水凝胶模板制备纳米TiO2及微流控合成TiO2微球

doi:10.15541/jim20140590

无机材料学报 ›› 2015, Vol. 30 ›› Issue (6): 605-609.DOI: 10.15541/jim20140590

水凝胶模板制备纳米TiO₂及微流控合成TiO₂微球

丁学强¹, 张骋¹, 董利民², 王晨², 梁彤祥²

(1. 上海应用技术学院材料科学与工程学院, 上海201418; 2. 清华大学核能与新能源技术研究院, 精细陶瓷北京市重点实验室, 北京100084)

收稿日期:2014-11-17 修回日期:2015-01-13 出版日期:2015-06-04 网络出版日期:2015-05-22
作者简介:丁学强(1989–), 男, 硕士研究生. E-mail: ding_xueqiang@126.com
基金资助:
国家自然科学基金(21271114, 91326203);校复合材料学科建设项目(10210Q140001)

Synthesis of TiO₂ Nanoparticles Using Hydrogel as Template and TiO₂ Microspheres Using Microfluidic

DING Xue-Qiang¹, ZHANG Cheng¹, DONG Li-Min², WANG Chen², LIANG Tong-Xiang²

(1. School of Materials Science and Engineering, Shanghai Institute of Technology, Shanghai 201418, China; 2. Beijing Key Lab of Fine Ceramics, Institute of Nuclear and New Energy Technology, Tsinghua University, Beijing 100084, China)

Received:2014-11-17 Revised:2015-01-13 Published:2015-06-04 Online:2015-05-22
About author:DING Xue-Qiang. E-mail: ding_xueqiang@126.com
Supported by:
National Natural Science Foundation of China (21271114, 91326203);Key Discipline Grant for Composite Materials from Shanghai Institute of Technology (10210Q140001)

摘要/Abstract

摘要：

以聚丙烯酰胺丙烯酸和聚乙二醇/聚丙烯酸两种水凝胶作为模板, 丙烯酸做抑制剂合成纳米颗粒。水凝胶的缓慢吸水和网络结构, 减缓了钛酸四丁酯的水解速率, 并抑制TiO₂的颗粒长大, 制备出的TiO₂纳米粉粒径分布窄, 且为锐钛矿相结构。对比研究发现, 聚乙二醇/聚丙烯酸水凝胶的吸水膨胀率更小, 前驱体溶液的稳定性更高。选用聚乙二醇/聚丙烯酸前驱体溶液, 采用微流控技术制备TiO₂微球, 制备出的微球具有球形度好、单分散的优点, 焙烧后TiO₂的晶体结构为锐钛矿。

关键词: 水凝胶, 水解, TiO2, 微流控

Abstract:

Poly (acrylamide-co-acrylic acid) and polyethylene glycol/polyacrylic acid as templates and acrylic acid as an inhibitor were used to prepare TiO₂ nanoparticles. Hydrogel with low speed of absorption and network structure suppressed the speed of hydrolysis of tetrabutyl titanate and growth rate of TiO₂ nanoparticles. The as-prepared titanium dioxide nanoparticles have anatase phase structure with a narrow size distribution. As compared with poly (acrylamide-co-acrylic acid), polyethylene glycol/polyacrylic acid has lower expansion rate of water-absorption and higher stability of precursor solution. Using microfluidic process, precursor solution of polyethylene glycol/polyacrylic acid is chosen to prepare TiO₂ microspheres. These as-prepared TiO₂ microspheres have a uniform size distrubition and good sphericity, which crystal structure is anatase phase after calcination.

Key words: hydrogel, hydrolysis, titanium dioxide, microfluidic

中图分类号:

TQ133

丁学强, 张骋, 董利民, 王晨,梁彤祥. 水凝胶模板制备纳米TiO₂及微流控合成TiO₂微球[J]. 无机材料学报, 2015, 30(6): 605-609.

DING Xue-Qiang, ZHANG Cheng, DONG Li-Min, WANG Chen, LIANG Tong-Xiang. Synthesis of TiO₂ Nanoparticles Using Hydrogel as Template and TiO₂ Microspheres Using Microfluidic[J]. Journal of Inorganic Materials, 2015, 30(6): 605-609.

图/表 7

图1 微流控装置示意图

Fig. 1 Schematic of the microfluidic device

图2 聚丙烯酰胺丙烯酸 (a) 和聚乙二醇/聚丙烯酸(b)的红外光谱

Fig. 2 IR spectra of poly(acrylamide-co-acrylic acid) (a) and polyethylene glycol/polyacrylic acid (b)

图3 聚丙烯酰胺丙烯酸(a)和聚乙二醇/聚丙烯酸(b)TG-DSC曲线

Fig. 3 TG-DSC curves of poly (acrylamide-co-acrylic acid) (a) and polyethylene glycol/polyacrylic acid (b)

图4 聚丙烯酰胺丙烯酸(a)和聚乙二醇/聚丙烯酸(b)水凝胶制备的TiO2粉末的XRD图谱

Fig. 4 XRD patterns of TiO2 prepared by poly (acrylamide-co- acrylic acid) (a) and polyethylene glycol/polyacrylic acid (b)

图5 两种水凝胶的溶胀率曲线

Fig. 5 Swelling ratio curves of two kinds of hydrogel (a) Poly (acrylamide-co-acrylic acid); (b) Polyethylene glycol/polyacrylic acid

图6 微球成球过程示意图

Fig. 6 Formation process of microspheres

图7 (a)焙烧前和(b)焙烧后TiO2微球的形貌

Fig. 7 Microspheres morphologies of TiO2 microspheres before (a) and after (b) calcinations

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水凝胶模板制备纳米TiO₂及微流控合成TiO₂微球

Synthesis of TiO₂ Nanoparticles Using Hydrogel as Template and TiO₂ Microspheres Using Microfluidic

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