溶胶凝胶法制备花生状TiO_2及光催化性能
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摘要
二氧化钛(TiO_2)作为环境友好型催化剂,在光催化中发挥着很重要的作用,是一种重要的光催化材料。以钛酸丁酯(TBT)为钛源,采用溶胶凝胶法在非搅拌状态下制得二氧化钛粉体。通过X-射线衍射(XRD)、扫描电镜(SEM)、透射电子显微镜(TEM)以及紫外-可见(UV-Vis)光谱对样品的晶体结构、形貌以及吸光度进行分析测定。试验结果表明,随着煅烧温度的升高,样品由锐钛矿相变为金红石相,形貌也发生了变化;在400℃下煅烧后的样品呈类似花生的形貌,500℃出现了不规则的形状,600℃开始出现金红石相,700℃全部为金红石相和不规则的形貌;以甲基橙为模拟污水,考察样品紫外光照射下降解甲基橙的能力,其中400℃煅烧的样品在光照80 min后甲基橙的降解率达到了91%,光催化性能最好。
As an environment-friendly catalyst,titanium dioxide(TiO_2) plays an important role in photocatalysis.In this paper,TiO_2 powder was prepared by sol-gel method without stirring,using butyl titanate(TBT) as the titanium source.The crystal structure,morphology and absorbance of the samples were analyzed by X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM) and ultraviolet-visible spectroscopy(UV-Vis),respectively.The results show that the phase of the samples changes from anatase to rutile with increase in calcination temperature,combined with the morphology variation.The sample roasted at 400 ℃ shows peanut-like morphology,and the irregular shapes appear at 500 ℃.The rutile phase begins to appear at 600 ℃.At the calcination temperature of 700 ℃,all the phases transfer into rutile with irregular morphology.Using methyl orange as the simulated wastewater,the degradation ability of the samples was investigated under ultraviolet irradiation.The best photocatalytic property can be obtained with the sample calcinated at 400 ℃,leading to 91% of degradation rate for methyl orange at 80 min of illumination.
As an environment-friendly catalyst,titanium dioxide(TiO_2) plays an important role in photocatalysis.In this paper,TiO_2 powder was prepared by sol-gel method without stirring,using butyl titanate(TBT) as the titanium source.The crystal structure,morphology and absorbance of the samples were analyzed by X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM) and ultraviolet-visible spectroscopy(UV-Vis),respectively.The results show that the phase of the samples changes from anatase to rutile with increase in calcination temperature,combined with the morphology variation.The sample roasted at 400 ℃ shows peanut-like morphology,and the irregular shapes appear at 500 ℃.The rutile phase begins to appear at 600 ℃.At the calcination temperature of 700 ℃,all the phases transfer into rutile with irregular morphology.Using methyl orange as the simulated wastewater,the degradation ability of the samples was investigated under ultraviolet irradiation.The best photocatalytic property can be obtained with the sample calcinated at 400 ℃,leading to 91% of degradation rate for methyl orange at 80 min of illumination.
引文
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[15]Ulrike Diebold.The surface science of titanium dioxide[J].Surface Science Reports,2003,48:53-22.
[16]Liu Chunyan.Nano-photocatalysis and photocatalytic environmental purification materials[M].Beijing:Chemical Industry Press,2008.(刘春艳.纳米光催化及光催化环境净化材料[M].北京:化学工业出版社,2008.)
[2]Kavan L,Grazel M,Gilbert S E,et al.Electrochemical and photoelectro chemical investigation of single-crystal anatase[J].Am.Chem.Soc,1996,118:6716-6723.
[3]Tong H,Ouyang S X,Bi Y P,et al.Nano-photocatalytic materials:Possibilities and challenges[J].Adv Mater,2012,24:229-234.
[4]Rajabi M,Shogh S,Zad A I.Defect study of Ti O2,nanorods grown by a hydrothermal method through photoluminescence spectroscopy[J].Journal of Luminescence,2015,157:235-242.
[5]Zhang Dongyun,Bai Menglan,Li Xinmei,et al.Synthesis of mesoporous Ti O2and its adsorption ability for congo red[J].China Powder Science and Technology,2014,20(3):30-33.(张冬云,白孟兰,李新梅,等.介孔Ti O2的合成及其对刚果红的吸附性能[J].中国粉体技术,2014,20(3):30-33.)
[6]Wang Hongxia,Li Xinxing,Tang Zhengwei,et al.Synthesis and properties of Ti O2hollow microspheres[J].Fine Chemicals,2017,34(12):1229-1233.(王红侠,李新星,唐正伟,等.TiO2中空微球的制备及性能[J].精细化工,2017,34(12):1229-1233.)
[7]Agartan L,Kapusuz D,Park J,et al.Effect of initial water content and calcination temperature on photocatalytic properties of Ti O2,nanopowders synthesized by the sol-gel process[J].Ceramics International,2015,70(2):12788-12797.
[8]Ye Yun,Li Qiaoling.Preparation of mesoporous titanium dioxide and research[J].Analytical Instrumentation,2012,6:68-76.(叶云,李巧玲.介孔二氧化钛的制备与研究[J].分析仪器,2012,6:68-76.)
[9]Lu Fan,Chen Min.Synthesis of size-controlled nanotitania particles via a simple so-gel method[J].Journal of Fudan University(Natural Science),2010,49(5):592-597.(卢帆,陈敏.溶胶凝胶法制备粒径可控纳米二氧化钛[J].复旦学报(自然科学版),2010,49(5):592-597.)
[10]Fan Guangsheng,Sun Xuexi,Zhang Bingbing,et al.Study on preparation of nanometer Ti O2powder by micro-emulsion method[J].New Chemical Materials,2016,44(5):130-135.(凡广生,孙学习,张兵兵,等.微乳液法制备纳米Ti O2粉体的研究[J]化工新型材料,2016,44(5):130-135.)
[11]Tian Guanfeng,Liu Hui’e,Chen Shuang,et al.Preparation of nano-TiO2via microemulsion and its modification with grapheme[J].Journal of Chemical Engineering of Chinese Universities,2017,31(1):133-140.(田关锋,刘会娥,陈爽,等.微乳液法制备纳米Ti O2及其与石墨烯的复合改性[J].高校化学工程学报2017,31(1):133-140.)
[12]Zhang Xin,Xu Haiyan,Chen Bo,et al.Preparation of Ti O2thin film with(004)orientation via liquid phase deposition[J].Journal of Synthetic Crystals,2016,45(5):1416-1420.(张欣,徐海燕,陈博,等.液相沉积法制备(004)取向的Ti O2薄膜[J].人工晶体学报,2016,45(5):1416-1420.)
[13]Li Xuandong,Han Xijiang,Sun Haojie,et al.Synthesis,characterization and photocatalytic activity of Ag-doped Ti O2films prepared by liquid phase deposition[J].Journal of Harbin Institute of Technology,2009,41(2):101-104.(李宣东,韩喜江,孙浩杰,等.液相沉积法制备掺银Ti O2薄膜及光催化性能[J].哈尔滨工业大学学报,2009,41(2):101-104.)
[14]Golubovic A,Scepanocic M.Raman study of the variation in anatase structure of Ti O2nanopowers due to the changes of sol-gol synthesis conditions[J].Sol-Gol Sci Technol,2009,49:311.
[15]Ulrike Diebold.The surface science of titanium dioxide[J].Surface Science Reports,2003,48:53-22.
[16]Liu Chunyan.Nano-photocatalysis and photocatalytic environmental purification materials[M].Beijing:Chemical Industry Press,2008.(刘春艳.纳米光催化及光催化环境净化材料[M].北京:化学工业出版社,2008.)
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