pH对离子液体辅助水热制备介孔二氧化钛结构的影响

doi:10.3724/SP.J.1077.2014.13229

无机材料学报 ›› 2014, Vol. 29 ›› Issue (2): 131-136.DOI: 10.3724/SP.J.1077.2014.13229 CSTR: 32189.14.SP.J.1077.2014.13229

pH对离子液体辅助水热制备介孔二氧化钛结构的影响

王凯¹, 张丽娟¹, 徐志坚¹, 亓滨¹, 底兰波^1, 张秀玲^1,2

(1. 大连大学物理科学与技术学院, 大连 116622; 2. 大连大学辽宁省生物有机化学重点实验室, 大连 116622)

收稿日期:2013-04-24 修回日期:2013-05-27 出版日期:2014-02-20 网络出版日期:2014-01-17
作者简介:王凯(1988-), 男, 硕士研究生. E-mail:wangkai04@126.com
基金资助:
国家自然科学基金(21173028); 辽宁省高等学校优秀科技人才支持计划(LR2012042)

Effects of pH on the Structure of Titania Prepared via Ionic Liquid-assisted Hydrothermal Method

WANG Kai¹, ZHANG Li-Juan¹, XU Zhi-Jian¹, QI Bin¹, DI Lan-Bo¹, ZHANG Xiu-Ling^1,2

(1. College of Physical Science and Technology, Dalian University, Dalian 116622, China; 2. Liaoning key Laboratory of Bio-organic chemistry, Dalian University, Dalian 116622, China)

Received:2013-04-24 Revised:2013-05-27 Published:2014-02-20 Online:2014-01-17
About author:WANG Kai. E-mail:wangkai04@126.com
Supported by:
National Natural Science Foundation of China (21173028); Program for Liaoning Excellent Talents in University (LR2012042)

摘要/Abstract

摘要： 以钛酸四丁酯为钛源, 离子液体1-丁基-3-甲基咪唑四氟化硼([C₄MIM]BF₄)为辅助剂, 采用水热法制备了锐钛矿相的介孔二氧化钛。用盐酸和氨水调节反应前驱体的pH, 考察了pH在1~11变化范围内对离子液体-水制备二氧化钛体系的影响。采用X射线衍射和N2吸附?脱附对样品的晶相和孔结构进行表征。结果表明: 离子液体抑制了板钛矿二氧化钛的形成, 随着pH的增大样品的晶化程度增强。pH在1~9较大范围变化时, 其孔径分布较窄, 平均孔径随pH增大由6.6 nm减小到5.0 nm, 此时离子液体能较好的将样品粒径控制在9 nm左右。这与透射电镜分析结果相一致。

关键词: 水热法, 离子液体, pH, 介孔二氧化钛

Abstract: The mesoporous anatase TiO₂ material was prepared by ionic liquid-assisted hydrothermal method using tetrabutyl titanate as titanium source and ionic liquid 1-butyl-3-methylimida-zolium tetrafluoroborate ([C₄MIM]BF₄) as template. The pH values of the starting suspensions were adjusted from 1 to 11 using HCl or NH₃·H₂O solution. The influence of pH on the ionic liquid-water system for the preparation of titanium dioxide was investigated. The obtained TiO₂ samples were characterized with X-ray diffraction (XRD) and N₂ adsorption-desorption measurements, respectively. The results showed that the addition of ionic liquid inhibited the formation of the brookite TiO₂, and increasing pH values enhanced the crystallization. When the pH was changed at a wide range (pH=1~9), the pore size distributions of the samples were relatively narrow, and the average pore diameter was reduced from 6.6 nm to 5.0 nm by increasing pH value. At the same time, the average size of the TiO₂ nanoparticles in the samples was controlled at about 9 nm by using ionic liquid-assisted hydrothermal method. This is consistent with the results of the transmission electron microscopy (TEM) analyses.

Key words: hydrothermal method, ionic liquid, pH, mesoporous titania

中图分类号:

O649

王凯, 张丽娟, 徐志坚, 亓滨, 底兰波, 张秀玲. pH对离子液体辅助水热制备介孔二氧化钛结构的影响[J]. 无机材料学报, 2014, 29(2): 131-136.

WANG Kai, ZHANG Li-Juan, XU Zhi-Jian, QI Bin, DI Lan-Bo, ZHANG Xiu-Ling. Effects of pH on the Structure of Titania Prepared via Ionic Liquid-assisted Hydrothermal Method[J]. Journal of Inorganic Materials, 2014, 29(2): 131-136.

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pH对离子液体辅助水热制备介孔二氧化钛结构的影响

Effects of pH on the Structure of Titania Prepared via Ionic Liquid-assisted Hydrothermal Method

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