Search results for "Solid"
showing 10 items of 3575 documents
Reactivity of cellulose during hydrothermal carbonization of lignocellulosic biomass
2020
Abstract Hydrothermal carbonization (HTC) of pure cellulose (CE) and birchwood (BW) samples was carried out at temperatures between 160 and 280 °C, 0.5 h residence time and biomass-to-water ratio 1:5, to investigate the reactivity of cellulose in lignocellulosic biomass. Thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR) showed that the CE samples remained unaltered at temperatures up to 220 °C, but were significantly decomposed at 230 °C producing a thermal recalcitrant aromatic and high energy-dense material. FTIR showed that dehydration and aromatization reactions occurred at temperature equal or higher than 230 °C for the CE samples while a similar incre…
Influence of the Preparation Temperature on the Photocatalytic Activity of 3D-Ordered Macroporous Anatase Formed with an Opal Polymer Template
2018
Even if many aspects of three-dimensionally ordered macroporous (3DOM) titania have been extensively studied, the interplay between the amorphous and crystalline components of their skeleton wall has not attracted too much attention, although it should strongly influence the properties of these materials. In order to gain new insight on this interplay, we have studied in detail the wall structure of three 3DOM titania samples prepared by heating the 3DOM titania precursor at 673, 773, and 873 K by X-ray diffraction, thermogravimetric analysis, differential thermal analysis, N2 adsorption/desorption, pore-size distribution, high-resolution transmission electron microscopy, and IHmagic-angle-…
PMMA-titania nanocomposites: Properties and thermal degradation behavior
2012
Titania nanoparticles were prepared using a solegel method and calcination at 200 and 600 � C in order to obtain anatase and rutile phases, respectively. The obtained powders were used to prepare PMMAe titania nanocomposites by a melt compounding method. The effect of the crystalline phase and the amount of titania, in the range 1e5 wt.%, on the morphology, mechanical properties and thermal degradation kinetics of PMMA was investigated by means of X-ray diffractometry (XRD), transmission electron microscopy (TEM), 13 C cross-polarization magic-angle spinning nuclear magnetic resonance spectroscopy ( 13 C{ 1 H}CP-MAS NMR), including the measurement of proton spinelattice relaxation time in t…
Microwave assisted synthesis and solid-state characterization of lithocholyl amides of isomeric aminopyridines
2011
Microwave (MW) assisted synthesis and solid state structural characterizations of novel lithocholyl amides of 2-, 3-, and 4-aminopyridine are reported. It is shown that the MW technique is a proper method in the preparation of N-lithocholyl amides of isomeric aminopyridines. It offers many advantages compared to conventional heating. The molecular and crystal structures as well as the polymorphic and hydrated forms of prepared conjugates with their thermodynamic stabilities have been characterized by means of high resolution liquid- and solid-state NMR spectroscopy, single crystal and powder X-ray diffraction, and thermogravimetric analysis. Owing to the many biological functions of bile ac…
Comparison of Permeation Measurements and Hybrid Density Functional Calculations on Oxygen Vacancy Transport in Complex Perovskite Oxides
2014
The oxygen vacancy (VO••) formation enthalpy (ΔHF) was determined from the effective activation energies obtained in the permeation measurements on a series of solid solutions La0.98–xSrxCo0.2Fe0.8O3−δ (x = 0.125–0.8) and compared with the results of ab initio calculations at finite temperatures based on the hybrid (PBE0) and GGA+U calculations, as well as previous thermogravimetric experiments. The Mulliken atomic charges, magnetic moments, and the Fe-VO•• and Sr-VO•• distances are analyzed. The strong dependence of formation enthalpy of VO•• on the Fe oxidation state due to variation in Sr and VO•• concentrations is discussed.
A Maze of Solid Solutions of Pimobendan Enantiomers: An Extraordinary Case of Polymorph and Solvate Diversity
2017
Over 10 polymorphs and solvatomorphs of the chiral pharmaceutically active ingredient pimobendan were found to lack enantioselectivity in the solid state, accordingly, forming solid solutions of enantiomers, which is reported to be a rare phenomenon. Solid form screening was performed on different enantiomeric composition samples to analyze obtained phases with powder X-ray diffraction and thermogravimetric differential scanning calorimetry. For nonsolvated forms, a melt phase diagram has been constructed convincingly showing the existence of stable and metastable solid solutions near the pure enantiomer and around the racemic composition regions. A crystal structure study combined with sol…
Thermogravimetric and Sorption Measurement Techniques/Instruments
2002
The survey covers commercially offered instruments for the determination of the surface structure of porous solids based on isothermal measurement of physisorption of inert gases and of thermogravimetric instruments. Basic assumptions, features and experimental uncertainties are compared.
A new approach to the synthesis of intermetallic compounds: mild synthesis of submicrometric CoxMy (M = Mo, W; x∶y = 3∶1 and 7∶6) particles by direct…
2002
A simple processing route to cobalt–molybdenum and cobalt–tungsten intermetallics (CoxMy, where M = Mo and W, and x∶y = 3∶1 and 7∶6) has been developed, on the basis of the use of precursors resulting from freeze-drying of aqueous solutions of the appropriate common metal salts. The influence of the preparative variables on the outcomes of this procedure is examined. These compounds are prepared as single phases by thermal reduction of amorphous freeze-dried powders under a hydrogen–argon atmosphere (8% H2), followed by slow cooling of the samples. The materials have been characterised by X-ray powder diffraction, metal analysis, scanning electron microscopy and thermogravimetry under an ox…
Synthesis of new vanadium–chromium and chromium–molybdenum oxynitrides by direct ammonolysis of freeze-dried precursors
2000
Interstitial vanadium–chromium and chromium–molybdenum oxynitrides in the solid solution series V1 − zCrz(OxNy) and Cr1 − zMoz(OxNy) (z = 0.0, 0.2, 0.4, 0.5, 0.6, 0.8, 1.0) have been obtained by direct ammonolysis of precursors resulting from the freeze-drying of aqueous solutions of the appropriate metal salts. A study of the influence of the preparative variables on the outcomes of this procedure is presented. Compounds in the V1 − zCrz(OxNy) series are prepared as single phases by nitridation at 1073 K, followed by fast cooling of the samples. Compounds in the Cr1 − zMoz(OxNy) series are prepared as nearly single phases by nitridation at different temperatures, optimized for each composi…
Nanoporous alumina membranes filled with solid acid for thin film fuel cells at intermediate temperatures
2004
Thin film fuel cells have been fabricated by impregnation of inorganic porous membranes with inorganic proton conductor. Anodic alumina membranes (50 μm thick and pore diameter of 200 nm), filled with CsHSO4 salt have been used as protonic conductor in a hydrogen-oxygen fuel cell working between 423 and 443 K in dry atmosphere. Polarization curves at 433 K showing ohmic control with open circuit values near 0.8 V and short circuit current around 8 mA cm−2 have been obtained. Possible causes of degradation as well as alternative routes to overcome some of the problems encountered with this approach will be reported. Keywords: Solid acid, Anodic alumina membranes, Pore filling, Thin film fuel…