合成条件对径向有序介孔二氧化硅中空亚微米球的形貌和结构的影响

doi:10.7517/j.issn.1674-0475.2010.06.442

影像科学与光化学 ›› 2010, Vol. 28 ›› Issue (6): 442-456.DOI: 10.7517/j.issn.1674-0475.2010.06.442

合成条件对径向有序介孔二氧化硅中空亚微米球的形貌和结构的影响

刘志新^1,2, 杜鑫¹, 贺军辉¹, 何勇², 张林³

1. 中国科学院, 理化技术研究所, 功能纳米材料实验室, 北京, 100190;
2. 北京化工大学, 材料科学与工程学院, 北京, 100029;
3. 中国工程物理研究院, 激光聚变研究中心, 四川, 绵阳, 621900

收稿日期:2010-06-20 修回日期:2010-07-14 出版日期:2010-11-23 发布日期:2010-11-23
通讯作者: 贺军辉(1965-), 男, 研究员, 博士生导师, 主要从事功能纳米材料研究, 电话:010-82543535.
基金资助:
国家自然科学基金委员会与中国工程物理研究院联合基金资助(10776034)

Effects of Synthetic Conditions on the Morphology and Structure of Silica Hollow Submicrospheres with Radially Oriented Mesochannels

LIU Zhi-xin^1,2, DU Xin¹, HE Jun-hui¹, HE Yong², ZHANG Lin³

1. Functional Nanomaterials Laboratory, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190, P.R.China;
2. College of Materials Science and Engineering, Beijing University of Chemical Technology, Beijing 100029, P.R.China;
3. Laser Fusion Research Center, China Academy of Engineering Physics, Mianyang 621900, Sichuan, P.R.China

Received:2010-06-20 Revised:2010-07-14 Online:2010-11-23 Published:2010-11-23

摘要/Abstract

摘要： 本文以硬模板与软模板结合的双模板方法(十六烷基三甲基溴化铵(CTAB)为介孔模板,聚苯乙烯(PS)球为中空模板),通过自组装制备出有良好分离性和单分散性且具有径向介孔的二氧化硅中空亚微米球.研究表明CTAB、TEOS的用量,催化剂的种类对二氧化硅中空亚微米球的形貌、壁厚、产品纯度等都有很大的影响.在保持其它实验条件不变的情况下,通过分别单独调节CTAB和TEOS的用量或同时调节CTAB和TEOS的用量,得出最佳原料配比是:TEOS/CTAB/NH3/乙醇/水的摩尔比是1:0.27:9.8:304:2955,TEOS/聚苯乙烯球的质量比是4/1.催化剂的种类对中空亚微米球的形貌也有较大影响,当NaOH(浓度为1 mol/L)的用量为0.05—0.10 mL时,生成由小粒子聚集而成的亚微米球;随着NaOH用量增大到0.10—0.20 mL,小粒子逐渐粘合在一起,亚微米球表面逐渐变光滑;进一步增大NaOH用量为0.20—0.30 mL则导致杂质小粒子的出现.在实验结果和文献报道的基础上,讨论并提出了径向有序介孔二氧化硅中空亚微米球的形成机理.

关键词: 径向介孔, 二氧化硅, 中空亚微米球, 单分散

Abstract: In this work,a dual-templating method using polystyrene submicrospheres(PS) as core template and cetyltrimethylammonium bromide(CTAB) as co-template(porogen) was developed to fabricate hollow silica submicrospheres with radially oriented mesochannels.The fabricated hollow submicrospheres were nearly monodisperse and well separated.The amounts of CTAB and tetraethoxysilane(TEOS) and the kinds of catalyst were shown to have large effects on the morphology,shell thickness and purity of the fabricated hollow submicrospheres.When the amount of CTAB was 0.077 g,severe coalescence of hollow submicrospheres occurred.When the amount of CTAB increased to 0.110 g,the obtained hollow submicrospheres were well dispersed.When the amount of CTAB further increased to 0.143 g,however,impurity of silica nanoparticles increased.When the amount of TEOS was 0.175 mL,the morphology of hollow submicrospheres was less spherical and the shell thickness was not uniform.When the amount of TEOS was 0.250 mL,hollow submicrospheres of good integrity and uniform shell thickness were obtained.When the amount of TEOS further increased to 0.325 mL,the shell thickness of hollow submicrospheres increased significantly and a small amount of silica nanoparticles appeared simultaneously as impurity.The morphology of hollow submicrospheres was also largely affected by the kinds of catalyst.When the amount of NaOH(concentration: 1 mol/L) was 0.05-0.10 mL,spherical aggregates of small silica nanoparticles formed.With increase of the NaOH amount to 0.10-0.20 mL,the small silica nanoparticles gradually fused together and the surface of spherical aggregate became smooth.When the NaOH amount further increased to 0.20-0.30 mL,smaller silica nanoparticles appeared simultaneously as impurity.On the basis of our experimental results and other reports,a tentative mechanism was proposed for the formation of silica hollow submicrospheres with radially oriented mesochannels.

Key words: radially oriented mesochannel, silica, hollow submicrosphere, monodisperse

中图分类号:

TQ174

刘志新, 杜鑫, 贺军辉, 何勇, 张林. 合成条件对径向有序介孔二氧化硅中空亚微米球的形貌和结构的影响[J]. 影像科学与光化学, 2010, 28(6): 442-456.

LIU Zhi-xin, DU Xin, HE Jun-hui, HE Yong, ZHANG Lin. Effects of Synthetic Conditions on the Morphology and Structure of Silica Hollow Submicrospheres with Radially Oriented Mesochannels[J]. Imaging Science and Photochemistry, 2010, 28(6): 442-456.

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合成条件对径向有序介孔二氧化硅中空亚微米球的形貌和结构的影响

Effects of Synthetic Conditions on the Morphology and Structure of Silica Hollow Submicrospheres with Radially Oriented Mesochannels

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