In this investigation, well defined mesoporous zirconia nanoparticles (ZrO2NPs) with cubic, tetragonal or monoclinic pure phase were synthesized via thermal recovery (in air) from chitosan (CS)- or polyvinyl alcohol (PVA)-ZrOxhybrid films, prepared using sol–gel processing. This facile preparative method was found to lead to an almost quantitative recovery of the ZrOx content of the film in the form of ZrO2NPs. Impacts of the thermal recovery temperature (450, 800 and 1100 °C) and polymer type (natural bio-waste CS or synthetic PVA) used in fabricating the organic/inorganic hybrid films on bulk and surface characteristics of the recovered NPs were probed by means of X-ray diffractometry and photoelectron spectroscopy, FT-IR and Laser Raman spectroscopy, transmission electron and atomic force microscopy, and N2sorptiometry. Results obtained showed that the method applied facilates control over the size (6–30 nm) and shape (from loose cubes to agglomerates) of the recovered NPs and, hence, the bulk crystalline phase composition and the surface area (144–52 m2/g) and mesopore size (23–10 nm) and volume (0.31–0.11 cm3/g) of the resulting zirconias.
Herein, we report the synthesis of chromium oxide nanoparticles, α -Cr2O3NPs, followed by full characterization via XRD, SEM, XPS, and N2sorptiometry. The synthesized nanoparticles were tested as catalysts toward the oxidation of CO. The impact of calcination temperature on the catalytic activity was also investigated. CO conversion (%), light-off temperature, T50, data were determined. The results revealed that chromia obtained at low calcination temperature (400 °C) is more active than those obtained at high calcination temperatures (600° or 800 °C) and this is ascribed to the smaller particle size and higher surface area of this sample. The results revealed a superior catalytic activity of Cr2O3NPs at lower temperature as we reached a complete conversion at 200 °C which is high value in the forefront of the published results of other non-noble catalysts. The high activity of Cr2O3nanoparticles (T50as low as 98 °C) where found to be dependent on a careful selection of the calcination temperature. These results may provide effective and economic solutions to overcome one of the major environmental threats.
1 August 2019 in Advances in Colloid and Interface Science
Chitosan‐silica (CSSi) hybrid films have been fabricated by sol‐gel process using tetraethoxysilane (TEOS) as precursor. The structure of the resulting hybrid has been characterized by Fourier transform infrared spectroscopy (FTIR). Fracture surface has been revealed through a field emission‐scanning electron microscopy/energy dispersive spectrometer (FE‐SEM/EDS) to probe the dispersion degree and the size of SiO2 particle. Study of morphology using a SEM micrograph and the High Resolution Transmission Electron Microscopy (HRTEM) images of the nanocomposite films suggests that the SiO2 nanoparticles are within the range of 2–7 nm in diameter and are uniformly dispersed in the polymer matrix. Thermal properties of these composite materials have been studied as a function of silica, indicating that thermal stability of the chitosan film is enhanced. Dynamical mechanical thermal analysis (DMTA) has been carried out to measure the shift in the glass transition temperature (Tg) of the composites from the maxima of the α transition curves. The glass transition temperature and the storage modulus show an increase with increasing silica content. The maximum increase in the Tg value, that is, 159.37∘C, is seen with 30 wt% silica. A gradual increase of 3.0 GPa in the modulus relative to the pure polymer is observed.