Mesoporous silica with pore sizes of 3–6 nm has been synthesized under refluxing and autogenous pressure conditions of hydrothermal synthesis from precursor gels having different alkaline pH. The mesoporous silica prepared is characterized by powder X-ray diffraction, nitrogen adsorption-desorption measurement and scanning electron microscopy. Thermal stability has been tested by XRD analysis of mesoporous silica after thermal treatment at 823 K, 6 h; 1023 K, 1 h and 1223 K, 1 h. The results indicate that the mesoporous silica prepared under refluxing condition from precursor gel of pH 11 has large surface area (ca.1103 m2 g− 1) and pore volume (ca. 0.868 cm3 g− 1) and is thermally stable at 1223 K. The surface area, pore volumes and pore wall thickness increase as the pH of the precursor gel is increased for refluxing condition of synthesis. The comparison of textural properties revealed that the refluxing condition is advantageous over autogenous pressure condition for obtaining mesoporous silica with higher surface area (852 m2 g− 1), pore volume (0.894 cm3 g− 1) and pore diameter > 4 nm with wall thickness of 1.59 nm, when synthesized from precursor gel of pH 9.2. The 29Si NMR spectra showed that a great part of the Si atoms exists as silanol groups. The mesoporous silica made at the lower pH (9.2) under refluxing conditions have more condensed framework. In calcined mesoporous silica, the proportion of partly condensed silica (Q3) is higher than fully condensed silica (Q4). 相似文献
Polyaniline/mesoporous silica hybrids were prepared by chemical modification with aniline and their capacitances were examined for application to electrode of electrochemical capacitor. The chemical modification was performed by two kinds of processes, polymer insertion into pores and in-situ polymerization within pores. In the case of the polymer insertion process, since the mean pore sizes of the hybrid did not change, polyaniline molecules were not inserted. On the other hand, in the case of the in-situ polymerization process, the mean pore sizes decreased from that of mesoporous silica, while the XRD patterns became broad. Therefore, aniline molecules polymerized in the inside of pores, however, the mesoporous silica collapsed in part. Maximum capacitance measured in 1 mol/l H2SO4 aqueous solution was around 226 F per unit mass of polyaniline. 相似文献
Barium strontium titanate (Ba0.05Sr0.95TiO3) ferroelectric thin films have been prepared on single crystal [001] MgO substrates using the pulsed laser deposition method. The X-ray diffraction (XRD) analysis show the films were oriented with the [001] direction perpendicular to the plane of the substrate. The refractive index of Ba0.05Sr0.95TiO3 is determined from model fitting with the calculated data of the reflectivity of Ba0.05Sr0.95TiO3 in the wavelength 1450-1580 nm at the room temperature. The dispersion curve decreases gradually with increasing wavelength. The average value of the refractive index is found to be 1.985 in the wavelength 1450-1580 nm which is important for optoelectronic device applications. 相似文献
Hybrid optical films of TiO2‐triethoxysilane‐capped polythiourethane (TCPTU) with high refractive indices have been prepared via an in situ sol‐gel method. The high refractive index triethoxysilane‐capped polythiourethane (TCPTU) was synthesized by polyaddition of the triethoxysilane‐modified trimercaptothioethylamine (TMTEA) and 2,2′‐dimercaptoethylsulfide (MES) with 2,4‐tolylene diisocyanate (TDI). The titania content in the hybrid films can be adjusted from 0 to 80 wt.‐% by the feed ratio of titania precursor [Ti(OBu)4] to polymer (TCPTU). Both FTIR and DSC analyses indicate that there is chemical bonding between the titania domain and the polymer chain. TGA results suggest that the titania of high content was successfully incorporated into polymer matrices and this series of hybrid films have good thermal properties. AFM measurements indicate that in the hybrid films the titania domains are of nanosize scale and the domain size averagely decreases from 60–80 nm to 5–20 nm with increasing content of titania, and the variation of surface roughness for the hybrid films has the same trend. These may be relative to the content of TCPTU and the interaction between titania and polymer (TCPTU). The refractive indices of the hybrid films at 632.8 nm increased from 1 632 to 1 879 as the titania content varied from 0 to 80 wt.‐%.
A series of hexagonal mesoporous silica (HMS) have been synthesized by the neutral assemble pathway in water-alcohol cosolvent systems, using dodecylamine (DDA) and tetraethyl orthosilicate (TEOS) as the starting materials. These materials were characterized with powder X-ray diffraction, nitrogen sorption measurement, differential thermal analysis, and transmission electron microscopy. The XRD patterns of these samples exhibited a strong intense reflection at low angle, suggesting the excellent mesostructures of the samples. The particle size of HMS decreased and the morphology of HMS exhibited high textural porosity as the HMS was prepared with high addition rate of TEOS. The particle size of HMS prepared without aging was smaller than that aged for 18 h, due to the reaction time of TEOS was not enough to form complete particles. Addition of NaCl and HCl hindered the formation of HMS mesoporous structure. In contrast, addition of 1-butanol did not affect the formation of HMS mesoporous structure. The sphereical HMS silica with uniform size has been synthesized by adjusting DDA and TEOS concentrations. The shape of HMS became larger and more spherical as the concentrate on of DDA decreased. The stirring rate of the reaction mixture had no effect on either the shape or the size of the spheroid HMS silicas. However, the particles started to crack at higher stirring rates. 相似文献
