Bonding strength and thermal shock resistance of a novel bilayer (c-AlPO4-SiCw-mullite)/SiC coated carbon fiber reinforced CMCs

Mullite coating, SiC whiskers toughened mullite coating (SiC_w-mullite), and cristobalite aluminum phosphate (c-AlPO₄) particle modified SiC_w-mullite coating (c-AlPO₄-SiC_w-mullite) were prepared on SiC coated C/SiC composites using a novel sol-gel method combined with air spraying. Results show that molten SiO₂ formed by the oxidation of SiC whiskers and molten c-AlPO₄ improved the bonding strength between mullite outer coating and SiC–C/SiC composites due to their high-temperature bonding properties. The bonding strength between mullite, SiC_w-mullite, c-AlPO₄-SiC_w-mullite outer coatings and SiC–C/SiC composites were 2.41, 4.31, and 7.38 MPa, respectively. After 48 thermal cycles between 1773 K and room temperature, the weight loss of mullite/SiC coating coated C/SiC composites was up to 11.61%, while the weight losses of SiC_w-mullite/SiC and c-AlPO₄-SiC_w-mullite/SiC coatings coated C/SiC composites were reduced to 7.40% and 5.12%, respectively. The addition of appropriate SiC whiskers can considerably improve the thermal shock resistance of mullite coating owing to their excellent mechanical properties at high temperature. In addition, c-AlPO₄ particles can further improve the thermal shock resistance of SiC_w-mullite coating due to their high-temperature bonding and sealing properties. No obvious micro-pores and cracks were observed on the surface of c-AlPO₄-SiC_w-mullite coating after 48 thermal cycles due to timely healing effect by formation of secondary mullite.     

Role of electronically coupled in situ grown silver sulfides (Ag2S) nanoparticles with TiO2 for the efficient photoelectrochemical H2 evolution

A solution-processed in situ grown synthesis method has been developed to grow electronically coupled silver sulfide (Ag₂S) nanoparticles (NPs) inside a titanium oxide (TiO₂) thin film. Taking the advantage of better charge transport between Ag₂S and TiO₂, this composite thin film has been utilized for electro-photocatalytic H₂ generation. This thin film growth requires three successive steps, including sol-gel derived ion-conducting thin film fabrication containing loosely bound light ion (Li⁺) followed by ion-exchange (with Li⁺↔Ag⁺) and subsequent sulfurization process. This entire solution-processed deposition technique is capable to fabricate cost-effective large area Ag₂S–TiO₂ thin film containing Ag₂S NPs ranging ~10–70 nm. Since, Ag₂S has a lower band gap and consider as a promising material for photoelectrochemical H₂ generation, therefore Ag₂S (NPs)-TiO₂ thin film is grown on three different substrates, including fluorine-doped tin oxide (FTO), FTO/TiO₂ (sol-gel), and FTO/TiO₂ (NPs) to fabricate photoanode for this study. A comparative photo-electrocatalytic measurement of these three different Ag₂S(NPs)-TiO₂ thin film coated photoanodes showed that sample on FTO/TiO₂ (NPs) substrate generate highest photocurrent of density ~50 mA cm⁻² at 0.5 V vs NHE in 1 M KOH solution which is three orders higher than pure TiO₂ and stable for more than 1.5 h, indicating it's excellent potential application for photoelectrochemical water splitting. The photocurrent generation of this Ag₂S–TiO₂ thin film is significantly higher than earlier reported Ag₂S–TiO₂ system, which is originated due to the reduced carrier recombination from electronically coupled Ag₂S/TiO₂ interface state of such in situ grown Ag₂S NPs.     

溶胶凝胶-液态熔盐静电自组装复合工艺制备cBN@Al核壳粉体

机械混合的cBN和金属Al粉是制备超硬切削刀具的重要原料,因此能有效提高两者接触面积的金属Al包覆cBN的核壳粉体具有潜在的经济价值。提出了一种先将cBN粉体表面羟基化,再通过溶胶-凝胶法对cBN表面进行硅氧纳米层改性,然后在熔融盐条件下包覆金属Al壳层,最后将核壳产物提纯的工艺路线。在不同条件的热处理和不同热处理时间下制备样品,并通过XRD、DSC、SEM、TEM和N_2等温吸附脱附测试,探讨对包覆的影响因素及其机理。结果表明:基于布朗运动和静电自组装机制形成了多孔结构的包覆层,硅氧桥接层、导电熔融盐环境和热处理时间都对包覆Al壳层有重要影响。热处理2 h可获得平均粒径5.7μm和比表面积10.988 m~2/g且含杂质较少的cBN@Al多孔粉末。该项工作为在惰性无机粉末上涂覆活泼的轻金属壳层提供了新的思路。     

Synthesis and Characterization of Microporous ZrO2 Membranes for Gas Permeation at 200°C

The development of gas separation membranes able to work at high temperatures require robust and thin ceramic layers. In this work, zirconia membranes have been prepared by the sol-gel method, following the colloidal sol route. The microporosity and crystallinity of the ZrO₂ material was tested by N₂ adsorption and XRD. The derived active zirconia layers were defect-free as seen by SEM. The optimum firing temperature range was set in the range 400–500°C. He, H₂, CO₂, N₂ gas permeation was conducted at temperatures up to 200°C. High permeances were obtained and the microporosity of the zirconia layer was confirmed.     

尖晶石型铁氧体CaxZn1-xFe2O4的制备及其光催化性能研究

采用改进的溶胶-凝胶法制备CaxZn1-xFe2O4粉体。用X射线粉末衍射仪(XRD)对样品进行结构表征,随着Ca2+掺杂量的增加,样品出现CaFe2O4的衍射峰。使用扫描电子显微镜(SEM)对样品进行形貌表征,结果表明样品的形貌呈不规则的颗粒状,且颗粒大小为2μm,并显现出片层堆叠情况。通过对甲基橙进行光催化降解实验,对CaxZn1-xFe2O4粉体的光催化活性进行了研究。结果表明,经过Ca2+掺杂的CaxZn1-xFe2O4样品,光催化活性明显提高。     

Ion-Exchange Behavior of New and Novel Zirconium(IV)-Based Composite Cation-Exchangers

The synthesized polyaniline-Zr(IV) selenoiodate and polyaniline-Zr(IV) selenomolybdate composite ion exchangers were characterized by Fourier transform infrared spectroscopy, UV spectra, X-ray diffraction, scanning electron microscope, thermogravimetric analysis, and conductivity studies. The ion-exchange capacities, effect of eluent concentration, elution time, elution behavior, and pH on ion-exchange capacity were also studied to exploit the ion-exchange capability of the composites. The study revealed that polyaniline-Zr(IV) selenoiodate and polyaniline-Zr(IV) selenomolybdate ion exchangers are having excellent ion-exchange capacity values for K⁺ ion 1.36 and 1.44?meq?g^?1, respectively. The organic polymeric part of the composites provides mechanical and chemical stability, whereas the inorganic part supports the ion-exchange behavior and thermal stability. The increase in electrical conductivity is due to the inorganic and organic parts. A mechanism for the formation of the polyaniline-Zr(IV) selenoiodate and polyaniline-Zr(IV) selenomolybdate composite ion exchangers is discussed, which may also be applied for the preparation of other composite ion exchangers. Sorption behavior of metal ions on the composites was studied in different solvent systems. On the basis of distribution coefficient values (K_d), it has been found that the cation-exchange materials are highly selective for Pb(II)-ions. Such modified composite materials can be applied as an electrochemically switchable ion exchanger for water treatment, especially water softening.     

Structural and luminescence enhancement properties of Eu3＋/Ag nanocrystallites doped SiO2-TiO2 matrices

We reported here the structural and optical characterisation of silver nanocrystallites/Eu3+ :SiO2-TiO2 matrices synthesised through sol-gel route. Structural characterisations were done by using energy dispersive spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), atomic force microscope (AFM) and transmission electron microscopy (TEM) measurements and optical characterisations were performed by absorption and emission spectroscopy. The TEM and XRD measurements confirmed the presence of nanocrystals. A broad absorption band was observed due to surface plasmon resonance of silver nanocrystals. The effect of silver nanocrystals on the emission spectrum of Eu3+ doped SiO2-TiO2 matrices was discussed. An attempt was made to explain this fluorescence enhancement by invoking phenomena such as energy transfer, asymmetry ratio, surface plasmon, surface roughness, crystallinity and grain boundary. Our analysis, based on the experimental results, suggested that all the phenomena except crystallinity and grain boundary had favourable effects on fluorescence enhancement. We also estimated the relevant parameters associated with the phenomena that affected the fluorescence emission from the Eu3+ ions in the matrix. It was seen that the theoretical estimate of fluorescence enhancement agreed well with the experimental estimate.     

Photocatalytic Self-Cleaning of Wool Fibers Coated with Synthesized Nano-Sized Titanium Dioxide

Nano-sized TiO₂ was successfully synthesized and deposited onto wool fibers using the sol–gel process at ambient temperature. The prepared samples were characterized using several structural, textural, and morphological techniques. The electron micrographs show formation of TiO₂ nanoparticles 10–30 nm in size. The photocatalytic activity of TiO₂-coated wool fibers was investigated through the solid-phase self-cleaning of methylene blue (MB) under UV-vis irradiation by the diffuse reflectance spectroscopy (DRS) method. The fibers' structure is not altered upon light exposure. This preparation technique can also be applied to new fabrics to create self-cleaning and UV irradiation protection properties in them.     

一种超亲水自清洁、智能控温的钨掺杂二氧化钒薄膜的制备及其性能表征

本实验采用一种简单、低成本有效的溶胶-凝胶法制备了热致变色钨掺杂二氧化钒薄膜。首先将乙酰丙酮氧钒和氯化钨置于甲醇溶液中反应制备出前驱体,然后将前驱物旋涂在衬底基材上。最后在氩气氛围中、600 ℃进行退火。同时,对所制备的二氧化钒薄膜进行了XRD、XPS、SEM、UV和WCA等表征和测试。结果表明,钨掺杂二氧化钒薄膜颗粒尺寸范围从30～150 nm,薄膜的表面展现出优异的亲水性,其静态水接触角为12°。根据光学测试,钨掺杂VO₂薄膜表现出优异的光学性能与可见光调节效率(T_lum,s = 80.75%,T_lum,m = 79.24%)和优良的太阳能调节效率(ΔT_sol = 9.10%,T_sol,s = 81.40%,T_sol,m= 72.30%)。VO₂薄膜相变表现出可适用的相变温度:在钨掺杂摩尔量为2%时,其相变温度为32 ℃。