丙酮为溶剂制备了SiO2气凝胶

本文介绍了以ＴＥＯＳ原料，使用丙酮为溶轩新型纳米多孔材料ｉＯ２气凝胶的方法，并用ＢＥＴ。ＴＥＭ和ＦＩＨ方法研究了该材料的基本结构，与使用酒精溶剂制备的气凝胶进行了比较，并讨论了对水解缩聚反应的影响。     

溶胶－凝胶法制备SiO_2气凝胶及其特性研究

本文以ＴＥＯＳ为原料，采用溶胶－凝胶法和超临界干燥工艺制备了轻质纳米多孔材料ＳｉＯ２气凝胶．研究了溶剂用量及ｐＨ值对溶胶的凝胶化过程和最后制成的气凝胶的特性的影响．并用ＢＥＴ、ＸＲＤ、ＳＥＭ等实验手段研究了这些气凝胶的结构和一些基本物理现象．     

HF催化快速制备SiO2气凝胶

ＳｉＯ２气凝胶晃一种新型轻质纳米多孔泡沫材料,本文以正硅酸乙酯（ＴＥＯＳ）为原料,以乙醇为溶剂,以ＨＦ为催化溶胶－凝胶法快速制备出了ＳｉＯ２气凝胶。ＨＦ的加入大大加速了溶胶－凝胶反应速度,使凝胶时间减少至几分钟甚至更短;同时使凝胶温度降低至室温。ＢＥＴ及ＴＥＭ测试结果表明所制备的ＳｉＯ２气凝胶具有大比表面积（６７３．８ｍ＾２ｇ＾－１）、纳米多孔结构（骨架颗粒为几纳米,孔洞尺寸为５～３０ｎｍ）。     

溶胶—凝胶法制备SiO2气凝胶及其特性研究

本文以ＴＥＯＳ为原料，采用溶胶－凝胶法和超临界干燥工艺制备了轻质纳米多孔材料ＳｉＯ２气凝胶。研究了溶剂用量ｐＨ值对溶胶的凝胶化过程和最后制成的气凝胶的特性的影响。并用ＢＥＴ、ＸＲＤ、ＳＥＭ等实验手段研究了这些气凝胶的结构和一些基本物理现象。     

二氧化硅气凝胶合成新工艺

以Ｅ－４０（多聚硅氧烷）为硅源,以ＨＦ为催化剂,用溶胶－凝胶法制备出了ＳｉＯ２气凝胶法时研究了催化剂、溶剂、水等制备因素对其溶胶－凝胶过程的影响,用孔径分布测定仪、透射电镜（ＴＥＭ）、比表面测试（ＢＥＴ）等方法对其微结构进行了研究。研究结果表明,ＨＦ的加入大大加束字溶胶－凝胶反应速度;ＢＥＴ以及ＴＥＭ测试结果表明所制备的ＳｉＯ２气凝胶具有大的比表面积和纳米多孔结构（骨架颗粒约为１０纳米,孔洞尺政变     

溶胶—凝胶法有机—无机精细复合材料P（VDF／TeFE）—SiO2的制备与显微 …

用溶胶－凝胶法制备了有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２。利用水解－聚合反应由正硅酸乙酯（ＴＥＯＳ）合成ＳｉＯ２溶胶，乙醇作溶剂，盐酸作催化剂。将Ｐ（ＶＤＦ／ＴｅＦＥ）溶于丙酮，并与ＳｉＯ２溶胶均匀混合。凝胶后经干燥和热处理得到有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２。用红外光谱分析、扫描电镜分析、差示扫描热分析和热失重分析对有机－无机精细复事材料Ｐ（ＶＤＦ／ＴｅＦ     

溶胶-凝胶法有机-无机精细复合材料P(VDF/TeFE)-SiO_2的制备与显微结构

用溶胶－凝胶法制备了有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２。利用水解－聚合反应由正硅酸乙脂（ＴＥＯＳ）合成ＳｉＯ２溶胶，乙醇作溶剂，盐酸作催化剂。将Ｐ（ＶＤＦ／ＴｅＦＥ）溶于丙酮，并与ＳｉＯ２溶胶均匀混合。凝胶后经干燥和热处理得到有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２。用红外光谱分析、扫描电镜分析、差示扫描热分析和热失重分析对有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２进行了显微结构表征。     

三嵌段共聚物合成SiO2中孔材料的制备化学

采用溶胶－凝胶法,以正硅酸乙酯（ＴＥＯＳ）为前驱体,添加聚氧乙烯醚（ＰＥＯ）－聚氧丙烯醚（ＰＰＯ）－聚氧乙烯醚（ＰＥＯ）共聚物为模板剂制备结构可控的ＳｉＯ２中孔材料,通过ＢＥＴ、ＴＧ／ＤＴＡ、ＦＴ－ＩＲ、＾２９ＳｉＮＭＲ等分析手段,     

三嵌段共聚物合成SiO2中孔材料的制备化学

采用溶胶一凝胶法,以正硅酸乙酯（ＴＥＯＳ）为前驱体,添加聚氧乙烯醚（ＰＥＯ）一聚氧丙烯醚（ＰＰＯ）一聚氧乙烯醚（ＰＥＯ）共聚物为模板剂制备结构可控的ＳｉＯ_２中孔材料,通过ＢＥＴ、ＴＧ／ＤＴＡ、ＦＴ－ＩＲ、^２９ＳｉＮＭＲ等分析手段,考察了不同条件下溶胶一凝胶制备化学及其热处理对ＳｉＯ_２中孔材料结构性质的影响规律和内在本质．结果表明：通过调节聚合度和添加量以及溶胶老化时间,可以对ＳｉＯ_２中孔材料织构性质进行有效的调控;同时由于该共聚物在不同气氛温度下的脱除机理不同,从而对材料的结构性质影响也有所不同;经真空热处理后,ＳｉＯ_２中孔材料柔性骨架得到加强,孔分布更趋集中．     

TiO2-SiO2复合半导体气凝胶制备及光催化活性研究

ＴｉＯ２－ＳｉＯ２复合半导体气交是一种新型纳米光催化氧化剂。本文以正硅酸乙酯、钛酸丁酯为原料,用溶胶－凝胶法经超临界干燥制备出了ＴｉＯ２－ＳｉＯ２复合半导体气凝胶。研究了ＴｉＯ２：ＳｉＯ２不同配比对溶胶－凝胶过程的影响;用ＢＥＴ、ＸＲＤ、ＳＥＭ、ＴＥＭ等测试方法对其结构进行了表征;以苯酚为探针考察了ＴｉＯ２－ＳｉＯ２复合半导体气凝胶的光催化氧化活性,并与普通锐钛矿型钛白粉光催化剂进行了对比结果表明     

Porosity of resorcinol-formaldehyde organic and carbon aerogels exchanged and dried with supercritical organic solvents

Organic and carbon aerogels have been prepared from resorcinol-formaldehyde resin diluted with various amounts of water. Water was exchanged by acetone or ethanol, and the gels were subsequently dried with supercritical acetone or with supercritical ethanol. We showed that the nature of the solvent with which water was exchanged only had a minor impact on the porosity of the resultant aerogels. In contrast, the same solvents used as drying fluids in the supercritical state led to significant differences, but only in the case of diluted gels. When the initial dilution was low, similar results were indeed obtained with both solvents. Ethanol was shown to lead to higher shrinkages and higher bulk densities than acetone. A higher chemical degradation of the resin during the drying process was also observed when ethanol was used.     

小角X射线散射研究制备炭气凝胶过程中凝胶的微结构演化

酚醛树脂和羟甲基化蜜胺在碱性水溶液中在80℃水浴中反应5d经溶胶－凝胶过程形成了水凝胶。水凝胶经丙酮置换产生酮凝胶，而后经超临界二氧化碳干燥生成有机气凝胶。有机气凝胶在氮气氛中800℃下裂解3h形成了炭气凝胶。采用小角X－射线散射技术和散射理论对上述四种凝胶的微结构进行了分析。结果发现：水凝胶粒子是单分散的，被水溶胀并在0．15nm处有强的散射峰，表明具有纳米尺度的空间周期结构，这种结构是通过不稳态纳米尺度相变－旋节微相分离产生的。由丙酮置换产生的酮凝胶也是单分解的，被丙酮稍微溶胀并在0．15nm具有肩峰，表明水凝胶在溶剂置换过程中发生轻微团聚产生的大粒子在较小角处发生强烈的散射致使强峰演化成肩峰。有机气凝胶和炭气凝胶都是多分散的，在小角处没有散射峰，表明在超临界干燥过程中粒子的团聚继续发生惜驳分散性并掩盖了纳米尺度的空间周期结构致使散射峰消失。有机气凝胶中存在的扩散界面层在其裂解过程中消失，这可能是由于在裂解过程中扩散界面层向粒子迁移以降低界面能所致。从小角X－射线散射数据用Shull-Roess法得到的有机气凝胶和炭气凝胶的回转半径分布比较可知，在裂解过程中，粒子的团聚长大、质量损失和致密化共同作用的结果使得炭气凝胶的回转半径分布比较可知，在裂解过程中，粒子的团聚长大、质量损失和致密化共同作用的结果使得炭气凝胶的回转半径分布比有机气凝胶稍宽，最可几回转半径稍微减少。     

Comparison of the Physicochemical and Electrochemical Properties of Vanadium Oxide-Based Nanomaterials Prepared by Cryochemical Synthesis and Supercritical Drying Technique

Vanadium oxide-based nanomaterials have been prepared by cryochemical synthesis (CCS) and supercritical drying (SCD) in n-hexane and acetone. We have performed the first comparative analysis which demonstrates differences in the physicochemical and electrochemical properties of the products, related to the key features of the effect of the CCS and SCD approaches. The nanomaterials prepared from the same precursor using CCS and SCD (in acetone and n-hexane) have been shown to differ in phase composition and morphology. The oxidizing annealing of the resultant aerogels and cryogel at 500°C in air leads to the formation of only one phase: α-V₂O₅. In all cases except the aerogel prepared using SCD in n-hexane, the crystalline α-V₂O₅ has a higher discharge capacity in comparison with the unannealed aerogels and cryogel. The highest discharge capacity among the annealed aerogels is offered by the sample prepared using SCD in acetone (255 mAh/g), and the highest discharge capacity among the unannealed materials is offered by the sample prepared using SCD in n-hexane (280 mAh/g). The samples range in energy density from 110 to 640 Wh/kg. The highest energy density is also offered by the aerogel prepared using SCD in n-hexane.     

超临界石油醚干燥和超临界二氧化碳干燥在制备有机和炭气凝胶中的比较研究

热固性酚醛树脂—羟甲基三聚氰胺经历聚合反应、溶胶—凝胶、超临界干燥和裂解过程生成了有机和炭气凝胶。比较了超临界石油醚干燥(240℃、6．0MPa下1h)和超临界二氧化碳干燥(60℃、10．0MPa下7d)在制备有机和炭气凝胶过程中的作用。结果发现：超临界石油醚干燥时间比超临界二氧化碳的显著短，虽然前者制备的有机气凝胶的BET比表面和中孔孔容比后者小，但前者制备的有机气凝胶在热裂解过程中的热稳定性比后者好，因此，超临界石油醚干燥制备的炭气凝胶的BET比表面和中孔孔容均比超临界二氧化碳的大。超临界石油醚干燥可以替代超临界二氧化碳干燥来制备炭气凝胶。     

间苯三酚-甲醛气凝胶的制备及氢吸附性能研究

以间苯三酚和甲醛为前驱体制备出了间苯三酚-甲醛气凝胶(PF)及碳气凝胶(CPF),并对气凝胶的结构进行了表征;采用自动吸附仪测定了1.01×10Pa内和液氮温度下PF/CPF气凝胶的氢吸附性能.实验结果表明在该条件下PF/CPF气凝胶氢吸附等温线为第一类微孔型吸附等温线;氢吸附量质量密度分别为1.73%和2.42%,碳化能显著提高气凝胶的氢吸附性能,有望通过改善气凝胶的结构增加微孔数量来提高氢吸附量以实现实际应用.     

炭气凝胶及其有机气凝胶前驱体的吸附性能

间苯二酚和糠醛的醇溶液在六次甲基四胺催化下经溶胶-凝胶过程合成醇凝胶,常压干燥后得到有机气凝胶,经炭化获得炭气凝胶.利用TEM和N2吸附表征了炭气凝胶及其有机气凝胶前驱体的结构,并通过有机蒸汽吸附实验研究了气凝胶的结构-吸附性能关系.实验结果表明：有机气凝胶和炭气凝胶对极性有机蒸汽的静态饱和吸附量高于对非极性有机蒸汽的静态饱和吸附量;提高热处理温度,有利于气凝胶对低浓度极性有机蒸汽和各种浓度非极性有机蒸汽的吸附,但不利于对高浓度极性有机蒸汽的吸附;随着有机蒸汽浓度的提高,气凝胶对极性有机蒸汽的吸附量明显增大,但对非极性有机蒸汽的吸附量影响不大,仅略微上升.此外,气凝胶的室温脱附率高达60 %～85 %.     

Strong, low density, hexylene- and phenylene-bridged polysilsesquioxane aerogel–polycyanoacrylate composites

Nanocomposite aerogels were prepared by chemical vapor deposition and polymerization of cyanoacrylate on the surface of bridged polysilsesquioxane aerogels. Phenylene- and hexylene-bridged aerogels were prepared by sol–gel polymerizations and supercritical carbon dioxide drying. Hydrophobic organic bridging groups in the polysilsesquioxane aerogels reduced the amount of adsorbed water available for initiating polymerizations and led to higher molecular weight polycyanoacrylate than was observed with silica aerogels. Densities increased as much as 65% due to the addition of the organic polymer, but the nanocomposite aerogels remained highly porous with surface areas between 440 and 750 m²/g. Polycyanoacrylate–phenylene-bridged aerogel composites were the strongest with flexural strengths up to 780 kPa or 16-fold stronger than the untreated phenylene-bridged aerogels and fivefold stronger than a silica aerogel of the same density. The strongest polycyanoacrylate–hexylene-bridged aerogel composites had flexural strength of 285 kPa or ninefold stronger than the untreated hexylene-bridged aerogels and twice as strong as a silica aerogel of comparable density. The greater strength of the new composites is, in part, due to the greater strength of the bridged aerogels. However, higher molecular weight polycyanoacrylate, due to less surface water on the hydrophobic bridged aerogels, also contributes to the greater nanocomposite strengths.     

Preparation and Characterization of Silica Aerogels Derived from Ambient Pressure

Silica aerogels were prepared by sol-gel technique from industrial silicon derivatives (polyethoxydisiloxanes, E-40), followed by silylation and drying under ambient pressure. The specific surface area, pore size distribution and thermal conductivity of the silica aerogels were investigated and the results showed that the diameter of the silica particles is about 6 nm and the average pore size of the silica aerogels is 14.7 nm. The specific surface area of which is about 1000 m2·g-1 and the thermal conductivity is about 0.014 wm-1·K-1 at room temperature and pressure of 1.01×105 Pa. The Si-CH3 groups were also detected on the internal surface of the silica aerogels, which show hydrophobic. Silica aerogels derived by this technique is low cost and have wide applications.     

Effect of solvents and catalysts on monolithicity and physical properties of silica aerogels

The effect of various solvents and catalysts on the monolithicity and physical properties of silica aerogels is reported. The aerogels were prepared by hydrolysis and polycondensation of tetramethoxysilane, followed by hypercritical drying, using 6 solvents of different chain lengths, and 17 catalysts consisting of strong and weak acids, bases and their mixtures. It was found that solvents of longer chain lengths and strong basic catalysts resulted in semitransparent to opaque aerogels, whereas strong acids and their combinations with a weak basic catalyst produced transparent but cracked aerogels. While weak acids and their combinations with a weak base were found to produce shrunk and semitransparent (opaque for CH₃COOH + NH₄OH) aerogels, the best quality transparent, monolithic, low-density and refractive index, and large surface area aerogels were obtained for a combination of weak basic catalysts and solvents of shorter branching and chain lengths. The physical properties of the aerogels were studied by BET analysis, porosity, density, refractive index and optical transmission measurements.     

苯酚-间甲酚-糠醛基炭气凝胶的制备及微结构控制

以苯酚、间甲酚和糠醛为原料,在正丙醇溶剂中以盐酸为催化剂经溶胶-凝胶过程合成了醇凝胶,直接超临界正丙醇干燥得到有机气凝胶,在氮气保护下裂解制备出富含中孔的炭气凝胶.用IR、N2吸附、SEM、TEM等表征气凝胶的结构特征,考察了问甲酚苯酚摩尔比对凝胶结构的影响.结果发现:提高间甲酚的含量能够增强聚合物的交联密度,减小聚合物与溶剂的相溶性,缩短相分离时间,有利于得到较小的纳米颗粒和孔径的炭气凝胶.所制得的炭气凝胶平均中孔孔径随间甲酚含量的增加从47 nm逐渐减小至13 nm,BET比表面积和中孔孔容在m-C/P=0.33时达到最大值.