Abstract: Magnesium containing boron compounds with hexagonal structure have been drawn much attention due to their superconductive nature. The main target of this work is new modified microwave oven by on our own has an ability about passing through a gas in the oven medium for attainment of oxygen-free compounds such as c-BN. Mg containing boride was synthesized by modified-microwave method under nitrogen atmosphere using amorphous boron and magnesium source in appropriate molar ratio. Microwave oven with oxygen free environment has been modified to aimed to obtain magnesium boride without oxygen. Characterizations were done by powder X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. Mg containing boride, generally named magnesium boride, with amorphous character without oxygen is obtained via designed microwave oven system.
Abstract: The catalytic oxidation of CO and volatile organic compounds (VOCs) is considered as one of the most efficient ways to reduce harmful emissions from various chemical industries. The effectiveness of gold-based catalysts for many reactions of environmental significance was proven during the past three decades. The aim of this work was to combine the favorable features of Au and Cu-Ce mixed oxides in the design of new catalytic materials of improved efficiency and economic viability for removal of air pollutants in waste gases from formaldehyde production. Supported oxides of copper and cerium with Cu: Ce molar ratio 2:1 and 1:5 were prepared by wet impregnation of g-alumina. Gold (2 wt.%) catalysts were synthesized by a deposition-precipitation method. Catalysts characterization was carried out by texture measurements, powder X-ray diffraction, temperature programmed reduction and electron paramagnetic resonance spectroscopy. The catalytic activity in the oxidation of CO, CH3OH and (CH3)2O was measured using continuous flow equipment with fixed bed reactor. Both Cu-Ce/alumina samples demonstrated similar catalytic behavior. The addition of gold caused significant enhancement of CO and methanol oxidation activity (100 % degree of CO and CH3OH conversion at about 60 and 140 oC, respectively). The composition of Cu-Ce mixed oxides affected the performance of gold-based samples considerably. Gold catalyst on Cu-Ce/γ-Al2O3 1:5 exhibited higher activity for CO and CH3OH oxidation in comparison with Au on Cu-Ce/γ-Al2O3 2:1. The better performance of Au/Cu-Ce 1:5 was related to the availability of highly dispersed gold particles and copper oxide clusters in close contact with ceria.
Abstract: Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters. After a successful synthesis of Nd2Zr3(MoO4)9 which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).
Abstract: Colemanite is the most common borate mineral, and the main source of the boron required by plants, human, and earth. Transition metals exhibit optical and physical properties such as; non-linear optical character, structural diversity, thermal stability, long cycle life and luminescent radiation. The doping of colemanite with a transition metal, bring it very interesting and attractive properties which make them applicable in industry. Iron doped calcium borate was synthesized by conventional solid state method at 1200 °C for 12 h with a systematic pathway. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS) were used to characterize structural and morphological properties. Also, thermal properties were recorded by thermogravimetric-differential thermal analysis (TG/DTA).
Abstract: One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO3 (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La0.8Sr0.2MnO3/Zr0.92Y0.08O2 (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10-1 S/cm at 600 oC with 0.22 eV activation energy.
Abstract: Cadmium oxide (CdO) nanoparticles have been
prepared by chemical coprecipitation method. The synthesized
nanoparticles were characterized by X-ray diffraction analysis
(XRD), scanning electron microscopy (SEM), transmission electron
microscopy (TEM), UV analysis, and dielectric studies. The
crystalline nature and particle size of the CdO nanoparticles were
characterized by Powder X-ray diffraction analysis (XRD). The
morphology of prepared CdO nanoparticles was studied by scanning
electron microscopy. The particle size was studied using the
transmission electron microscopy (TEM).The optical properties were
obtained from UV-Vis absorption spectrum. The dielectric properties
of CdO nanoparticles were studied in the frequency range of 50 Hz–5
MHz at different temperatures. The frequency dependence of the
dielectric constant and dielectric loss is found to decrease with an
increase in the frequency at different temperatures. The ac
conductivity of CdO nanoparticle has been studied.
Abstract: The 1:1 cocrystal of 2-amino-4-chloro-6-
methylpyrimidine (2A4C6MP) with 4-methylbenzoic acid (4MBA)
(I) has been prepared by slow evaporation method in methanol,
which was crystallized in monoclinic C2/c space group, Z = 8, and a
= 28.431 (2) Å, b = 7.3098 (5) Å, c = 14.2622 (10) Å and β =
109.618 (3)°. The presence of unionized –COOH functional group in
cocrystal I was identified both by spectral methods (1H and 13C
NMR, FTIR) and X-ray diffraction structural analysis. The
2A4C6MP molecule interact with the carboxylic group of the
respective 4MBA molecule through N—H⋯O and O—H⋯N
hydrogen bonds, forming a cyclic hydrogen–bonded motif R2
2(8).
The crystal structure was stabilized by Npyrimidine—H⋯O=C and
C=O—H⋯Npyrimidine types hydrogen bonding interactions.
Theoretical investigations have been computed by HF and density
function (B3LYP) method with 6–311+G (d,p)basis set. The
vibrational frequencies together with 1H and 13C NMR chemical
shifts have been calculated on the fully optimized geometry of
cocrystal I. Theoretical calculations are in good agreement with the
experimental results. Solvent–free formation of this cocrystal I is
confirmed by powder X-ray diffraction analysis.
Abstract: Cesium molybdates with general formula
CsMIII(MoO4)2, where MIII = Bi, Dy, Pr, Er, exhibit rich
polymorphism, and crystallize in a layered structure. These properties
cause intensive studies on cesium molybdates. CsBi(MoO4)2 was synthesized by microwave method by using
cerium sulphate, bismuth oxide and molybdenum (VI) oxide in an
appropriate molar ratio. Characterizations were done by x-ray
diffraction (XRD), fourier transform infrared (FTIR) spectroscopy,
scanning electron microscopy/energy dispersive analyze (SEM/EDS),
thermo gravimetric/differantial thermal analysis (TG/DTA).
Abstract: The first laboratory synthesis of hard materials such as
diamond proceeded to attack of developing materials with high
hardness to compete diamond. Boron rich solids are good candidates
owing to their short interatomic bond lengths and strong covalent
character. Boron containing hard material was synthesized by modifiedmicrowave
method under nitrogen atmosphere by using a fuel
(glycine or urea), amorphous boron and/or boric acid in appropriate
molar ratio. Characterizations were done by x-ray diffraction (XRD),
Fourier transform infrared (FTIR) spectroscopy, scanning electron
microscopy/energy dispersive analyze (SEM/EDS), thermo
gravimetric/differential thermal analysis (TG/DTA).
Abstract: This article presents summary on preparation and
characterization of zinc, copper, cadmium and cobalt chromite
nanocrystals, embedded in an amorphous silica matrix. The
ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2
nanocomposites were prepared by a conventional sol-gel method
under acid catalysis. Final heat treatment of the samples was carried
out at temperatures in the range of 900−1200 ◦C to adjust the
phase composition and the crystallite size, respectively. The resulting
samples were characterized by Powder X-ray diffraction (PXRD),
High Resolution Transmission Electron Microscopy (HRTEM),
Raman/FTIR spectroscopy and magnetic measurements. Formation
of the spinel phase was confirmed in all samples. The average size of
the nanocrystals was determined from the PXRD data and by direct
particle size observation on HRTEM; both results were correlated.
The mean particle size (reviewed by HRTEM) was in the range from
∼4 to 46 nm. The results showed that the sol-gel method can be
effectively used for preparation of the spinel chromite nanoparticles
embedded in the silica matrix and the particle size is driven by the
type of the cation A2+ in the spinel structure and the temperature
of the final heat treatment. Magnetic properties of the nanocrystals
were found to be just moderately modified in comparison to the bulk
phases.
Abstract: L-asparagine admixture Paranitrophenol (LAPNP) single crystals were grown successfully by solution method with slow evaporation technique at room temperature. Crystals of size 12mm×5 mm×3mm have been obtained in 15 days. The grown crystals were Brown color and transparent. The solubility of the grown samples has been found out at various temperatures. The lattice parameters of the grown crystals were determined by X-ray diffraction technique. The reflection planes of the sample were confirmed by the powder X-ray diffraction study and diffraction peaks were indexed. Fourier transform infrared (FTIR) studies were used to confirm the presence of various functional groups in the crystals. UV–visible absorption spectrum was recorded to study the optical transparency of grown crystal. The nonlinear optical (NLO) property of the grown crystal was confirmed by Kurtz–Perry powder technique and a study of its second harmonic generation efficiency in comparison with potassium dihydrogen phosphate (KDP) has been made. The mechanical strength of the crystal was estimated by Vickers hardness test. The grown crystals were subjected to thermo gravimetric and differential thermal analysis (TG/DTA). The dielectric behavior of the sample was also studied
Abstract: The mineral having chemical compositional formula MgAl2O4 is called “spinel". The ferrites crystallize in spinel structure are known as spinel-ferrites or ferro-spinels. The spinel structure has a fcc cage of oxygen ions and the metallic cations are distributed among tetrahedral (A) and octahedral (B) interstitial voids (sites). The X-ray diffraction (XRD) intensity of each Bragg plane is sensitive to the distribution of cations in the interstitial voids of the spinel lattice. This leads to the method of determination of distribution of cations in the spinel oxides through XRD intensity analysis. The computer program for XRD intensity analysis has been developed in C language and also tested for the real experimental situation by synthesizing the spinel ferrite materials Mg0.6Zn0.4AlxFe2- xO4 and characterized them by X-ray diffractometry. The compositions of Mg0.6Zn0.4AlxFe2-xO4(x = 0.0 to 0.6) ferrites have been prepared by ceramic method and powder X-ray diffraction patterns were recorded. Thus, the authenticity of the program is checked by comparing the theoretically calculated data using computer simulation with the experimental ones. Further, the deduced cation distributions were used to fit the magnetization data using Localized canting of spins approach to explain the “recovery" of collinear spin structure due to Al3+ - substitution in Mg-Zn ferrites which is the case if A-site magnetic dilution and non-collinear spin structure. Since the distribution of cations in the spinel ferrites plays a very important role with regard to their electrical and magnetic properties, it is essential to determine the cation distribution in spinel lattice.
Abstract: Solid dispersions (SD) of curcuminpolyvinylpyrrolidone
in the ratio of 1:2, 1:4, 1:5, 1:6, and 1:8 were
prepared in an attempt to increase the solubility and dissolution.
Solubility, dissolution, powder X-ray diffraction (XRD), differential
scanning calorimetry (DSC) and Fourier transform infrared
spectroscopy (FTIR) of solid dispersions, physical mixtures (PM)
and curcumin were evaluated. Both solubility and dissolution of
curcumin solid dispersions were significantly greater than those
observed for physical mixtures and intact curcumin. The powder
X-ray diffractograms indicated that the amorphous curcumin was
obtained from all solid dispersions. It was found that the optimum
weight ratio for curcumin:PVP K-30 is 1:6. The 1:6 solid dispersion
still in the amorphous from after storage at ambient temperature for 2
years and the dissolution profile did not significantly different from
freshly prepared.