Raman Spectrum of Vanadium-Zirconia Yellow Pigment

Monoclinic vanadium-zirconia yellow pigments were prepared by gelling mixtures of zirconium n-propoxide and vanadyl acetylacetone. The nature of interactions between the host ion and the foreign cation in the vanadium-zirconia pigment was investigated in order to contribute to a better understanding of the origin of this pigmenting system using Raman scattering measurements. The Raman spectra of powdered samples of the vanadium-zirconia pigment recorded between 100 and 1400 cm^?1 show the peaks at 991, 701, and 403 cm^?1 assigned to the asymmetric and symmetric stretching and bending vibrations of the V⁴⁺ = O bonds, respectively. The assignment of these peaks was discussed by comparison with Raman spectra of vanadium oxides and on the basis of V-O bond distances deduced from the Hardcastle and Wachs equation and from the valence state of the vanadium cation calculated by Brown in the valence sum rule. This suggests that the V⁴⁺ cations replace Zr⁴⁺ in sevenfold coordinated site in the monoclinic zirconia structure. The V⁴⁺ cation allowing the d-d electronic transition is related to the origin of the lemon yellow coloration.     

Thermal stability of amine-functionalized MCM-41 in different atmospheres

In the present work, we report on the thermal stability of NH₂-MCM-41 hybrid material under different atmospheres (nitrogen and air). The thermal stability of this hybrid material is very important because of its common use in catalysis, adsorption, biomedical and biotechnological applications, based on mesoporous and aminopropyl functionalities. Samples were prepared by one pot co-condensation method with different loadings of 3-aminopropyltriethoxysilane (APTES). The thermal stability of hybrid samples (NH₂-MCM-41) heat treated in nitrogen and air at 30–800 °C has been investigated. Samples were synthesized under basic media in the presence of cetyltrimethylammonium bromide (CTABr) as structure-directing agent, tetraethyl orthosilicate as silica source, and APTES as functionalizing agent with molar composition of 0.055 CTABr:045 SiO₂:0.054 APTES:5.32 NH₄OH:14.99 H₂O at 50 °C for 24 h at pH 12.4. The obtained hybrid materials have been characterized by thermogravimetric analysis (TG), derivative thermogravimetric analysis, differential scanning calorimetry, X-ray powder diffraction, Fourier-transform infrared spectroscopy, transmission electron microscopy, and surface area determination by the BET method. Based on TG measurements of the treated samples, it was found out that the thermal stability varied greatly in different atmospheres.     

The effect of recrystallization time on pore size and surface area of mesoporous SBA-15

Triblock copolymer, pluronic P123 (EO₂₀PO₇₀EO₂₀) was used as the structure directing agent for the simple synthesis and characterization of mesoporous SBA-15 with various porosities. Extending the sample recrystallization time, after the initial synthesis and ageing, seems to have a significant effect on the pore size. It also leads to an increase in the surface area and a narrow pore size distribution. The prepared materials could find applications in areas where the diffusion of large molecules is important, and in catalysis, where greater pore accessibility would enhance the activity and selectivity of the catalyst. A possible mechanism has been proposed to describe the effect of extended recrystallization on pore sizes.     

Thermal stability of Ti–MCM-41

Ti containing mesoporous MCM-41 materials have been synthesized through two methods: heating and non-heating [room temperature (RT)]. The synthesized materials have been characterized using X-ray diffraction, Fourier transform infrared, nitrogen sorption, and X-ray fluorescence methods and their thermal stabilities evaluated using thermogravimetric methods in inert atmosphere. The thermal stabilities have been analyzed based on the synthesis method, as well as on the amount of titanium in the MCM-41 materials. The thermal stability results suggest that uncalcined MCM-41 materials generally show higher mass loss than their calcined counterparts. Also, the RT-synthesized materials showed lower stability than the high-temperature synthesized samples for the uncalcined samples. It is also been found that MCM-41 materials show improved thermal stabilities as the amount of titanium is increased.     

Expanding the synthesis of Stöber spheres: towards the synthesis of nano-magnesium oxide and nano-zinc oxide

In order to synthesise Stöber spheres of different diameters, fixed amounts of ethanol, ammonia and water were used with varying amounts of tetraethyl orthosilicate. This simple method was further applied to the synthesis of nano-ZnO and nano-MgO from their respective precursors, zinc methoxide and magnesium ethoxide. The spherical nano-SiO₂, nano-ZnO and nano-MgO synthesised in this way were characterised by X-ray diffraction, Fourier-transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. Preliminary investigations found that nano-ZnO and nano-MgO showed good catalytic activity in the trans-esterification reaction that converts vegetable oil to biodiesel.