遮光剂掺杂Al2O3-SiO2气凝胶/莫来石纤维毡复合材料的高温隔热性能研究

doi:10.15541/jim20170570

摘要/Abstract

摘要：

分别以TiCl₄和ZrOCl₂·8H₂O作为钛源和锆源, 经过溶胶-凝胶和超临界CO₂干燥过程, 将遮光剂粒子TiO₂和ZrO₂掺入到Al₂O₃-SiO₂气凝胶, 并进一步以莫来石纤维毡为增强相制备出具有一定力学性能的耐高温气凝胶复合材料, 分别探究了两种遮光剂粒子对复合材料的微观结构、力学性能和热导率的影响。结果显示: 遮光剂粒子的引入可以有效阻止气凝胶在高温下的塌陷和团聚, 保持气凝胶高孔隙率的特性; 复合材料呈现典型的气凝胶填充纤维结构, 并且具有轻质(0.21~0.24 g·cm^-1)和高强度(弯曲强度为0.98~1.26 MPa)的优异性能, 拓展了材料的实用性; 在 1050℃的高温下, 由于 TiO₂和 ZrO₂粒子对红外电磁波具有吸收和散射作用, 可以将复合材料的热导率由0.098 W·m^-1·K^-1分别降低至0.085 W·m^-1·K^-1和0.076 W·m^-1·K^-1, 从而有效提高材料的高温隔热性能。

关键词: Al₂O₃-SiO₂气凝胶, 红外遮光剂, 热导率, 高温隔热性能

Abstract:

Infrared opacifier-doped Al₂O₃-SiO₂ aerogel/mullite fiber composites were successfully prepared through a mixed Sol-Gel and supercritical drying process by using TiCl₄ and ZrOCl₂·8H₂O as the source of TiO₂ and ZrO₂, respectively. Effects of two kinds of infrared opacifier on microstructure, mechanical property and thermal conductivity of composites were studied. The results show that introduction of infrared opacifier effectively prevent the aerogels from collapse and agglomeration when exposed to high temperature, leading to high-level retention of porosity. The aerogel/mullite fiber composites demonstrate a typical structure of aerogel filled fibrous fiber with marvelous properties—low density (0.21-0.24 g·cm^-1) and high bending strength performance (0.98-1.26 MPa), which expands brilliant potential in many areas of application. When exposed to high temperature of 1050℃, the thermal conductivity of TiO₂ and ZrO₂ doped composites can be significantly reduced from 0.098 W·m^-1·K^-1 to 0.085 W·m^-1·K^-1 and 0.076 W·m^-1·K^-1, respectively, which could be attributed to outstanding scattering and absorbing ability of the infrared opacifiers to the infrared electromagnetic wave. All results indicate that the addition of infrared opacifiers is a promicsing approach to enhance high-temperature properties of aerogel materials.

Key words: Al₂O₃-SiO₂aerogels, infrared opacifier, thermal conductivity, high temperature insulation properties

中图分类号:

TB35

朱召贤, 王飞, 姚鸿俊, 董金鑫, 龙东辉. 遮光剂掺杂Al₂O₃-SiO₂气凝胶/莫来石纤维毡复合材料的高温隔热性能研究[J]. 无机材料学报, 2018, 33(9): 969-975.

ZHU Zhao-Xian,WANG Fei,YAO Hong-Jun,DONG Jin-Xin,LONG Dong-Hui. High-temperature Insulation Property of Opacifier-doped Al₂O₃-SiO₂Aerogel/Mullite Fiber Composites[J]. Journal of Inorganic Materials, 2018, 33(9): 969-975.

图/表 10

图1 800℃高温处理前后气凝胶的SEM照片

Fig. 1 SEM images of aerogels before and after thermal treatment at 800℃(a) AS; (b) AST; (c) ASZ; (d) AS-800; (e) AST-800; (f) ASZ-800

图2 不同温度煅烧后气凝胶的XRD图谱

Fig. 2 XRD patterns of aerogels after calcined at different temperatures(a) AS; (b) AST; (c) ASZ

图3 800℃热处理前后气凝胶的N2吸脱附等温线及孔径分布曲线

Fig. 3 Nitrogen adsorption isotherms (a, c) and pore size distribution curves (b, d) of aerogels before and after heat-treatment at 800℃

表1 气凝胶的孔结构参数

Table 1 Pore structure of aerogels

Sample	S ^a_BET/(m²·g^-1)	V ^b_total/(cm³·g^-1)	D_p^c/nm
AS	856	3.15	24.4
AST	540	1.86	4.2
ASZ	590	1.65	4.4
AS-800	332	1.93	16.9
AST-800	496	1.45	3.8
ASZ-800	447	1.57	4.3

图4 莫来石纤维毡增强复合气凝胶SEM照片

Fig. 4 SEM images of mullite fiber/aerogels composites(a) ASMF; (b) ASTMF; (c) ASZMF

图5 复合材料的弯曲应力-应变曲线图

Fig. 5 Flexural stress-strain curves of composites

表2 复合材料基本物理特征参数

Table 2 Basic physical properties of composites

Sample	Density /(g·cm^-3)	Content of aerogels/%	Bending strength/MPa
ASMF	0.21	42.9	0.98
ASTMF	0.23	47.8	0.62
ASZMF	0.24	50.0	1.26

图6 800℃热处理前后复合材料的N2吸脱附等温线及孔径分布曲线

Fig. 6 Nitrogen adsorption isotherms (a, c) and pore size distribution curves (b, d) of composites before and after heat-treatment at 800℃

表3 复合材料的孔结构数据

Table 3 Pore structure of composites

Sample	S ^t_BET/(m²·g^-1)	S ^a_BET/(m²·g^-1)	V ^b_total/(cm³·g^-1)	D_p^c/nm
ASMF	396	251	0.62	4.4
ASTMF	284	277	0.95	4.8
ASZMF	320	207	0.67	4.3
ASMF-800	/	136	0.34	3.5
ASTMF-800	/	204	0.77	4.4
ASZMF-800	/	192	0.61	3.9

图7 莫来石纤维毡增强复合气凝胶的热导率随温度变化曲线

Fig. 7 Thermal conductivity of composites varying with temperature

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遮光剂掺杂Al₂O₃-SiO₂气凝胶/莫来石纤维毡复合材料的高温隔热性能研究

High-temperature Insulation Property of Opacifier-doped Al₂O₃-SiO₂Aerogel/Mullite Fiber Composites

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