纯水体系SiO2纳米多孔材料的低成本制备与表征

doi:10.15541/jim20150119

无机材料学报 ›› 2015, Vol. 30 ›› Issue (10): 1081-1084.DOI: 10.15541/jim20150119 CSTR: 32189.14.10.15541/jim20150119

纯水体系SiO₂纳米多孔材料的低成本制备与表征

赵晶晶, 沈军, 邹丽萍, 王文琴, 祖国庆, 张志华

(同济大学波耳固体物理研究所, 上海市人工微结构材料与技术重点实验室, 上海 200092)

收稿日期:2015-03-10 修回日期:2015-05-21 出版日期:2015-10-20 网络出版日期:2015-09-30
作者简介:赵晶晶(1989–), 女, 硕士研究生. E-mail: jjzhao2009@163.com
基金资助:
国家科技支撑计划(2013BAJ01B01);上海市科委纳米专项(11nm0501600, 12nm0503001);上海航天科技创新基金(SAST201469);科技部863项目

A Low-cost Preparation of SiO₂ Aerogel Monoliths from Silica Sol

ZHAO Jing-Jing, SHEN Jun, ZOU Li-Ping, WANG Wen-Qin, ZU Guo-Qing, ZHANG Zhi-Hua

(Pohl Institute of Solid State Physics, Tongji University, Shanghai 200092, China)

Received:2015-03-10 Revised:2015-05-21 Published:2015-10-20 Online:2015-09-30
About author:ZHAO Jing-Jing. E-mail: jjzhao2009@163.com
Supported by:
National Key Technology R&D Program of China(2013BAJ01B01);Shanghai Municipal Science and Technology Comission Nano Special Project, China(11nm0501600, 12nm0503001);Science and Technology Innovation Fund of Shanghai Aerospace, China(SAST201469);Ministry of Science and Technology Project 863

摘要/Abstract

摘要：

以低成本工业级硅溶胶为硅源, 水为溶剂, 在常压条件下干燥后制备出纳米多孔SiO₂块体材料。在制备过程中, 采用表面活性剂十六烷基三甲基溴化铵(CTAB)来降低水的表面张力, 减少样品在干燥过程中开裂和收缩, 避免了繁琐的溶剂替换过程。所制备的SiO₂块体密度为150~260 mg/cm³, 比表面积为91~140 m²/g, 平均孔径为15~27 nm, 其室温热导率可达0.048 W/(m·K)。该方法大大缩减了制备SiO₂纳米多孔材料的成本, 并降低了操作工艺难度和危险, 将在很大程度上推动硅纳米孔材料的工业化生产与应用。

关键词: SiO2纳米多孔材料, 硅溶胶, 常压干燥, 表面活性剂

Abstract:

Porous monolithic SiO₂ materials were prepared via ambient pressure drying process with low cost silica sol as precursor and water as solvent. Cetyl trimethyl ammonium bromide (CTAB) was used as the surface modifier to get rid of the cumbersome process of solvent substitution which was necessary in the traditional ambient drying process. The densities, specific surface area and the average pore size of the obtained SiO₂ monoliths are in the range of 150-260 mg/cm³, 91-140 m²/g and 15-27 nm, respectively. The thermal conductivity was as low as 0.048 W/(m·K) at room temperature. This method greatly reduced the preparation cost as well as the operation difficulty and risk, which will largely promote the industrial production and application of porous SiO₂materials.

Key words: porous SiO2 materials, silica hydrosol, ambient drying, the surfactant

中图分类号:

O648

赵晶晶, 沈军, 邹丽萍, 王文琴, 祖国庆, 张志华. 纯水体系SiO₂纳米多孔材料的低成本制备与表征[J]. 无机材料学报, 2015, 30(10): 1081-1084.

ZHAO Jing-Jing, SHEN Jun, ZOU Li-Ping, WANG Wen-Qin, ZU Guo-Qing, ZHANG Zhi-Hua. A Low-cost Preparation of SiO₂ Aerogel Monoliths from Silica Sol[J]. Journal of Inorganic Materials, 2015, 30(10): 1081-1084.

图/表 7

表1 制备多孔SiO2材料的原料配比

Table 1 Starting compositions of porous SiO2 materials

Samples	Silica sol/mL	Deionized water/mL	CTAB/g	HF/mL
S2-1	10	20	0.1	0.1
S2-2	10	20	0.1	1.0
S2-3 S2-4	10 10	20 20	0.1 0.2	1.0 0.1
S3	10	30	0.2	1.0

图1 样品S3的实物照片

Fig. 1 Photograph of the sample S3

图2 样品S3在600℃热处理前(a, b)与处理后(c)的SEM照片

Fig. 2 SEM images of sample S3 before (a, b) and after (c) heat-treatment at 600℃for 2 h

图3 样品S3的N2吸附-脱附等温线(a)和孔径分布图(b)

Fig. 3 N2 adsorption-desorption isotherm (a) and pore size distribution (b) of sample S3

表2 样品的部分物理性能

Table 2 Physical properties of the obtained samples

Samples	Bulk density/(mg·cm^-3)	Thermal conductivity^a/(W·m^-1·K^-1)	Surface area/(m²·g^-1)	Average pore size/nm
S2-1	263	—^b	—^b	—^b
S2-2	231	0.057	91.7	15.30
S2-3 S2-4	189 241	0.052 —^b	—^b 140.9	—^b 27.67
S3	158	0.048	119.5	18.60

图4 样品S3分别经过70℃、400℃和600℃处理2 h后的红外图谱

Fig. 4 FT-IR spectra of sample S3 after heat-treatment at 70℃, 400℃ and 600℃ for 2 h

图5 样品S3的DSC/TGA曲线(升温速率为10℃/min, 气氛为空气)

Fig. 5 DSC/TGA curves of the sample S3 tested in air at heating rate of 10℃/min

参考文献 9

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纯水体系SiO₂纳米多孔材料的低成本制备与表征

A Low-cost Preparation of SiO₂ Aerogel Monoliths from Silica Sol

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