疏水SiO2气凝胶的制备及表征

以聚二乙氧基硅氧烷(PDEOS)为原料,通过六甲基二硅氮烷(HMDZ)改性剂对制备的凝胶进行表面改性,并常压干燥得到疏水的SiO2气凝胶.研究了改性剂用量对气凝胶疏水性和结构的影响.疏水气凝胶与水的接触角达120°,常压干燥制备的气凝胶具有典型的气凝胶结构特征,气凝胶颗粒尺寸＜100nm,密度和比表面积分别在140～255kg/m3和480～605m2/g范围内.     

常压制备低孔径高比表面积疏水SiO2气凝胶

以正硅酸乙酯为先驱体,丙三醇为干燥控制化学添加剂(DCCA),通过酸碱两步溶胶-凝胶法制备了二氧化硅气凝胶,同时利用六甲基二硅氮烷(HMDZ)和正己烷的混合液对湿凝胶进行表面疏水改性。测试分析了所制备气凝胶的密度、疏水性、比表面积和形貌。结果表明,经过表面改性的SiO2气凝胶具有良好疏水性,与水的接触角约为139.4°,比表面积为952m2/g,平均孔径为5～10nm,孔隙率达94.2%,且其密度仅为0.127g/cm3。     

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。     

水玻璃法SiO_2气凝胶的制备及其疏水改性

以水玻璃为硅源,水为溶剂,采用冷冻干燥法制备了纳米多孔SiO_2气凝胶材料。采用三甲基氯硅烷(TMCS)和六甲基二硅胺烷(HMDS)进行疏水改性,以减少样品在使用过程中的收缩和坍塌。结果表明,TMCS疏水改性SiO2气凝胶的表观密度为0.1682g/cm3,比表面积为363m2/g,HMDS疏水改性SiO_2气凝胶的表观密度为0.2536g/cm3,比表面积为336m2/g。SEM测试结果表明,所得产品具有非晶纳米介孔结构。接触角测定分析表明,TMCS疏水改性SiO2气凝胶与水的接触角为149°,表现出良好的疏水性。     

常压制备低孔径高比表面积疏水SiO2气凝胶

以正硅酸乙酯为先驱体，丙三醇为干燥控制化学添加刑（DCCA），通过酸碱两步溶胶-凝胶法制备了二氧化硅气凝胶，同时利用六甲基二硅氮皖（HMDZ）和正己烷的混合液对湿凝胶进行表面疏水改性。测试分析了所制备气凝胶的密度、疏水性、比表面积和形貌。结果表明，经过表面改性的SiO2气凝胶具有良好疏水性，与水的接触角约为139．4°...     

疏水型SiO2气凝胶薄膜的制备

二氧化硅气凝胶薄膜是一种应用广泛的功能材料.本文采用sol-gel技术和dip-coating镀膜工艺,在玻璃表面上形成了SiO2气凝胶薄膜,对SiO2膜层进行表面修饰处理,得到了疏水型SiO2气凝胶薄膜.研究了催化剂与老化过程对薄膜物性的影响.结果表明该疏水膜能使玻璃表面与水的接触角由50°提高至125°,有明显的疏水效果.     

常压干燥制备SiO2气凝胶的研究

以水玻璃为硅源,采用常压干燥制备了SiO2气凝胶。研究了老化时间、老化剂种类、干燥溶剂种类以及表面改性对SiO2气凝胶结构和性能的影响。结果表明:制得的SiO2气凝胶具有良好的疏水性,密度为0.082g/cm3,孔隙率为96.26%,比表面积达到585.4m2/g。采用扫描电镜(SEM)、傅里叶变换红外分析(FT-IR)、热重分析(TG)、差热分析(DTA)等对疏水型气凝胶的结构和性能进行了研究。     

Al2O3-SiO2复合膜的疏水改性及表征

采用溶胶-凝胶法制备Al2O3-SiO2复合薄膜,通过添加二甲基二乙氧基硅烷(DDS)对其进行疏水改性。研究了DDS添加量对复合溶胶体系稳定性和复合膜表面疏水性的影响,采用接触角测量、红外光谱(IR)、热重分析(TG-DTG)、原子力显微镜(AMF)对样品进行表征。结果表明,对于Al2O3∶SiO2(mol/mol)=1∶2比例下制得的复合膜,随着DDS的加入,薄膜表面疏水性明显增强,当DDS加入过多时,会影响复合溶胶的稳定性,实验确定DDS加入量的最佳值为1%(体积分数);DDS的加入没有破坏复合膜的网格结构,复合膜仍以SiO2颗粒为骨架;经200℃热处理后,可得到具有良好的疏水性能的复合膜。     

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。     

大块SiO_2气凝胶的制备及疏水性能的研究

以廉价工业水玻璃为原料,乙二醇为干燥控制化学添加剂,三甲基氯硅烷为表面改性剂,醋酸为催化剂,通过溶胶凝胶法和常压干燥技术制备出SiO2气凝胶。采用XRD、SEM和FT-IR等方法研究了醋酸浓度对SiO2气凝胶结构的影响,以及表面改性对其疏水性能的影响。结果表明:SiO2气凝胶为典型的无定型非晶态,呈现疏松多孔三维网络纳米结构。采用浓度为1.2mol/L的醋酸进行催化时,得到大块不开裂SiO2气凝胶,其表观密度为0.22g/cm3,孔隙率高达90%。当用三甲基氯硅烷对气凝胶表面进行疏水处理后,凝胶骨架表面接上了硅甲基,表现出较好的疏水性。     

疏水性聚酰亚胺增强SiO2气凝胶复合材料的制备与表征

采用化学交联、溶胶-凝胶和表面改性的方法,制得疏水性聚酰亚胺（PI）增强SiO₂气凝胶复合材料。以均苯四甲酸二酐（PMDA）和4’,4’-二氨基二苯醚（ODA）为聚合单体,3-氨丙基-三己氧基硅烷（APTES）为封端剂,合成APTES封端的聚酰亚胺,与正硅酸乙酯（TEOS）混合形成前驱体。采用酸碱两步催化凝胶、湿凝胶依次进行表面疏水改性、溶液置换及CO₂超临界干燥,得到聚酰亚胺增强SiO₂气凝胶复合材料样品。利用FTIR、SEM、比表面积测试仪、万能材料试验机、接触角分析仪等表征样品的化学组成、微观形貌、孔结构、力学性能及疏水性能等。结果表明：PI质量分数为6wt%的样品密度为0.124 g/cm³,比表面积为724 m²/g,平均孔径尺寸为14 nm,接触角为134°,抗压强度为0.295 MPa。20wt%含量的PI增强SiO₂气凝胶样品抗压强度为0.556 MPa。     

Morphologies and Superhydrophobicity of Hybrid Film Surfaces Based on Silica and Fluoropolymer

Fluoropolymer and different kinds of silica particles were used for controlling surface chemistry and morphology, respectively. A superhydrophobic surface originated from strawberry-like or quincunx-shaped composite silica particles was obtained. The dual size particles are obtained by utilizing the graft of different modified silica particles with epoxy functional group and amine functional group, This makes the surface of film form a composite interface to have irregular binary structure which plays an essential role in trapping air between the substrate surface and the liquid droplets to be necessary for high contact angle and low contact angle hysteresis. The maximum contact angle for water on the hybrid film is about 174±2° and the contact angle hysteresis is less than 2°. The surface morphologies, roughness and the wettability on the surface of films containing different structural silica particles were compared. It was shown that the hierarchical irregularly structure with a low roughness factor and high air-trapped ratio is indispensable for superhydrophobic surface. Although this structural surfaces based on composite silica particles play a vital role in governing the surface wettability, it is necessary to combine with a low surface energy to make the surface superhydrophobic.     

常压干燥制备疏水SiO2气凝胶的影响因素分析

常压干燥制备SiO2气凝胶是近年来该领域的研究重点,工艺条件的优化是提高气凝胶性能的关键。以正硅酸乙酯为硅源,甲基三乙氧基硅烷为共前驱体,采用溶胶-凝胶法,结合老化和三甲基氯硅烷-正己烷-无水乙醇混合溶液的二次表面改性,通过常压干燥工艺制备疏水SiO2气凝胶。利用BET,FT-IR,SEM,TEM和接触角测试等手段对气凝胶进行表征,系统研究水解时间、老化时间、老化温度和改性剂用量对气凝胶性质的影响。结果表明:水解16h,凝胶于55℃下老化48h后,在三甲基氯硅烷与正硅酸乙酯的摩尔比为1.56的混合液下改性48h制备的SiO2气凝胶的性能最好,其孔隙率92%,比表面积969m2/g,接触角达157°。     

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。     

A switchable hydrophilicity solvent mediated process to prepare fine silica aerogel powder as an excellent flatting agent

This work demonstrates a facile two-step method to produce fine silica aerogel powder from silica hydrogel by using N,N-dimethylcyclohexylamine (CyNMe₂) as a CO₂-mediated switchable hydrophilicity solvent. The solvent can almost be totally recycled. More than 70% pore water from silica hydrogel was removed by a quick CO₂ reaction with CyNMe₂ to form a water miscible phase. The silica cake was then dried under ambient pressure with assistance of ethyl acetate as an azeotropic agent. The N₂ adsorption-desorption analysis showed that, the as-prepared silica aerogel powder from a typical hydrogel had a BET surface area of 507.8?m²/g, BJH pore volume of 2.6?cm³/g, and an average pore size of 29.1?nm. The pore volume as well as a narrow particle size distribution (D₅₀?=?6.7?μm) significantly affected the application of the as-produced silica aerogel powder as a flatting agent (FA). Film transmittance index was additionally applied for comparison of the transparence of the applied FA beside the normal extinction index as the performance index. The extinction indices of 61.7 and 52.8% and film transmittance indices of 78.3 and 86.1%, separately for both hydrophobic and hydrophilic applications were measured, hence revealing excellent performance of the as-produced silica aerogel powder.     

Antireflective silica thin films with super water repellence via a solgel process

A solgel process was developed, through which silica films possessing both high antireflection and super water repellence were obtained. In this process, methyl-modified SiO2 sols synthesized by colloidal suspension of SiO2 particles and hexamethyldisilazane (HMDS) were used to deposit spinning-coating films on optical glass substrates. On the resultant films the contact angle for water increased with the increasing amount of HMDS in the reaction mixture. The biggest contact angle was 165 degrees, and the lowest reflectivity on one-sided film reached 0.03%. The antireflections were high all the while. One advantage of this process is that neither a roughened surface nor fluoroalkyltrialkoxylsilane (FAS) is needed to obtained super water repellence.     

SiO2气凝胶的疏水性改性研究

采用三甲基氯硅烷（TMCS）对硅溶胶制备的湿SiO2气凝胶进行表面疏水改性处理,研究了TMCS与孔洞中水的摩尔比对气凝胶的疏水改性作用与性能,用红外光谱法检测了疏水性改性的SiO2气凝胶,发现气凝胶表面的-OH被-OR基团取代,以此构建SiO2气凝胶的疏水性改性机理及模型,试验结果表明,TMCS与孔洞中水的摩尔比控制在0．35左右时可获得不开裂、完好的、具有憎水性特征的二氧化硅气凝胶。     

Preparation of superhydrophobic boehmite and anatase nanocomposite coating films

Developing a surface with water-repelling and self-cleaning ability has attracted much interest in nano-technology. We prepared superhydrophobic films in this study using a mixture of small anatase particles and large boehmite particles. Additionally, a N₂ automated adsorption apparatus, atomic force microscopy and contact angle meter were employed to examine the effects of the added boehmite and anatase to the boehmite ratio on the roughness, micropore ratio and contact angle of the hydrophobic films.As boehmite addition increased from 0 to 8 wt.%, the average roughness increased up to 30 nm, which resulted in the water contact angles increasing from 105° to 155°. The hardness of the films increased from 6B to 2H. The addition of a proper amount of small anatase particles into the large boehmite particles could lead to increasing the micropore ratio in the films, which would enhance the contact angle.