Physical Properties of Silica Aerogels Prepared with Polyethoxydisiloxanes

Silica aerogels were made by sol-gel techniques using industrial silicon derivatives (polyethoxydisiloxanes, E-40), followed by supercritical drying with ethanol. The morphology and microstructure of the silica aerogels were investigated by using specific surface area, S_BET, SEM, TEM and the pore size distribution techniques. The thermal conductivity was also measured as a function of air pressure. The results show that the diameter of the silica particles is about 13 nm and the pore size of the silica aerogels is 20–80 nm. The specific surface area of the silica aerogel is about 470 m²/g and the thermal conductivity of the silica aerogel prepared with E-40 is 0.014 w m^–1 K^–1 at room temperature and 1 atm.     

Effect of Processing Temperature on Gelation and Physical Properties of Low Density TEOS Based Silica Aerogels

In the present paper the experimental results of the effect of sol-gel processing temperature on the physical properties of the TEOS based silica aerogels are reported and discussed. The aerogels were produced by the two step sol-gel process at various temperatures in the range of 26–70^∘;C followed by supercritical drying using methanol solvent extraction. A remarkable reduction in the gelation time was observed from three and a half days at room temperature to a mere 18 hours at 50^∘;C. The best quality aerogels in terms of low density and high optical transmission were obtained for 6 hours hydrolysis time. The aerogels were characterized by the measurements of bulk density, volume shrinkage, porosity, refractive index and optical transmission. Monolithic aerogels with ultra low density (∼0.018 g/cm³), extremely high porosity (∼99%) and optimum optical transmission at 700 nm (∼75%) were obtained for the molar ratio of TEOS:MeOH:acidic water:basic water at 1:99:10.42:14.58 respectively.     

Synthesis and Properties of Hyperbranched Polyimides Combined with Silica

Summary: The novel hyperbranched polyimide - silica hybrid materials containing theoretically 16 wt% of an inorganic phase were prepared via a sol-gel process. An amine terminated polyimide precursor (hyperbranched polyamic acid) was prepared from commercially available monomers 4,4′,4″-triaminotriphenylmethane and 4,4′-oxydiphthalic anhydride in molar ratio 1:1. Tetramethoxysilane and/or 3-glycidoxypropyltrimethoxysilane (also used as a coupling agent) were used as silica precursors. During thermal exposition the polyimide precursor was transformed to hyperbranched polyimide and hydrolyzed alkoxy groups reacted mutually to form silica. The final products were self-standing films, whose structure was characterized by using IR and ¹³C and ²⁹Si solid state NMR spectroscopy. The influence of the amount of silica and/or coupling agent on their structure and thermal properties was described.     

Sol-Gel Fabrication and Properties of Silica Cores of Optical Fibers Doped with Yb3+, Er3+, Al2 O3 or TiO2

Optical cores of preforms for drawing optical fibers doped with Er3+ and Yb3+ were fabricated by the sol-gel method with the aim of increasing the thickness of glass layers coated in a single coating cycle and to determine the relation between the preparation conditions and optical properties of the fibers. Al2O3-P2O5-SiO2 and TiO2-P2O5-SiO2 glasses have been studied as matrices for entrapping the rare-earth elements. Input sols have been prepared from silicon and titanium alkoxides, AlCl3, ErCl3, YbCl3, POCl3, water and a modifier under acidic catalysis of HCl. The sols were coated on the inner wall of a silica substrate tube and the gel layers were sintered at high temperatures up to 2000°C after which the tube was collapsed into the preform. Continuous and homogenous glass films with the maximum thickness of about 8 m were fabricated. The influence of high-temperature heat treatment of the layers on their composition and optical attenuation was observed. The amplified stimulated emission of Er3+ around 1.55 m was measured under the excitation of the fibers by an Nd : YAG laser at 1.064 m.     

Optical and Structural Properties of Doped ZnS Nanoparticles Produced by the Sol-Gel Method

Optical and structural properties of Mn2+-doped ZnS nanoparticles in an organic matrix are experimentally and theoretically studied. The nanoparticles, which were produced by the sol-gel method, are nearly monodisperse with a diameter of approximately 3 nm and show the characteristic orange-red luminescence of Mn2+ centers in a crystalline ZnS matrix. The absorption spectrum of the embedded ZnS nanoparticles is slightly blue shifted and broadened compared to the reference system containing ZnS microparticles. This blue shift is caused by quantum size effects, whereas the broadening is due to defects such as lattice distortions, and vacancies, which are probably located close to the surface in the case of small particles. With increasing temperature the absorption spectra shift to the red and are broadened due to thermal activated diffusion of ions close to the surface. In contrast, the spectral feature of the emission spectra via the Mn2+ center is nearly unchanged compared to the ZnS microparticles. Furthermore, the quantum efficiency is increased and the decay time of the electron-hole pairs is shortened to the nanosecond regime because of the enhanced probability of the electron-hole pairs to see the Mn2+ center. Therefore, the only effect of doping of ZnS nanoparticles with Mn2+ center is the suppression of the relaxation of electron-hole pairs via surface defects generating a highly efficient and fast relaxation of the electron-hole pairs via the Mn2+ center.     

Physical,Thermal and Biological Properties of Yellow Dyes with Two Azodiphenylether Groups of Anthracene

Two yellow bis-azo dyes containing anthracene and two azodiphenylether groups (BPA and BTA) were prepared, and an extensive investigation of their physical, thermal and biological properties was carried out. The chemical structure was confirmed by the FTIR spectra, while from the UV–Vis spectra, the quantum efficiency of the laser fluorescence at the 476.5 nm was determined to be 0.33 (BPA) and 0.50 (BTA). The possible transitions between the energy levels of the electrons of the chemical elements were established, identifying the energies and the electronic configurations of the levels of transition. Both crystals are anisotropic, the optical phenomenon of double refraction of polarized light (birefringence) taking place. Images of maximum illumination and extinction were recorded when the crystals of the bis-azo compounds rotated by 90° each, which confirms their birefringence. A morphologic study of the thin films deposited onto glass surfaces was performed, proving the good adhesion of both dyes. By thermal analysis and calorimetry, the melting temperatures were determined (~224–225 °C for both of them), as well as their decomposition pathways and thermal effects (enthalpy variations during undergoing processes); thus, good thermal stability was exhibited. The interaction of the two compounds with collagen in the suede was studied, as well as their antioxidant activity, advocating for good chemical stability and potential to be safely used as coloring agents in the food industry.     

Preparation and Optical Properties of Sb2S3 Microcrystallite Doped Silica Glasses by the Sol-Gel Process

The sol-gel process has been applied to the preparation of nano-size Sb2S3 crystallite doped silica glasses and thin films. Silica glasses containing 1–1.5 wt% Sb2S3 are prepared by hydrolysis of complex solution of Si(OC2H5)4, SbCl3 and SC(NH2)2, and subsequent heat treatment. The nano-size crystallite in the matrix is observed by means of TEM. The transmission spectra of the films show that the transmission valley shifts toward longer wavelengths with increasing heat treatment time and temperature. Second harmonic generation (SHG) has been observed in the glasses illuminated with intense 1.06 m and frequency-doubled laser beams from mode-locked Nd:YAG laser.     

氧化钇掺杂块状SiO_2气凝胶的制备与表征

以正硅酸四乙酯(TEOS)为前驱体,YCl3·6H2O为掺杂剂,采用溶胶-凝胶法并结合CO2超临界干燥工艺得到了块状Y2O3-SiO2气凝胶,其中Y2O3掺杂含量控制在5wt%~30wt%范围内。利用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、比表面积测定(BET)、X射线荧光分析(XRF)等测试手段对样品进行表征。结果表明:经过氧化钇掺杂后得到的Y2O3-SiO2气凝胶,不仅维持了SiO2气凝胶原有的空间网络结构,而且具有更高的热稳定性,经过900℃热处理2 h后,10wt%Y2O3(0.447 g的YCl3·6H2O)掺杂的Y2O3-SiO2气凝胶仍然处于无定形态,平均孔径约为21.3 nm,比表面积高达643.8 m2·g-1。     

氧化钇掺杂块状SiO2气凝胶的制备与表征

以正硅酸四乙酯（TEOS）为前驱体,YCl₃·6H₂O为掺杂剂,采用溶胶-凝胶法并结合CO₂超临界干燥工艺得到了块状Y₂O₃-SiO₂气凝胶,其中Y₂O₃掺杂含量控制在5wt%~30wt%范围内。利用扫描电镜（SEM）、透射电镜（TEM）、X射线衍射（XRD）、比表面积测定（BET）、X射线荧光分析（XRF）等测试手段对样品进行表征。结果表明：经过氧化钇掺杂后得到的Y₂O₃-SiO₂气凝胶,不仅维持了SiO₂气凝胶原有的空间网络结构,而且具有更高的热稳定性,经过900℃热处理2h后,10wt%Y₂O₃（0.447g的YCl₃·6H₂O）掺杂的Y₂O₃-SiO₂气凝胶仍然处于无定形态,平均孔径约为21.3nm,比表面积高达643.8m₂·g^-1。     

Impact of Chemical and Physical Properties of Organic Solvents on the Gas and Hydrogen Formation during Laser Synthesis of Gold Nanoparticles

Laser ablation in liquids has been established as a scalable preparation method of nanoparticles for various applications. Particularly for materials prone to oxidation, it is established to suppress oxidation by using organic solvents as a liquid medium. While this often functionalizes the nanoparticles with a carbon shell, the related chemical processes that result from laser-induced decomposition reactions of the organic solvents remain uncertain. Using a systematic series of C₆ solvents complemented by n-pentane and n-heptane during the nanosecond laser ablation of gold, the present study focuses on the solvent-dependent influence on gas formation rates, nanoparticle productivity, and gas composition. Both the permanent gas and hydrogen formation was found to be linearly correlated with ablation rate, ΔH_vap, and pyrolysis activation energy. Based on this, a decomposition pathway linked to pyrolysis is proposed allowing the deduction of first selection rules for solvents that influence the formation of carbon or permanent gases.     

Synthesis and Characterisation of Polyvinyl alcohol (PVA)/Silica Hybrid Composites Derived Through the Sol-Gel Method in Aqueous Medium: Effect of Acid Content,Silica Content and Viscosity of PVA on the Dispersion Characteristics of Silica and the Physical Properties of the Composites

A cheap and environment friendly route towards the synthesis of Polyvinyl alcohol/silica hybrid composites is presented. Polyvinyl alcohol/silicate hybrid materials were synthesised in aqueous medium by the sol-gel method using dil HCl (0.5 N) as catalyst and a cost-effective silica source sodium silicate. The synthesis method was aimed at enhancing the rate of co-condensation of silica within the polyvinyl alcohol matrix. Transparent and flexible hybrid films of homogenous thickness were obtained after gelation at 45°C for 24 h and extended drying for another 48 h. The hybrid composites were characterised by fourier transform infrared spectroscopy (FTIR), scanning electron microscopoy (SEM), thermogravimeric analysis (TGA), tensile strength, elongation at break and water uptake measurements. SEM micrographs revealed that silica was dispersed in the PVA matrix without the large aggregation of particles for a molar composition of 0.0004 PVA:0.048 Sodium silicate: 0.004 HCl.     

Optical and Electrical Properties of the PLT Films with Various Compositions Deposited by Sol-Gel Process

In order to study optical and electrical properties of (Pb_1-xLa_x)TiO₃ (PLT) films with varying La concentration, the PLT films were deposited by sol-gel process. X-ray diffraction revealed that a pseudocubic phase of the PLT film became dominant with increasing La concentration due to decrease of lattice constant of c-axis. Three-dimensional atomic force microscopy images showed that the grain size and root mean square surface roughness decreased by addition of La. The optical band gap of the PLT films became wider when Pb was substituted with La. The addition of La increased the transparency of the PbTiO₃ film and shifted the threshold for initiation of absorption to shorter wavelength. Hysteresis loops of the PLT films showed that remanent polarization and coercive field decreased with increasing La concentration. In addition, we modified the surface of the PLT film with La concentration of 5% using a keV oxygen ion beam at different doses. The optical band gap of the PLT film was changed by the oxygen ion beam irradiation although the XRD patterns and the transmittance values were not significantly changed. In measuring AFM images of the surface of modified PLT film, significant changes of the grain shape and size were not found. Moreover, polarization and dielectric constant were not changed after oxygen ion irradiation. These results suggested that addition of La could affect the optical and electrical properties of the PbTiO₃ and PLT films and that surface modification by oxygen ion beam modification with 1 keV energy can change the surface property but not bulk property.     

Conductance and Thermodynamic Study of the Complexation of Ethyl p-Tert-butylcalix[4]arene Tetraacetate with Alkali Metal and Silver Ions in Various Solvents

The first conductometric studies for the complexation reactions between alkali metaland silver cations with ethyl p-tert-butylcalix[4]ester in the cone conformation using acetonitrile and methanol in the temperature range 278–303 K are reported. The observed molar conductivities were found to decrease significantly for mole ratios less than unity. The conductivity data were analysed using a computer program based upon 1 : 1 stoichiometry. Stability constants of the resulting 1 : 1 complexes were determined, indicating that the sequence of stability in acetonitrile is Na⁺ > Li⁺ > K⁺. The H⁰ and S⁰ values of the calix[4]ester complexation reactions were determined from the temperature dependence of the complexation constants, and their significance are discussed.     

ChemInform Abstract: Temperature and Bias Effects on the Physical and Tribological Properties of Diamond-Like Carbon.

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