碳纳米管掺杂SiO2气凝胶隔热材料的制备与性能表征

以正硅酸乙酯（TEOS）和碳纳米管（CNTs）为原料，采用溶胶-凝胶法和常压干燥法制备不同碳纳米管（CNTs）含量的SiO2气凝胶隔热材料。采用DET、SEM、XRD等测试方法考察了添加CNTs对SiO2气凝胶比表面积、孔结构特征和密度的影响。结果表明：添加CNTs不仅能够增强SiO2气凝胶的强度，而且能够在很大程度上提高气凝胶的比表面积，使孔结构分布更加均匀。     

高比表面积块状氧化铝气凝胶的合成与热性能研究（英文）

采用酸碱两步溶胶凝胶法,以仲丁醇铝为前驱体,硝酸/氨水为酸/碱催化剂,通过酒精超临界干燥制备了氧化铝气凝胶。制备得到的气凝胶块体密度低(50~120kg/m3)、比表面积高(400~500m2/g),具有介孔结构和良好的热稳定性。采用TEM、FTIR、XRD、BET、DSC/TGA等手段表征了氧化铝气凝胶热处理前后的结构和性能。实验表明,制备的氧化铝气凝胶为拟勃姆石结构,经800和1000℃热处理后分别变为γ-Al2O3和δ-Al2O3,对应的比表面积仍分别高达381和183m2/g。添加少量的乙酰丙酮制备的氧化铝气凝胶在热处理前后晶相和比表面积的变化趋势跟未添加的相同,但具有更高的热稳定性。此外,研究了水、氨水和络合剂乙酰丙酮的用量对气凝胶的微结构及比表面积和孔径的影响。     

常压制备低密度高比表面积SiO_2气凝胶的工艺研究

以正硅酸乙酯、乙醇、去离子水、盐酸和氨水为原料制备出SiO_2凝胶后,经老化、表面改性、溶剂置换工艺,再通过常压干燥制备出SiO_2气凝胶,研究了表面改性及溶剂置换工艺对SiO_2气凝胶性能的影响.结果表明,随着表面改性次数和改性剂浓度的增加,气凝胶的密度和比表面积降低;溶剂置换对气凝胶的密度和比表面积影响不大.通过优化的工艺制备出的SiO_2气凝胶具有疏水性,与水的接触角约为118°,密度为0.124 g/cm~3,孔隙率94.3%,平均孔径为23.3 nm,比表面积712 m~2/g.     

MgO气凝胶制备及结构研究

以甲醇镁为镁源,甲醇和去离子水为溶剂,采用溶胶-凝胶法结合乙醇超临界干燥工艺制备MgO气凝胶,考察去离子水、甲醇、丙三醇对MgO气凝胶凝胶时间及比表面积的影响,采用红外光谱(FTIR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)、氮气吸脱附测试仪等对其结构及形貌进行表征,并且利用同步辐射小角X射线散射(SAXS)对其进行了分形结构分析。结果表明：MgO气凝胶具有丰富的网络骨架结构、高的孔隙率(98%)、高的比表面积(904.9 m₂/g)、较低的密度(0.055 g/cm₃),平均孔径为19.6 nm,属典型的介孔材料,SAXS测试显示MgO气凝胶分形维数为2.32,表面粗糙且疏松,具有明显的孔分形结构。     

碳气凝胶的纳米结构控制及其在锂离子电池中的应用(英文)

以间苯二酚和甲醛为前驱体,通过溶胶凝胶法制备有机气凝胶,通过高温裂解制备得到碳气凝胶。由于其高的比表面积,低的电阻率,空间网络结构以及化学惰性,碳气凝胶被认为是可充电电池的理想电极材料。研究了碳气凝胶的制备和结构控制,通过SEM,BET,XRD等手段测试其显微结构性质和结构控制。BET测试结果表明有机气凝胶炭化以后,比表面积显著增加,碳气凝胶具有518～621m2/g的较高比表面积。碳电极分别由碳气凝胶、石墨、碳气凝胶和石墨的混合物与黏结剂组成,以锂片为对电极制成纽扣电池。电化学测试结果显示其具有很高的首次放电容量(958.6mAh/g),但是可逆容量只有总容量的30%到40%。并且混合电极的性能优于其他纯电极。     

纤维增强气凝胶柔性隔热复合材料的制备

以正硅酸乙酯(TEOS)为原料,酸碱催化两步法配制溶胶,浸渍柔性纤维毡后进行超临界干燥制备柔性隔热复合材料.研究表明,随着超临界干燥溶胶之前老化时间的延长(1 h～7 d),复合材料在600℃下的抗拉强度变大(0.13～0.21MPa),红外光谱分析确定是由于其水解程度变大.复合材料中的纯气凝胶比表面积为209.8 m2/g,平均孔径为18.8 nm.场发射扫描电镜照片表明气凝胶很好地填充于纤维之间,避免了纤维与纤维的接触.从而柔性复合材料具有低热导率,120、500℃下分别为0.019、0.054 W/m·K.     

PAN预氧丝复合RF气凝胶的性能研究

本文以间苯二酚(C6H4(OH)2)和甲醛(HCHO)为前驱体,碳酸钠(Na2CO3)为催化剂,采用溶胶-凝胶技术、超临界干燥工艺制备了间苯二酚-甲醛(RF)气凝胶。另外,通过添加聚丙烯腈(PAN)预氧丝改善了RF气凝胶的力学性能,制备了PAN预氧丝复合RF气凝胶。文中通过调节质量分数ω、间苯二酚与催化剂摩尔比(R/C值)这两个参数对微结构进行调控,其中选取质量分数ω为15%, R/C值为100和500的气凝胶进行比较,经过分析可知R/C值为100的气凝胶性能优良,复合后样品的比表面积变为618.6 m₂/g,孔体积为2.423 cm₃/g,平均孔径为15.1nm。PAN预氧丝复合后的气凝胶依然具有优异的热学性能,在常温下热导率为0.032W/(m.K)。力学性能有了很好的改善,压缩模量为1.499MPa,比纯RF气凝胶提高了0.6倍。     

混合溶剂对氧化铬基气凝胶微结构的影响

采用环氧化物法和无机分散溶胶凝胶法,通过改变甲苯/乙醇混合溶剂比例制备了氧化铬基气凝胶和干凝胶。当甲苯/乙醇体积比由1:3增大至3:1时,环氧化物添加法制备的氧化铬基气凝胶的平均孔径从14nm变为21nm,比表面积从66m2/g升为244m2/g,总孔体积容量由0.2339cm3/g增至1.296cm3/g。无机分散溶胶凝胶法制备的气凝胶(添加聚丙烯酸PolyAcrylicAcid,PAA),比表面积则由276m2/g降至66m2/g,总孔体积容量从0.9601cm3/g降至0.2339cm3/g。结果表明,采用混合溶剂和和添加PAA的方法可能实现对气凝胶微结构的连续调控。     

二氧化硅气凝胶的制备与表征(英文)

二氧化硅气凝胶是目前世界上最轻的人造多孔固体材料。采用硅酸钠为硅源,通过采取老化、溶剂置换、表面改性和分级干燥等一系列措施,常压干燥制得SiO2气凝胶颗粒,并利用红外光谱、比表面分析、扫描电镜等测试方法对其结构、形貌及化学组成进行了分析。研究表明:该样品呈疏水性,孔径较小,比表面积为740m2/g,孔体积为0.89cm3/g,平均孔径为4.8nm。     

高分子纤维增韧SiO_2气凝胶复合材料的制备

以正硅酸乙酯为硅源,乙醇和水为溶剂,芳纶纤维为增强相,通过溶胶凝胶及常压干燥等步骤,实现了芳纶增韧SiO_2气凝胶复合材料的非超临界制备.采用扫描电镜、吸附-脱附等分析手段及热导率测试对所得气凝胶样品进行结构分析和性质表征.结果表明,调节反应体系的各反应参数可以获得具有不同外形、密度及热导率的复合材料;所得气凝胶平均孔径约为10～20 nm,比表面积可达1000 m~2/g,可望在隔热材料等领域得到应用.     

Hydrogen Storage Property of Porous/Hollow TiO2 Using Yeast as Template

研究表明：在620 ℃煅烧后,模板除去,TiO2形成。产物主要由TiO2 和少量的H2Ti3O7组成。得到的产物的比表面积为252.6 m2/g。P-C-I测试结果表明,30 ℃时TiO2显示可逆的吸/放氢过程。在吸/放氢过程中,化学键发生微小的偏移,表明氢可能和OH基团发生反应。随着吸/放氢循环的增加以及比表面积的明显的降低,多孔/中空TiO2坍塌。同时,随着温度的升高,化学吸附量增加,吸氢量升高     

Carbon aerogels for electric double-layer capacitors

In this study, carbon aerogels were derived via the pyrolysis of resorcinol-formaldehyde (RF) aerogels, which were cost-effectively manufactured from RF wet gels by an ambient drying technique instead of conventional supercritical drying. By varying the R/C ratio (molar ratio of resorcinol to catalyst), mesoporous carbon aerogels with high specific surface area were prepared successfully and further investigated as electrode materials for electric double-layer capacitors (EDLCs). The textural properties of carbon aerogels obtained were characterized by nitrogen adsorption/desorption analysis and SEM. The electrochemical performances of carbon aerogels were investigated by impedance spectroscopy, galvanostatic charge/discharge and cyclic voltammetry methods. The results show that BET surface area and specific capacitance increase with R/C ratio, the maximum values of 727 m2·g-1 and 132 F·g-1 are achieved at R/C ratio will of 300. Increasing R/C ratio increase the average pore size of carbon aerogel electrode, which has improved the rate capability. Furthermore, EDLC with carbon aerogel electrodes has an excellent stability at large discharge current and long cycle life.     

Preparation and characterization of CuO-CoO-MnO/SiO2 nanocomposite aerogels as catalyst carriers

CuO-CoO-MnO/SiO₂ nanocomposite aerogels were prepared by using tetraethyl orthosilicate (TEOS) as Si source, and aqueous solution of Cu, Co and Mn acetates as the precursors via sol-gel process and ethanol supercritical drying technique. The gelatination mechanism was investigated by nuclear magnetic resonance (NMR) and X-ray photoelectron spectroscopy (XPS). The microstructure and composition of the CuO-CoO-MnO/SiO₂ nanocomposite aerogels were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron dispersive spectroscopy (EDS) and XPS. The specific surface area, pore size and pore size distribution of the nanocomposite aerogels were determined by the Brunauer-Emmett-Teller (BET) method. The products were analyzed by gas chromatography (GC). The results show that the CuO-CoO-MnO/SiO₂ nanocomposite aerogels are porous, with a particle size distribution of 10–150 nm, a pore size distribution of 2–16 nm, an average pore size of 7.68 nm, and a specific surface area of 664.4–695.8 m²/g. The molar fraction of transition metals in the nanocomposite aerogels is 0.71%-13.77%. This kind of structure is favorable not only to increase the loading of catalysts, but also to make full use of the effect of transition metal oxides as cocatalysts; CuO-CoO-MnO/SiO₂ nanocomposite aerogels can be used as a novel catalyst carrier in the safer and environment-friendly synthesis of diphenyl carbonate and other fields of catalysis.     

稻壳灰制备掺杂TiO2硅气凝胶研究

以稻壳为硅源制备SiO2气凝胶，在溶胶凝胶过程中加入TiO2纳米粉末，可制得掺杂TiO2硅气凝胶。通过SEM、BET吸附．脱附测试等手段，与同种方法制得的纯SiO2气凝胶在结构和物性特征方面等进行了比较。结果显示，掺杂TiO2气凝胶的平均颗粒直径为50nm左右，而纯SiO2气凝胶的粒径约为20nm，且孔洞直径明显减小、孔径分布更为均匀；此外，TiO2纳米粉末的加入可以使气凝胶的弹性模量提高约23％，并且通过TiO2对气凝胶溶胶-凝胶过程的影响研究了其影响机理。     

Capacitance performance enhancement of TiO2 doped with Ni and graphite

Nano-amorphous TiO2 was prepared by a sol-gel method. The results of X-ray diffraction (XRD) and scanning electron microscopy (SEM) show that the composite electrode material (TiO2-NiO-C) is made of powder with a grain size of 36.2 nm. Doping of nickel and graphite can increase the electrical conductivity and the specific surface area of nano-amorphous TiO2. The electrochemical properties of TiO2-NiO-C,such as self-discharge, leakage current, and cycle life, were studied using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and charge-discharge test. With a charge-discharge current density of 500 mA/g, the specific capacity of the TiO2-NiO-C composite material reaches 12.88 mAh/g. Also, the expense of capacity is only 3.88% after 500 cycles. The electrochemical capacitor with the electrode material of TiO2-NiO-C shows excellent capacity and cycling performance.     

Effect of dehydration on porous structure of monolithic aerogels based on fibrous aluminum oxyhydroxide

Aluminum oxide monolithic aerogels (PMAOs) with specific surfaces of up to 400 m²/g and densities of up to 0.004 g/cm³ were obtained by the direct oxidation of metallic aluminum by water vapors. Studies of the obtained aerogels using the methods of scanning and transmission electron microscopy showed that a freshly prepared aerogel represents the amorphous structure from alumina fibrous with a diameter of about 5 nm. Parameters of a porous aerogel structure were determined from the isotherms of adsorption of nitrogen vapors at 77 K. It is shown that the specific surface area decreases by 50% upon the dehydration of aerogel by temperature pretreatment at 900°C until the phase transition temperature is reached. At the same time, heat treatment at temperatures above 1200°C results in a phase transition at which significant contraction of structure occurs and the specific surface area decreases to 20 m²/g. The number of primary adsorption centers was obtained from comparative plots of water vapor adsorption. It was found that preliminary dehydration only slightly affects the number of primary centers of water adsorption.     

Photocatalytic degradation of MO by complex nanometer particles WO3/TiO2

Complex nanometer particles WO3/TiO2 were prepared using a sol-gel process and characterized using XRD spectra. The photocatalytic activity of TiO2 can be increased by doping W^6＋ with TiO2 because the doped W^6＋ that entered into the crystal lattices of TiO2 led to the formation of defects in the crystal lattices of TiO2 and thereby improved the photocatalytic activity of TiO2.When WO3 doped in TiO2 exceeded 3%, the excess W^6＋ did not enter into the crystal lattices of TiO2 but were uniformly dispersed in TiO2 or they covered the surface of TiO2, which reduced the effective illumination area of TiO2 and thereby lowered the photocatalytic activity of TiOE.The relationship among the composition of the catalyst, the amount of photocatalyst, the illumination time, and the decolorizing rate of methyl orange （MO） were discussed. The results show that the decolorizing rate of MO can reach 82.3% using WO3/TiO2 as the photocatalyst, with the composition of WO3/TiO2 -3：97, the mass of catalyst = 0.400 g, the initial concentration of MO = 20 mg/L, pH = 6.5, and the illumina- tion time = 7 h.     

Photocatalysis Performance of Nb-doped TiO2 Film in Situ Growth Prepared by a Micro Plasma Method

采用微等离子体氧化法,在H2SO4溶液为电解液中以钛合金为基体制备原位生长的TiO2薄膜,并以罗丹明B溶液为目标污染物测试其光催化性能。为提高所得TiO2薄膜的光催化性能,向电解液中添加了不同浓度的草酸铌,制备了原位Nb掺杂TiO2薄膜。利用扫描电镜(SEM)和X射线衍射仪(XRD)分别对Nb掺杂前后的TiO2薄膜表面形貌、元素组成和晶体结构进行了分析。结果表明,Nb掺杂能使介孔TiO2晶粒细化,比表面积增大,Nb对TiO2晶相组成影响不大,但对晶胞参数有所影响,Nb掺杂可有效提高TiO2的光催化活性,其中当草酸铌为1.2g/L时,对初始浓度为10 mg/L罗丹明B溶液90min的降解率可达到85%,表现出最强的光降解能力。