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Comparative studies of the physical and hydrophobic properties of TEOS based silica aerogels using different co-precursors

机译:使用不同的前驱体对基于TEOS的二氧化硅气凝胶的物理和疏水性能的比较研究

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In the present paper, the experimental results on the physical and hydrophobic properties of tetraethoxysilane (TEOS) based silica aerogels using six different organosilane co-precursors (C.P) of the type RnSiX4-n as synthesis components, are reported and discussed. The aerogels have been produced by sol-gel processing followed by supercritical drying using methanol solvent extraction. The molar ratio of TEOS, ethanol (EtOH), water (0.001M oxalic acid (H2C2O4) catalyst) was kept constant at 1:5:7, respectively, and the molar ratio of C.P/TEOS (A) was varied from 0.1 to 0.6 and compared the aerogel properties. The hydrophobicity of the aerogels has been tested by the contact angle measurements. The contact angle (θ) has been found to be the highest (θ=136°) for the trimethylethoxysilane (TMES) co-precursor, while for the other co-precursors it is in between 120° and 130°. The surface chemical modification of the hydrophobic aerogels has been studied using Fourier Transform Infrared Spectroscopy (FTIR). As the C.P/TEOS molar ratio increased, the intensity of the C–H and Si–C peaks in the FTIR spectra increased, clearly indicating the organic modification of the aerogels. The aerogels based on mono-alkyl (CH3) trialkoxysilane co-precursor have shown higher optical transmission (≈65%) compared to the phenyl, di or tri alkyl alkoxysilanes (5–50%). The trialkyl modified aerogels showed the lowest bulk density (118.3 kg/m3) and volume shrinkage (<2%). The alkyl alkoxy/chloro–silane modified aerogels have been found to be thermally stable up to a maximum temperature of 573 K, whereas the phenyl trialkoxysilane modified aerogels are stable up to a temperature as high as 823 K. The aerogels have been characterized by scanning electron microscopy, thermogravimetric and differential thermal analyses.
机译:在本文中,使用六种不同的R n SiX 4-型有机硅烷共前体(CP)对基于四乙氧基硅烷(TEOS)的二氧化硅气凝胶进行物理和疏水性能的实验结果n 作为合成成分,已有报道和讨论。气凝胶是通过溶胶-凝胶加工,然后使用甲醇溶剂萃取进行超临界干燥而制得的。保持TEOS,乙醇(EtOH),水(0.001M草酸(H 2 C 2 O 4 )催化剂的摩尔比) C / TEOS(A)的摩尔比分别为1:5:7和0.1 / 0.6,并比较了气凝胶性能。气凝胶的疏水性已经通过接触角测量进行了测试。已经发现三甲基乙氧基硅烷(TMES)共前体的接触角(θ)最高(θ= 136°),而其他共前体的接触角在120°至130°之间。疏水气凝胶的表面化学改性已使用傅立叶变换红外光谱(FTIR)进行了研究。随着C.P / TEOS摩尔比的增加,FTIR光谱中C–H和Si–C峰的强度增加,这清楚地表明了气凝胶的有机修饰。与单烷基,二或三烷基烷氧基硅烷(5-50%)相比,基于单烷基(CH 3 )三烷氧基硅烷共前体的气凝胶显示出更高的透光率(≈65%)。三烷基改性气凝胶的堆积密度最低(118.3 kg / m 3 ),体积收缩率最低(<2%)。已发现烷基烷氧基/氯硅烷改性的气凝胶在最高温度为573 K时是热稳定的,而苯基三烷氧基硅烷改性的气凝胶在高达823 K的温度下是稳定的。电子显微镜,热重和差热分析。

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