制备条件对气凝胶粉末粒径的影响

 利用超声波乳化技术，结合溶胶-凝胶反应制备了间苯二酚-甲醛有机气凝胶粉末和碳化气凝胶粉末。通过大量实验，探讨了制备条件对气凝胶粉末粒径的影响。在粉末干燥前以Zeta电位-粒径分布测试仪对乙醇悬浊液进行分析测试，对有机粉末和碳化粉末用TEM方法进行表征。研究了反应液质量分数、反应温度和时间以及分散剂与反应液体积比对产物粒径的影响。实验表明：制备条件对于制备纳米级的气凝胶粉末影响非常大，通过优化实验条件可以制备出分布较好的气凝胶粉末，超声功率较大容易实现体系均匀混合，反应液在反应过程中温度和时间的控制起着关键的作用，低质量分数的反应液所生成的产物比高质量分数的粒径要小,经碳化后粉末粒径进一步降低。     

掺钛空心玻璃微球制备技术

为实现惯性约束聚变靶用空心玻璃微球的均匀掺杂,采用溶胶-凝胶技术结合炉内成球法,以钛酸四丁酯为掺杂剂,对钛掺杂玻璃溶胶-钛掺杂玻璃凝胶-钛掺杂干凝胶粒子-钛掺杂空心玻璃微球（Ti-HGM）这一掺钛空心玻璃微球的制备方法进行了探索。实验结果表明:掺钛效应使空心玻璃微球壁厚均匀性、同心度有所降低,但对壁厚、直径控制基本无影响;Ti与Si原子分数比为2.23%的Ti-HGM掺杂基本均匀,近70%微球的保气半寿命在一个月以上。     

纳米碳管复合凝胶玻璃结构及谱学性能研究

用物理掺杂工艺将纳米碳管引入二氧化硅凝胶玻璃基质, 成功制备了纳米碳管复合凝胶玻璃, 采用X射线衍射、透射电子显微镜、紫外-可见吸收光谱、红外光谱、拉曼光谱等测试方法对其结构和谱学性能进行了表征. 结果表明, 通过优化掺杂工艺能够实现纳米碳管与基质的均匀复合, 纳米碳管本身的结构在掺杂过程中并未发生改变. 纳米碳管的引入对二氧化硅凝胶玻璃基质的紫外-可见吸收光谱和红外光谱未产生显著影响.     

TiO2 .nH2O凝胶预处理对水热合成SrTiO3粉的影响

以TiCl4为钛源,首先制备TiO2*nH2O凝胶,然后在80℃的水热条件下制备了SrTiO3粉.利用X射线衍射(XRD)、透射电子显微镜(TEM)和红外光谱(FTIR)研究了TiO2*nH2O凝胶水洗方式、阴离子(Cl-和NO3-)以及TiO2*nH2O热处理对SrTiO3粉性能的影响.结果表明,水洗和热处理都能使TiO2*nH2O凝胶产生晶化;TiO2*nH2O的晶化程度对产物SrTiO3颗粒的粒度和粒度分布有很大影响,以非晶质TiO2*nH2O为钛源制备的SrTiO3颗粒粒度大且粒度分布宽.以结晶TiO2*nH2O为钛源制备的SrTiO3颗粒粒度小且粒度分布窄,而且可以得到纳米颗粒.水热反应液相中存在Cl-或NO3-能使产物SrTiO3颗粒粒度稍有增大.综合以上结果,TiO2*nH2O凝胶水洗对产物颗粒的影响主要是由于使凝胶产生了晶化,而由阴离子脱除产生的影响很小.因此,在不考虑阴离子对其它工程化影响(如设备腐蚀等)的前提下,可采用热处理代替水洗.     

制备条件对纳米晶吸收剂的吸波性能影响的实验研究

采用柠檬酸盐溶胶凝胶法制备出不同Co掺杂的Ba纳米晶铁氧体吸收剂,分析了制备条件对其物性、吸波性能等的影响,确定了最佳制备工艺条件. 研究了粒径对纳米晶吸波性能的影响,同时还测试了纳米晶吸收剂的雷达波吸收性能. 结果表明,纳米晶吸收剂是一种性能优良的雷达波吸收材料. 关键词： 纳米晶吸收剂 烧结温度 溶胶凝胶法     

TiO2·nH2O凝胶预处理对水热合成SrTiO3粉的影响

以TiCl4为钛源,首先制备TiO2.nH2O凝胶,然后在80度的水热条件下制备了SrTiO3粉。利用X射线衍射（XRD）,透射电子显微镜（TEM）和红外光谱（FTIR）研究了TiO2·nH2O凝胶水洗方式,阴离子（Cl^-和NO3－）以及TiO2·nH2O热处理对SrTiO3粉性能的影响。结果表明,水洗和热处理都能使TiO2·nH2O凝胶产生晶化;TiO2·nH2O的 化程度对产物SrTiO3颗粒的粒度和粒度分布有很大影响,以非晶质TiO2·nH2O为钛源制备的SrTiO3颗粒度大且粒度分布宽,以结晶TiO2·nH2O为钛源制备的SrTiO3颗粒粒度小且粒度分布窄,而且可以得到纳米颗粒,水热反应液相中存在Cl^-或NO3^-能使产物SrTiO3颗粒粒度稍有增大,综合以上结果,TiO2·nH2O凝胶水洗对产物颗粒的影响主要是由于使凝胶产生了晶化,布阴离子脱除产生的影响很小,因此,在不考虑阴离子对其它工程化影响（如设备腐蚀等）的前提下,可采用热处理代替水洗。·     

辐照还原法制备Au掺杂MF气凝胶

利用辐照还原法在500 kGy辐照剂量下制备了Au掺杂MF有机气凝胶。通过X射线衍射（XRD）、能量色散光谱仪（EDX）和透射电子显微镜（TEM）测试证实了辐照法成功地制备出Au掺杂MF有机气凝胶复合物。EDX和TEM照片表明辐照处理后Au纳米颗粒均匀地分布在MF气凝胶骨架中,并且Au纳米颗粒的平均尺寸为5.8 nm。N2吸附数据分析表明掺入Au纳米颗粒后,MF气凝胶的比表面积、总孔体积、微孔体积和介孔体积都有所下降。     

纳米级SiO_2玻璃粉制备和测试

采用溶胶-凝胶法制备纳米级SiO2粉，分别用X射线衍射仪、透射电子显微镜、红外光谱仪和差热扫描量热分析仪对其进行了分析测试。结果表明于凝胶在1200℃热处理1小时仍是无定型的SiO2粉，其平均粒度大小为40nm。     

Synthesis and Luminescent Properties of Nano-scale Y2Si2O7:Re3+ (Re=Eu, Tb) Phosphors via Sol-Gel Method

用溶胶凝胶方法制备了稀土离子掺杂的焦硅酸钇纳米粉末，并用XRD对不同温度处理的样品结构进行了表征，结果表明1000 ℃时产物成α-Y2Si2O7相，粒径约为27 nm，且掺杂离子的浓度并不影响样品的结构，测量了Eu3+和Tb3+离子掺杂的样品的激发谱和发射谱，并对其进行了分析．激发谱中真空紫外区对应基质的吸收，紫外区分别对应Tb3+的4f~5d的吸收Eu3+的电荷迁移带的吸收，对发光强度随掺杂离子浓度的变化关系也进行了讨论．对室温下的寿命进行了测量和分析．     

溶胶-凝胶法制备YAG∶Ce,Yb纳米荧光粉及其发光性质研究

使用溶胶-凝胶法在不同煅烧温度下制备了不同掺杂的YAG∶Ce,Yb荧光粉。使用扫描电镜、X射线衍射仪对其形貌、结构进行了表征;采用光致发光、荧光寿命等技术,对其发光性质进行了研究。结果表明:粉体粒径随煅烧温度上升而增大,在1 000℃下,得到平均尺寸~84 nm的纳米荧光粉。溶胶-凝胶法产物与高温固态法产物相比,Yb~(3+)离子发光的猝灭浓度由10%下降至5%。这可能是由于溶胶-凝胶反应产物体系中掺杂离子分布更加均匀所致。     

Study on the Dynamic Rheometry and Swelling Properties of the Polyacrylamide/Laponite Nanocomposite Hydrogels in Electrolyte Media

Polyacrylamide/laponite/chromium triacetate nanocomposite (NC) hydrogels were prepared by incorporation of the laponite nanoparticles in partially hydrolyzed polyacrylamide followed by cross-linking of their aqueous solutions with chromium triacetate. Influence of nanoparticle, cross-linker, polymer concentrations, and gelation media (water) temperature, salinity, and rheometer frequency on the viscoelastic behavior of the NC hydrogels were studied by probing the network properties. In addition, swelling behaviors of these NC gels in tap and oil reservoir water were evaluated. According to dynamic rheometry of the gelation process, the limiting storage modulus of the NC gels increased with increasing laponite content. The addition of laponite into the polyacrylamide gelling system increased their viscous properties more strongly than the elastic properties. The ultimate elastic modulus of the NC gels increased with increasing water salinity and temperature. Increasing rheometer frequency during gelation retarded the sol–gel transition and decreased the ultimate elastic modulus. The equilibrium swelling ratio of the NC hydrogels in tap water decreased with increasing laponite content. The salt sensitivity of the NC gels in oil reservoir water slightly decreased with increasing laponite content. These results suggest the superiority of the hydrolyzed polyacrylamide (HPAM)/chromium acetate/laponite NC hydrogels for water shut-off applications in oil reservoirs as compared with unfilled HPAM gels.     

溶胶-凝胶法制备均相掺钛干凝胶

以溶胶-凝胶法制备掺钛干凝胶,采用冰乙酸控制钛酸四丁酯水解,结合钛源与硅源独立预水解技术制备前体掺钛溶胶和凝胶。考察了溶剂量、抑制剂量和掺钛量对溶胶稳定性和均匀性的影响,以及老化、干燥条件和掺钛量对凝胶均匀性的影响,并优化了工艺参数。结果表明,冰乙酸能够有效地控制钛源水解并改善溶胶均匀性,结合钛源和硅源独立预水解技术,能够可控地制备出掺钛溶胶。在乙醇与醇盐物质的量比为5、冰乙酸与钛酸四丁酯物质的量比为6、钛硅原子数比为2%~20%的条件下可以得到均匀、稳定的溶胶。钛硅原子数比低于10%的溶胶在100℃老化24h,100℃开放条件下干燥24h能够形成均匀的干凝胶。钛硅原子数比高于10%的凝胶在干燥过程中析出氯化钠,得不到均匀的凝胶。     

Preparation and Swelling Behavior of Partially Hydrolyzed Polyacrylamide Nanocomposite Hydrogels in Electrolyte Solutions

In this research, nanocomposite hydrogels were prepared by cross‐linking of partially hydrolyzed polyacrylamide/sodium montmorillonite aqueous solutions with chromium triacetate. The gelation process and influence of nanoclay content and salt concentration on swelling behavior were investigated. Study of gelation behavior using dynamic rheometry method showed that increasing the nanoclay content decreases the storage modulus, due to the partial adsorption of polymer chains onto the clay surface and ionic interaction between negative layers of sodium montmorillonite and Cr.³⁺ By increasing the cross‐linker concentration of the gelation system, the viscous energy dissipation properties of the nanocomposite gel decreases. Swelling ratio of the nanocomposite gels in distilled water decreased as the concentration of the nanoclay increased. However, nanocomposite gels showed lower salt sensitivity in electrolyte media compared with unfilled gels.     

Particle tracking to reveal gelation of hectorite dispersions

Passive microrheological techniques using particle tracking have been developed for the study of the gelation of hectorite suspensions. By following the Brownian motion of the particles, it is possible to determine the increasing caging of the particles with time, as the system gels. Since only the Brownian motion is followed, the gelation process itself should not be affected by the measurement. As gelation proceeds the increasing heterogeneity of the particle environments can be monitored by a variety of measures, including kurtosis. An effective viscosity can be extracted from the measurements and used to indicate the gelation process.     

The structure and properties of titanium oxide nanoheterogeneous films doped with molybdenum oxide

Thin films of titanium oxide nanoparticles doped with molybdenum oxide were synthesized by vacuum cocondensation of titanium atom and molybdenum oxide molecule flows onto a substrate cooled with liquid nitrogen. Atomic-force, scanning tunnel, and scanning electron microscopy were used to study the structure and composition of the films. It was shown that doping caused the formation of a large number of point defects in the titanium oxide lattice and an increase in its specific conductivity. Point defects were three-dimensional F centers and surface hydrate complexes. Tests of films as photoanodes in a photoelectrochemical cell showed that doping of titanium oxide with molybdenum oxide offered promise for increasing the effectiveness of sources for the decentralized production of hydrogen by electrochemical methods.     

Steady state and time resolved laser-induced fluorescence of garlic plants treated with titanium dioxide nanoparticles

The study involves investigation of the effect of the interaction of titanium dioxide nanoparticles with garlic plant by spectroscopy techniques. For this, garlic plants have been grown in the laboratory under controlled conditions of light flux, temperature, humidity, and nutrient media. The growth and biomass parameters in terms of shoot length, fresh, and dry mass are found to increase upon the treatment of titanium dioxide nanoparticles while a reduction is observed in the root length of the garlic plants. The steady state laser-induced fluorescence, time resolved laser-induced fluorescence, and ultraviolet visible spectra of the control and titanium dioxide nanoparticles-treated plants have been acquired. The curve fitting data reveal that titanium dioxide nanoparticles decrease the intensity and fluorescence intensity ratio of red and far red chlorophyll fluorescence bands indicating increase in the photosynthetic activity and chlorophyll content. The evaluation of life time of the excited chlorophyll molecule shows that life time is effected by the treatment of the titanium dioxide nanoparticles. The results pertaining to ultraviolet visible measurement indicate increase in the concentration of chlorophyll a, chlorophyll b, total chlorophyll, carotenoid, and quercetin in the leaves of garlic plants treated with titanium dioxide nanoparticles.     

Ultrasound assisted synthesis of doped TiO2 nano-particles: Characterization and comparison of effectiveness for photocatalytic oxidation of dyestuff effluent

The present work deals with the synthesis of titanium dioxide nanoparticles doped with Fe and Ce using sonochemical approach and its comparison with the conventional doping method. The prepared samples have been characterized using X-ray diffraction (XRD), FTIR, transmission electron microscopy (TEM) and UV–visible spectra (UV–vis). The effectiveness of the synthesized catalyst for the photocatalytic degradation of crystal violet dye has also been investigated considering crystal violet degradation as the model reaction. It has been observed that the catalysts prepared by sonochemical method exhibit higher photocatalytic activity as compared to the catalysts prepared by the conventional methods. Also the Ce-doped TiO₂ exhibits maximum photocatalytic activity followed by Fe-doped TiO₂ and the least activity was observed for only TiO₂. The presence of Fe and Ce in the TiO₂ structure results in a significant absorption shift towards the visible region. Detailed investigations on the degradation indicated that an optimal dosage with 0.8 mol% doping of Ce and 1.2 mol% doping of Fe in TiO₂ results in higher extents of degradation. Kinetic studies also established that the photocatalytic degradation followed the pseudo first-order reaction kinetics. Overall it has been established that ultrasound assisted synthesis of doped photocatalyst significantly enhances the photocatalytic activity.     

Synthesis, characterization and application of iodine modified titanium dioxide in phototcatalytical reactions under visible light irradiation

Iodine doped titanium dioxide has been successfully prepared by simple hydrolysis of tetrabutyl titanate in the presence of iodic acid. The adopted method allowed for the production of spherical iodine doped titaniun dioxide nanoparticles with varied amount of iodine content. Analysis by X-ray diffraction, Raman, transmission electron microscopy as well as UV-vis DRS revealed that titanium dioxide nanostructures were doped with iodine which existed in two different valence states I⁵⁺ and I⁻. The iodine in the form of I⁵⁺ is believed to have doped into the lattice whereas I⁻ was well dispersed on the surface of TiO₂ probably as iodine adducts hence rendering it to be highly absorbing in visible light region. The I-TiO₂ exhibited improved photocatalytic activity toward degradation of acid orange 7 (AO7), methyl orange (MO) and 2,4-dichlorophenol (2,4-DCP) under visible light over the pristine TiO₂ prepared by the same method. High catalytic properties are attributed to iodine doping which led to high specific surface area, absorption in visible region as well as alleviation of charge carrier recombination. The most probable route undertaken in the degradation of AO7 is through indirect oxidation by the hydroxyl radicals.     

Gelation and Swelling Behavior of Semi-Interpenetrating Polymer Network Hydrogels Based on Polyacrylamide and Poly(vinyl alcohol)

Novel semi-Interpenetrating Polymer Network (semi-IPN) hydrogels based on partially Hydrolyzed Polyacrylamide (HPAM) and Poly(Vinyl Alcohol) (PVA) were prepared by solution crosslinking using chromium triacetate. Effects of PVA content on the gelation process and swelling behavior in tap water and different electrolyte solutions were investigated. Study of the gelation behavior using dynamic rheometery showed that the limiting storage modulus of the semi-IPN gels decreased with increasing PVA content. It was also found that increasing the PVA content increases the loss factor, indicating that the viscous properties of this gelling system increase more strongly than the elastic properties. The swelling ratio of the semi-IPN gels in tap water decreased as the concentration of the PVA increased. However, the semi-IPN gels showed lower salt sensitivity factor in synthetic oil reservoir water as compared with HPAM gels. Therefore, they are potentially good candidates for enhanced oil recovery applications.     

Fractal Dimensions of κ-Carrageenan Gels during Gelation and Swelling

A photon scattering technique for research on the sol-gel and gel-sol transitions in κ-carrageenan-water systems with various carrageenan contents (CC) was utilized for characterizing the fractal dimensions during gelation and swelling. It was observed that the scattered photon intensity, I_sc, increased at all temperatures with an increase in the CC when I_sc was monitored against temperature. Additionally, the sol-gel transition temperatures were found to be much lower than the gel-sol transition temperatures, causing hysteresis of the phase transition loops. I_sc increased with an increase in CC at all test temperatures, which is attributed to the formation of a fractal-like carrageenan gel. After drying, the gels were used in swelling experiments where the gels were immersed in water at room temperature, reswelling to the original structure. It was observed that I_sc from the carrageenan gels increased as the CC was increased. The fractal dimension, d, during gelation was found to increase as the gelation temperature was increased. On the other hand, the d values during swelling decreased as the swelling time was increased.