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干燥条件对二氧化硅基干凝胶和气凝胶微观结构的影响。

Effect of the drying conditions on the microstructure of silica based xerogels and aerogels.

作者信息

Durães L, Ochoa M, Rocha N, Patrício R, Duarte N, Redondo V, Portugal A

机构信息

CIEPQPF Department of Chemical Engineering, University Coimbra, Pólo II, Rua Sílvio Lima, 3030-790 Coimbra, Portugal.

出版信息

J Nanosci Nanotechnol. 2012 Aug;12(8):6828-34. doi: 10.1166/jnn.2012.4560.

Abstract

Nanostructured silica based xerogels and aerogels are prepared by sol-gel technology, using methyltrimethoxysilane as precursor. The influence of the drying method and conditions on the microstructure of the obtained materials is investigated, since the drying stage has a critical influence on their porosity. Two types of drying methods were used: atmospheric pressure drying (evaporative), to produce xerogels, and supercritical fluids drying, to obtain aerogels. Although the supercritical fluids drying technique is more expensive and hazardous than the atmospheric pressure drying, it is well known that aerogels are less dense than the xerogels due to less pore shrinkage. However, the ideal situation would be to use atmospheric pressure drying in conditions that minimize the pore collapse. Therefore, in this work, different temperature cycles for atmospheric pressure drying and two heating rates for the supercritical fluids drying are tested to study the gels' shrinkage by analyzing the density and porosity properties of the final materials. The best materials obtained are aerogels dried with the lower heating rate (approximately 80 degrees C/h), since they exhibit very low bulk density (approximately 50 kg/m3), high porosity (95%)-mainly micro and mesopores, high surface area (approximately 500 m2/g), moderate flexibility and a remarkable hydrophobic character (>140 degrees). It was proved that the temperature cycles of atmospheric pressure drying can be tuned to obtain xerogels with properties comparable to those of aerogels, having a bulk density only approximately15 kg/m3 higher. All the synthesized materials fulfill the requirements for application as insulators in Space environments.

摘要

基于纳米结构二氧化硅的干凝胶和气凝胶是采用溶胶 - 凝胶技术,以甲基三甲氧基硅烷作为前驱体制备而成。由于干燥阶段对所制备材料的孔隙率有至关重要的影响,因此研究了干燥方法和条件对所得材料微观结构的影响。使用了两种干燥方法:常压干燥(蒸发法)以制备干凝胶,以及超临界流体干燥以获得气凝胶。尽管超临界流体干燥技术比常压干燥更昂贵且更具危险性,但众所周知,由于孔隙收缩较小,气凝胶的密度比干凝胶小。然而,理想的情况是在使孔隙坍塌最小化的条件下使用常压干燥。因此,在这项工作中,测试了常压干燥的不同温度循环以及超临界流体干燥的两种加热速率,通过分析最终材料的密度和孔隙率特性来研究凝胶的收缩情况。所获得的最佳材料是采用较低加热速率(约80℃/h)干燥的气凝胶,因为它们具有非常低的堆积密度(约50kg/m³)、高孔隙率(95%)——主要是微孔和介孔、高比表面积(约500m²/g)、适度的柔韧性以及显著的疏水特性(>140°)。事实证明,可以调整常压干燥的温度循环以获得性能与气凝胶相当的干凝胶,其堆积密度仅高出约15kg/m³。所有合成材料均满足在太空环境中用作绝缘体的应用要求。

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