-),the sulphur content was about 0. 3 at%. In addition,the S-doped TiO_2powders had a good visible photocatalytic activity. The S-doped TiO_2calcined at 550 ℃ with an optimal photocatalytic activity were fabricated with the Na2 SO_4 concentration of 0. 6 wt%. The photocatalytic degradation rate of MB in 2 h increased from 74. 12% for TiO_2to 86. 15% for S/TiO_2.
引文
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[2]刘畅,暴宁钟,杨祝红,等.过渡金属离子掺杂改性Ti O2的光催化性能研究进展[J].催化学报,2001,22(2):215-218.
[3]Ju J F,Chen X,Shi Y J,et al.Hydrothermal Preparation and Photocatalytic Performance of N,S-doped Nanometer Ti O2Under Sunshine Irradiation[J].Powder Technol.,2013,237:616-622.
[4]Lu X N,Tian B Z,Chen F,et al.Preparation of Boron-doped Ti O2Films by Autoclaved-sol Method at Low Temperature and Study on Their Photocatalytic Activity[J].Thin Solid Films,2010,519(1):111-116.
[5]高岳君,许宜铭.氟离子掺杂和吸附对二氧化钛光催化活性的影响[J].物理化学学报,2012,28(3):641-646.
[6]魏凤玉,曾华灵,师彬,等.硫与铁共掺杂对二氧化钛光催化性能的影响[J].硅酸盐学报,2008,36(9):1272-1277.
[7]李媛媛,倪刚,王嘉楠,等.S掺杂Ti O2/粉煤灰复合材料的制备及光催化性能的研究[J].现代化工,2014,34(3):60-63.
[8]陈孝云,陆东芳,林淑芳.S掺杂S-Ti O2/Si O2可见光响应光催化剂的制备及性能[J].催化学报,2012,33(6):993-999.
[9]叶钊,张汉辉,潘海波.Ti(SO4)2水热法制纳米SO2-4/Ti O2光催化剂的光谱研究[J].光谱学与光谱分析,2004,24(3):261-265.
[10]王玉萍,曹金丽,彭盘英.S掺杂形式对Ti O2基光催化剂结构和性能的影响[J].无机化学学报,2009,25(11):2010-2015.
[11]Wagner C D,Riggs W M,Davis L E,et al.Handbook of X-ray Photoelectron Spectroscopy[M].Perkin-Elmer Corporation,Physical Electronics Division,USA,1979.
[12]Hojamberdiev M,Zhu G Q,Sujaridworakun P,et al.Visible-light-driven N-F-codoped Ti O2Powders Derived from Different Ammonium Oxofluorotitanate Precursors[J].Powder Technol.,2012,218:140-148.
[13]江学良,孙刚,张玉婷,等.硫掺杂Ti O2空心球制备及光催化性能研究[J].功能材料,2015,18(46):18078-18082.