锌离子掺杂的二氧化钛介孔空心微球的制备及光催化性能.pdf

第30卷第10期
无机化学学报
Vol 30 No10
2014年10月
CHINESE JOURNAL OF INORGANIC CHEMISTRY
2323-2331
锌离子掺杂的二氧化钛介孔空心微球的制备及光催化性能
尚鹏博郑玉婴*1冀峰2刘先斌1樊志敏1汪晓莉1
(福州大学材料科学与工程学院,福州350108)
(天津大学化工学院,天津300072)
摘要:以二氧化硅为模板,钛酸四丁酯(TBOn)为钛源,硝酸锌为锌源,采用溶胶凝胶法制备了锌离子掺杂的介孔二氧化钛空心
微球。采用X射线行射(KRD)、比表面积(BED、透射电镜(TEMO、扫描电镜SEM和X射线光电子能谱(XPS等技术对样品进行表
征,以亚甲基蓝(MB)的光催化降解为目标反应评价其光催化活性。结果表明,去核之后的复合微球为空心微球,壁厚为20nm左
右。钛酸四丁酣溶液的滴加时间对微球的形貌影响较大,当滴加时间大于15min时,可以得到结构清晰的空心微球。用氢氧化
钠溶液去除二氧化硅核,反应90min,二氧化硅可以被完全去除。X射线衍射表明,实验得到的掺杂锌离子的空心徽球和没有摻
杂锌离子的空心黴球都是锐钛矿。当锌离子的摩尔分数为0.3%时,二氧化钛空心微球的晶粒尺寸最小,比表面积最大,催化亚
甲基蓝降解的效率最高。
关键词:二氧化钛;空心微球;锌掺杂;溶胶一凝胶;滴加速度;腐蚀时间
中图分类号:0643文献标识码:A文章编号:1001-4861(201410-2323-09
DOI:10.11862/CJIC.2014.317
Zinc Doped Tio 2 Mesoporous Hollow Microspheres
Preparation and Photocatalytic Activity
SHANG Peng-bo ZHENG Yu-ying JI Feng LIU Xian-bin FAN Zhi-min WANG Xia-li
College of Materials Science and Engineering, Fuzhou University, Fuzhou 350108, China)
( College of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
Abstract: Zinc doped Tio, mesoporous hollow microspheres were synthesized based on sol-gel method by using
Sio as the template, tetra-n-butyl titanate as Ti source and Zinc nitrate hexhydrate as Zinc source. The prepared
samples were characterized by means of X-ray diffraction (XRD), low temperature nitrogen adsorption-desorption
( BET surface area), transmission electron microscope (TEM, scanning electron microscopy (EM)and -ray
photoelectron spectroscopy(XPS). Methyl blue dye was used as a target dye to evaluate the photocatalytic activity
of the samples. The results show that microspheres are hollow after removing the Si02 template using an aqueous
solution of NAOH and it takes more than 90 min to completely remove the Sio2 template. The thickness of the
Ti02 shell is about 20 nm. The dropping rate of tetra-n-butyl titanate solution plays an important role in the
structure. When the dropping time exceeds 15 min, the obtained hollow microspheres have clear structure. The
XRD results indicate that pure hollow microspheres and Zinc doped hollow microspheres exist in the form of
anatase. When the doping molar ratio of Zn*to tetra-n-butyl titanate is 0.3%, the obtained hollow microspheres
have the smallest particle size, the biggest BET surface area and show the most efficient degradation of methy
e dye
Key words: titanium dioxide; hollow microspheres; zinc doping; sol-gel; dropping rate; etching time
收稿日期:201404-16。收修改稿日期:2014-07-03。
福建省高校产学合作科技重大关键资助项目(N。.2012H600)、桶州市科技计划项目(No2013-C92)资助项目
通讯联系人。F-mail: yizheng@fzu.edu.en;TEL:1895911811