SiO_2溶胶配比对气凝胶隔热复合材料力学性能的影响

以无机陶瓷纤维为增强体,与SiO2溶胶混合,经超临界干燥制备了SiO2气凝胶隔热复合材料,研究了SiO2溶胶配比对气凝胶及其复合材料微观结构和力学性能的影响。结果表明,随着SiO2溶胶中乙醇含量的增大,SiO2气凝胶的密度逐渐降低,平均孔径增大,气凝胶中含有的大孔、连孔数量增加,网络骨架结构强度降低。纤维与SiO2气凝胶复合后,气凝胶充满了纤维间的孔隙,形成较好的界面结合。当乙醇/正硅酸乙酯(EtOH/TEOS)摩尔比由2∶1增加到20∶1时,SiO2气凝胶基体传递载荷能力逐渐减弱,材料的力学性能逐渐降低,其拉伸强度、弯曲强度和压缩强度分别由1.9 MPa、2.7 MPa、1.73 MPa(10%应变)降低到0.17 MPa、0.12 MPa、0.04 MPa(10%应变)。     

纤维增强二氧化硅气凝胶复合材料的制备和低温性能

以正硅酸四乙酯(TEOS)为前驱体制备SiO2溶胶,并分别与玄武岩纤维和玻璃纤维复合,经超临界干燥工艺制备了疏水耐低温SiO2气凝胶复合材料。利用傅里叶红外光谱仪、接触角分析仪、激光法导热仪、万能试验机、氮气吸附法对SiO2气凝胶复合材料的结构和性能进行了表征。结果表明:两种纤维增强SiO2气凝胶复合材料在常温及低温下均具有良好的疏水性能和隔热性能,玄武岩纤维增强SiO2气凝胶复合材料和玻璃纤维增强SiO2气凝胶复合材料的接触角分别为148°和142°,常温热导率分别为0.030 W·m-1·K-1和0.026 W·m-1·K-1,-50℃时的热导率分别为0.027 W·m-1·K-1和0.024 W·m-1·K-1,在低温条件下,体积无明显收缩。纤维的加入提供了力学支撑,两种材料不仅在常温下具有良好的力学性能,而且在低温下的力学性能有所增强。     

常压干燥制备疏水性SiO_2气凝胶

以正硅酸四乙酯(TEOS)为前驱体,盐酸和氨水作为催化剂,通过溶胶-凝胶法制备了SiO2醇凝胶,再利用三甲基氯硅烷(TMCS)和正己烷(Hexane)对醇凝胶进行表面改性,最后在常压条件下干燥后制备了疏水性SiO2气凝胶。采用X射线衍射、扫描电镜(SEM)、比表面积测试(BET)、傅里叶转换红外光谱(FT-IR)等测试方法对所得样品的形貌、结构及化学组成等进行了分析。结果表明,所得SiO2气凝胶比表面积可达900m2/g以上,密度200kg/m3,并且具有优异的疏水性。     

复合纤维增强疏水SiO2气凝胶的制备及其性能

以正硅酸乙酯(TEOS)为前驱体,复合纤维为增强相,采用溶胶-凝胶法和常压干燥技术制备了纤维增强疏水SiO_2气凝胶复合材料。利用傅里叶变换红外光谱仪、扫描电子显微镜、比表面积分析仪等手段对气凝胶的化学组成、形貌及结构等进行了分析,并且测量了样品的密度和抗折强度。结果表明:经常压干燥制备的SiO_2气凝胶复合材料加工成块性较好,密度在0.27g/cm~3左右,比表面积达到878.544m~2/g;随着复合纤维的掺入,凝胶填充了纤维之间的大部分微米空隙,并与纤维形成了比较密实的结构,复合材料的抗折强度提高到了1.53 MPa,使得材料有较好的韧性,适用于不规则形状的隔热。     

纤维素气凝胶及纤维素-SiO2复合气凝胶的疏水改性

利用NaOH/Thiourea/H2O作为溶剂体系,采用低温冷冻,常温解冻的方法制备了纤维素水凝胶。通过对正硅酸乙酯(TEOS)水解-缩聚反应速率的控制,采用浸泡的方法获得了纤维素-SiO2复合水凝胶。使用冷冻干燥法分别得到了纤维素气凝胶和纤维素-SiO2复合气凝胶。经过冷等离子改性,以CCl4为等离子体,纤维素及其复合气凝胶由亲水型转变为疏水型,水接触角分别为102°,132°。SiO2的复合降低了纤维素气凝胶的亲水性,复合气凝胶的结构有利于疏水改性。本工作得到的疏水型纤维素气凝胶和复合气凝胶材料,为其在更多领域的应用提供了可能性。     

改性剂对二氧化硅气凝胶性能的影响

本文以正硅酸乙酯(TEOS)为前驱体,通过酸碱两步溶胶-凝胶法,常压干燥制备疏水性SiO2气凝胶。研究了两种改性剂(三甲基氯硅烷、六甲基二硅氮烷)对二氧化硅气凝胶结构和性能的影响。对制备的气凝胶样品进行表面微观形态分析、热重差热分析、傅里叶红外分析以及比表面积分析。结果表明,通过改性制备的样品具有较好的性能,使用六甲基二硅氮烷改性得到的SiO2气凝胶密度为0.204g/cm3,接触角为128°,BET比表面积为973m2/g,平均孔径7.57nm;使用三甲基氯硅烷改性得到的SiO2气凝胶密度为0.115g/cm3,疏水性优良,接触角为158°,BET比表面积为1067m2/g,平均孔径13.40nm。综合考虑各种因素,采用TMCS进行改性制备得到的SiO2气凝胶综合性能更加优异。     

掺杂六钛酸钾晶须SiO_2气凝胶复合材料的研究

以正硅酸四乙酯(TEOS)为硅源,在溶胶-凝胶过程中添加六钛酸钾晶须制备SiO2复合凝胶,通过表面改性和超临界CO2干燥技术获得了大块无裂纹的SiO2气凝胶复合材料。由分析可知,SiO2溶胶的凝胶时间与溶胶体系酸碱性有密切关系,而掺杂不同含量的六钛酸钾晶须对凝胶时间无显著影响;用红外光谱(FT-IR)、BET技术等进一步对其表征,结果表明,制备的样品密度范围为0.20g/cm3~0.29g/cm3,经过疏水改性后,气凝胶表面存在大量憎水基团。BET检测显示,SiO2气凝胶复合材料比表面积达到700m2/g以上,平均孔径为18nm左右,是一种轻质纳米多孔材料。     

Al2O3纤维增强SiO2气凝胶复合材料的制备及其隔热机理

以正硅酸乙酯为先驱体,采用溶胶-凝胶工艺制备SiO2溶胶,将其与Al2O3纤维复合,经超临界流体干燥技术制得SiO2气凝胶复合绝热材料。采用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、压力试验机、平板导热仪等测试手段对样品的微观形貌、抗压强度以及热导率等进行了研究。讨论了材料的绝热机理,并对进一步降低SiO2气凝胶热导率的途径进行了概述。结果表明:添加Al2O3纤维能够明显增强SiO2气凝胶的综合力学性能;经过1000℃热处理的复合材料仍保持SiO2气凝胶的纳米多孔结构,这赋予复合材料优异的绝热特性。当Al2O3纤维添加量为8%(质量分数)左右时,可使复合材料同时具有较低的热导率(λ=0.051W/(m.K),298K)和较高的抗压强度(σbc=1.977MPa)。     

疏水改性对SiO2气凝胶薄膜性能与结构的影响

以正硅酸乙酯(TEOS)为前驱体,采用溶胶-凝胶法制备SiO2气凝胶薄膜,并以不同体积分数的六甲基二硅胺烷(HMDZ)对SiO2气凝胶薄膜进行了疏水改性研究,采用椭偏仪、FITR、接触角测试仪、SEM和光谱仪等对薄膜的疏水性、微观结构及透光性进行了表征,研究了HMDZ疏水改性对SiO2气凝胶薄膜性能与结构的影响。结果表明,疏水改性后,SiO2胶粒表面的大部分亲水性-OH被疏水基团-CH3所取代,其与水的接触角达159°,疏水性好;SiO2气凝胶薄膜在可见光范围内透光率接近90%,透光性高;其孔隙率为78.8%,密度为0.464g/cm3,骨架颗粒尺寸小于40nm,具有纳米多孔网络结构特性。     

疏水性棉短绒纤维素/SiO_2复合气凝胶的制备及性能研究

以棉短绒纤维素为原料,以NaOH/尿素/H_2O为绿色溶剂体系,采用溶胶-凝胶法制备纤维素水凝胶,以硅酸钠(Na_2SiO_3)为硅源,代替传统正硅酸乙酯(TEOS)作为溶剂,通过浸泡法制备了4种纤维素/SiO_2复合气凝胶,再利用十六烷基三甲氧基硅烷(HDTMS)对纤维素/SiO_2复合气凝胶进行疏水改性,采用傅里叶变换红外光谱(FT-IR)和扫描电子显微镜(SEM)等手段对产物进行表征。结果表明:疏水改性后复合气凝胶三维网状结构的孔隙变小,随着Na_2SiO_3用量的增加,疏水纤维素/SiO_2复合气凝胶的接触角逐渐增大,达到147°,吸油量可达到自身质量的8倍,具有较好的疏水亲油性能。     

Synthesis of sustainable silica xerogels/aerogels using inexpensive steel slag and bean pod ash: A comparison study

Low cost silica xerogels/aerogels were synthesized from steel slag and bean pod ash by sol–gel method. Comparison study showed differences between structural, morphological, textural, thermal and physical properties of the silica xerogels and aerogels. Formation of amorphous structure and silica network was confirmed by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy analyses, respectively. Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) analyses revealed that silica xerogels had smaller interlinked network in contrast to silica aerogels. Typical type IV isotherm was observed for all samples in N₂ adsorption-desorption isotherms. The highest surface area was determined as 371 m² g⁻¹ for silica aerogel synthesized from steel slag. Particle size of silica aerogels was lower than that of the silica xerogels. The more porous structure made silica aerogels desirable materials with lower bulk density and thermal conductivity when compared to silica xerogels. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) exhibited high thermal stability of the silica xerogels/aerogels. Although silica xerogels had highly hydrophilic structure, contact angle of silica aerogels synthesized from steel slag and bean pod ash was 60° and 74°, respectively. The comparison study will give a new point of view about differences between silica xerogels and aerogels synthesized from by-products or inorganic/organic waste instead of silicon alkoxides.     

亚临界干燥制备疏水SiO2气凝胶

以E－40（多聚硅氧烷）为硅源,三甲基氯硅烷的异丁醇溶液为干燥介质,用溶胶凝胶法,在亚临界条件下制备出疏水的SiO2气凝胶,通过SEM,孔径分布,比表面积,接触角以及红外光谱的测试对其物性进行了研究,结果表明,所制备的SiO2气凝胶具有典型的纳米网络结构,比表面大具具有疏水性能,亚临界干燥使得制备压力从6．4MPa降低到2．3MPa,降低了制备成本和风险,同时疏水性能提高了SiO2气凝胶环境适应性,从而十分有利于气凝胶的商业应用。     

Hydrophobicity and physical properties of TEOS based silica aerogels using phenyltriethoxysilane as a synthesis component

The experimental results on the hydrophobic and physical properties of tetraethoxysilane (TEOS) based silica aerogels by incorporating phenyltriethoxysilane (PTES) as a synthesis component, are reported. The molar ratio of tetraethoxysilane (TEOS), ethanol (EtOH), water (0.001 M oxalic acid catalyst) was kept constant at 1:5:7 respectively while the molar ratio of PTES/TEOS (M) was varied from 0 to 0.7. After gelation, the alcogels were dried supercritically by the high temperature solvent extraction. For lower M values (<0.1), transparent and monolithic aerogels but for higher M values (>0.5) opaque and cracked aerogels were obtained. For M values in between 0.1 and 0.5, monolithic aerogels with decreasing optical transmission have been obtained. The hydrophobicity of the aerogels was tested by measuring the percentage of water uptake by the aerogels when exposed to 95% humidity at 40°C for 24 h and also by measuring the contact angle. The contact angle varied from 120 to 130° for M values from 0.1 to 0.5, respectively. It was found that as the M value increased, the hydrophobicity of the aerogels increased but the optical transmission decreased from 60% to 5% in the visible range. The thermal conductivity and the specific heat of the aerogels found to decrease with the increase in M values. In order to determine the thermal stability in terms of retention of hydrophobicity of the aerogels, they were heat treated in air in the temperature range of 25–600°C. The hydrophobic aerogels are thermally stable upto a temperature of 520°C, which is the highest value ever reported, and above this temperature the aerogels become hydrophilic. The chemical bonds, responsible for the hydrophobic nature of the aerogels, have been identified by Fourier transform infrared spectroscopy (FTIR). The aerogels have been characterized by density, optical transmission, scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and differential thermal analysis (DTA).     

亚临界干燥制备疏水SiO_2气凝胶

以Ｅ－４０（多聚硅氧烷）为硅源、三甲基氯硅烷的异丁醇溶液为干燥介质,用溶胶凝胶法,在亚临界条件下制备出疏水的ＳｉＯ２气凝胶．通过ＳＥＭ、孔径分布、比表面积、接触角以及红外光谱的测试对其物性进行了研究．结果表明,所制备的ＳｉＯ２气凝胶具有典型的纳米网络结构、比表面积大且具有疏水性能．亚临界干燥使得制备压力从６．４ＭＰａ降低到２．３ＭＰａ,降低了制备成本和风险,同时疏水性能提高了ＳｉＯ２气凝胶环境适应性,从而十分有利于气凝胶的商业应用．     

Physical properties of methyltrimethoxysilane based elastic silica aerogels prepared by the two-stage sol–gel process

The experimental results on the physical properties of methyltrimethoxysilane (MTMS) based elastic silica aerogels prepared by the two stage sol–gel process, are reported. The molar ratio of methanol (MeOH)/MTMS, (M), was varied from 14 to 42 and the molar ratios of acidic water/MTMS, (A) and basic water/MTMS, (B) were each varied from 0.8 to 7.2. The acidic water and basic water concentrations were also varied from 0–0.1 M and 6–13.36 M, respectively. The MTMS based superhydrophobic elastic aerogels could be obtained by adding only distilled water without an acid in the first step which would prevent the possible corrosion of the autoclave during the supercritical drying. With an increase in the MeOH/MTMS molar ratio, the aerogels have been found to become flexible which was characterized by the Young’s modulus. The best quality elastic superhydrophobic aerogels in terms of contact angle (160°), density (37 kg/m³), volume shrinkage (6%), porosity (98%) and thermal conductivity (0.057 Wm⁻¹ K⁻¹) have been obtained for the molar ratio of MTMS:MeOH:acidic water:basic water:: 1:35:3.97:3.97, respectively. The hydrophobicity was confirmed by Fourier Transform Infrared (FTIR) spectroscopy and contact angle measurements. The microstructure of the aerogels has been studied by the transmission electron microscopy (TEM).     

A new route for preparation of sodium-silicate-based hydrophobic silica aerogels via ambient-pressure drying

An in-depth investigation into the synthesis of hydrophobic silica aerogels prepared by the surface derivatization of wet gels followed by subsequent drying at ambient pressure is reported. The following sol–gel parameters were examined for their effect on the physical properties of the derived aerogels: number of gel washings with water, percentage of hexane or methanol in silylating mixture, molar ratio of tartaric acid: Na₂SiO₃, gel aging period, weight% of silica, trimethylchlorosilane (TMCS) percentage, and silylation period. These parameters were varied from 1 to 4, 0 to 100%, 0.27 to 1.2, 0 to 4 h, 1.5 to 8 wt.%, 20 to 40% and 6 to 24 h, respectively. The properties of hydrophobic silica aerogels synthesized by this new route were investigated in terms of bulk density, percentage volume shrinkage, percentage porosity, thermal conductivity and contact angle with water, and by Fourier transform infrared spectroscopy (FTIR). The as-prepared hydrophobic silica aerogels exhibited high temperature stability (up to approximately 435 °C) as measured by thermogravimetric/differential thermal analysis (TGA-DTA). The optimal sol-gel parameters were found to be a molar ratio of Na₂SiO₃:H₂O : tartaric acid : TMCS of 1 : 146.67 : 0.86 : 9.46, an aging period of 3 h, four washings with water in 24 h and the use of a 50% hexane- or methanol-based silylating mixture. Aerogels prepared with these optimal parameters were found to exhibit 50% optical transparency in the visible range, 84 kg m⁻³ density, 0.090 W mK⁻¹ thermal conductivity, 95% porosity and a contact angle of 146° with water.     

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

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 R_nSiX_4-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.     

A new route for preparation of sodium-silicate-based hydrophobic silica aerogels via ambient-pressure drying

Abstract

An in-depth investigation into the synthesis of hydrophobic silica aerogels prepared by the surface derivatization of wet gels followed by subsequent drying at ambient pressure is reported. The following sol–gel parameters were examined for their effect on the physical properties of the derived aerogels: number of gel washings with water, percentage of hexane or methanol in silylating mixture, molar ratio of tartaric acid: Na₂SiO₃, gel aging period, weight% of silica, trimethylchlorosilane (TMCS) percentage, and silylation period. These parameters were varied from 1 to 4, 0 to 100%, 0.27 to 1.2, 0 to 4 h, 1.5 to 8 wt.%, 20 to 40% and 6 to 24 h, respectively. The properties of hydrophobic silica aerogels synthesized by this new route were investigated in terms of bulk density, percentage volume shrinkage, percentage porosity, thermal conductivity and contact angle with water, and by Fourier transform infrared spectroscopy (FTIR). The as-prepared hydrophobic silica aerogels exhibited high temperature stability (up to approximately 435 °C) as measured by thermogravimetric/differential thermal analysis (TGA-DTA). The optimal sol-gel parameters were found to be a molar ratio of Na₂SiO₃:H₂O : tartaric acid : TMCS of 1 : 146.67 : 0.86 : 9.46, an aging period of 3 h, four washings with water in 24 h and the use of a 50% hexane- or methanol-based silylating mixture. Aerogels prepared with these optimal parameters were found to exhibit 50% optical transparency in the visible range, 84 kg m^?3 density, 0.090 W mK^?1 thermal conductivity, 95% porosity and a contact angle of 146° with water.     

SiO2/C/M气凝胶纳米复合材料的结构及吸波性能

本文在SiO2/M(M=Fe,Co,i)复合气凝胶骨架上采用气相催化裂解乙炔的方法合成出SiO2/C/M气凝胶纳米复合材料,用扫描电镜、比表面分析仪、激光导热仪等对材料的结构和物理性能进行了表征,并初步测试了其电磁吸波性能.结果表明,在SiO2/C/M气凝胶纳米复合材料中,碳元素一般以纤维形式均匀分布于气凝胶骨架中,该材料具有低密度,低热导率().05～0.2W/mk),在2mm厚度,8-18GHz的范围内有一定的吸波性能,且吸波性能随频率升高而增加.     

Influence of various processing parameters on water-glass-based atmospheric pressure dried aerogels for liquid marble purpose

Experimental results on the influence of various processing parameters on water-glass-based atmospheric pressure dried aerogels for liquid marble purpose are reported. Silica aerogels were prepared by varying the parameters namely washing temperature of the gels with water, washing period of the gels, protic solvents, and drying method. The physical properties of silica aerogels were studied by measuring granular bulk density, contact angle with water, thermal conductivity, and thermal stability in the furnace. The elemental analyses were carried out using Atomic Absorption Spectroscopy (AAS) and FT-Raman spectroscopy. The structural studies were carried out using Transmission Electron Microscopy (TEM). Also, the effect of humidity on the silica aerogels was studied in humidity chamber. Opaque silica aerogels with hydrophobicity (150°), low density (0.053 g/cm³), and low thermal conductivity (0.068 W/mK) have been obtained for the molar ratio of Na₂SiO₃: H₂O: citric acid: TMCS at 1:146.67:0.72:9.46. The hydrophobic powder of silica aerogels can form the liquid marbles.