Structural and Morphological Characterization of Pt/WO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>–ZrO<Subscript>2</Subscript> Catalysts

Abstract  Catalysts of Pt/WO _x –ZrO₂ type with 1 wt% of Pt and 10, 15 and 20 wt% of tungsten were synthesized and characterized. The structural and morphological features of these catalysts were studied. The samples were synthesized by impregnation method and calcined at 600 °C, 700 °C and 800 °C. The characterizations were carried out using different techniques: X-ray diffraction, Raman spectroscopy, scanning electronic microscopy, nitrogen adsorption measurement and refinement of their crystalline structures by Rietveld method. X-ray diffraction patterns revealed the formation ZrO₂ and WO₃ crystalline structures and its crystallite size were determined. The zirconium oxide crystallized into tetragonal and monoclinic phases and tungsten trioxide crystallized into monoclinic phase. Crystalline WO₃ and amorphous WO _x species were detected by Raman spectra. Index Abstract  Catalysts of Pt/WO _x –ZrO₂ type with 1 wt% of Pt and 10, 15 and 20 wt% of tungsten were synthesized and characterized. The structural and morphological features of these catalysts were studied. The samples were synthesized by impregnation method and calcined at 600 °C, 700 °C and 800 °C. The characterizations were carried out using different techniques: X-ray diffraction, Raman spectroscopy, scanning electronic microscopy, nitrogen adsorption measurement and refinement of their crystalline structures by Rietveld method. X-ray diffraction patterns revealed the formation ZrO₂ and WO₃ crystalline structures and its crystalline size were determined. The zirconium oxide crystallized into tetragonal and monoclinic phases and tungsten trioxide crystallized into monoclinic phase. Crystalline WO₃ and amorphous WO _x species were detected by Raman spectra.     

Preparation and characterization of indium doped tin oxide (ITO) via a non-aqueous sol-gel

ABSTRACT

Tin-doped indium oxide (ITO) nanoparticles (NPs) were conceived as promising materials using as noncarbon support for Pt NPs on the cathode side of Proton Exchange Membrane Fuel Cells (PEMFC). In this paper, ITO nanoparticles have been synthesized via a nonaqueous sol-gel process using indium acetylacetonate and tin bis(acetylacetonate)dichloride in oleyamine as starting materials. The ITO exhibits solid solution phase, relatively porous, good crystallinity with a uniform size of 15–20 nm, resulting in a high specific surface area and excellent conductivity. The effects of reaction temperature, calcination temperature on the specific surface area as well as the conductivity of ITO nanoparticles were studied in this paper. We found that the ITO nanoparticles synthesized at 235°C and calcination temperature at 500°C for 3 hours shows the excellent conductivity of 1.242 S/cm, was significantly ～8-fold higher than that of commercial ITO produced by Sigma-Aldrich (0.15 S/cm). The results of this research suggested that the ITO synthesized by non-aqueous sol-gel process exhibits relatively good properties as well as can apply this process to prepare the others nanomaterial support based on In₂O₃-materials by doping different oxide into indium oxide.     

Crystal Structure and Vibrational Spectra of Erbium Trisodium Bis(Cyclotriphosphate) Nonahydrate,ErNa<Subscript>3</Subscript>(P<Subscript>3</Subscript>O<Subscript>9</Subscript>)<Subscript>2</Subscript> · 9H<Subscript>2</Subscript>O

Abstract The cyclotriphosphate salt, ErNa₃(P₃O₉)₂ · 9H₂O, has been characterized by single-crystal X-ray diffraction [hexagonal, space group , with unit cell parameters of a = b = 30.8451(14), c = 12.8063(8) ?; Z = 18]. The structure consists of alternating layers of [P₃O₉]³⁻ groups, ErO₈ dodecahedra, Na(1)O₆ and Na(2)O₇ polyhedra linked together by water molecules. The P₃O₉ rings are grouped along the c-axis in a P₃O₉–ErO₈ arrangement thereby producing broad, hexagonal channels of diameter of 6.65 ? with a side dimension of 3.907 ?. The absence of coincidences for the majority of the IR and Raman bands observed for the cyclotriphosphate salt is in accord with the centrosymmetric structure of the material. The vibrational spectra have been interpreted on the basis of factor group effects. Graphical abstract We report the crystal structure and vibrational spectra of erbium trisodium bis(cyclotriphosphate)nanohydrate salt ErNa ₃ (P ₃ O ₉ ) ₂ · 9H ₂ O H. Assaaoudi, M. Ijjaali, A. Ennaciri, I. S. Butler* and J. A. Kozinski Crystal structure and vibrational spectra of erbium trisodium bis(cyclotriphosphate) nonahydrate,ErNa₃(P₃O₉)₂ · 9H₂O. Projection of the coordination polyhedra of ErNa₃(P₃O₉)₂ · 9H₂O down the c axis     

Structural and electrical properties of lead-free perovskite ceramic: Ba(In1/2Nb1/2)O3

Lead-free perovskite Ba(In_1/2Nb_1/2)O₃ was prepared by conventional ceramic fabrication technique at 1350 °C/5 h in air atmosphere. The crystal symmetry, space group and unit cell dimensions were determined from Rietveld analysis using FullProf software whereas crystallite size and lattice strain were estimated from Williamson-Hall approach. XRD analysis of the compound indicated the formation of a single-phase cubic structure with the space group Pm3m. EDAX and SEM studies were carried out in order to evaluate the quality and purity of the compound. Complex impedance as well as electric modulus analyses suggested the dielectric relaxation to be of non-Debye type. The correlated barrier hopping (CBH) model was employed to successfully explain the mechanism of charge transport in Ba(In_1/2Nb_1/2)O₃.     

Synthesis and Photocatalytic Properties of TiO2 Intercalated H4Nb6O17

Abstract

TiO₂ intercalated H₄Nb₆O₁₇ has been synthesized by the reactions of H₄Nb₆O₁₇ with a titanyl acylate complex followed by UV irradiation. The gallery height, specific surface area and Ti content of the sample synthesized by using titanyl acylate complex were larger than that using TiO₂ sol solution. Furthermore, the photocatalytic activity of the TiO₂ pillared H₄Nb₆O₁₇ prepared using a titanyl acylate precursor was twice larger than that fabricated using a TiO₂ sol solution.     

Addition effects of bismuth oxide on Samaria-doped ceria based lithium carbonate composite electrolytes for intermediate temperature-solid oxide fuel cells

ABSTRACT

The effect of amounts (3, 5, 10, 20 wt%) of Bi₂O₃ on the sintering characteristics and porosity of Samaria-doped Ceria (SDC) based Lithium carbonate has been evaluated. The density had a maximum as high as 98.5% of theoretical density at 800°C with only 1wt%Li₂CO₃ and 3 wt%Bi₂O₃. The composite electrolytes showed high ion conductivity at evaluated temperatures. Composition and calcination temperature were found to affect the morphology and conductivity of the composite electrolytes greatly. The total conductivity closed to 3 orders of magnitude greater than pure SDC at operating temperature of 900°C and 3.5 orders of magnitude greater than pure SDC at operating temperature of 600°C. Especially, the best sample containing 3 wt% Bi₂O₃ sintered at 800°C for 2 h which had an ionic electrical conductivity of 0.17S cm^?1. According to fuel cell performance, these composite electrolytes are chemically stable, which is an attractive prospect in intermediate temperature solid oxide fuel cell applications.     

The effect of Zn-acetate molar variation on phase formation and photocatalytic degradation activity of Fe3O4/ZnO core-shell nanocomposite

Abstract

The aim of this research is to investigate the photodegradation of Methylene Blue with Fe₃O₄/ZnO core-shells. Fe₃O₄/ZnO core-shells were synthesized by a simple two-step chemical method (co-precipitation and precipitation) using a molar variation of Zn-acetate precursor. We found that the presence of Fe₂O₃ plays an important role in enhancement of photocatalytic activity due to the existence of higher concentration of surface oxygen vacancies and the suppressing effect of the Fe²⁺ ions on the recombination of photoinduced electron-hole pairs. The core-shell photocatalyst can be easily separated by using a commercial magnet without reduces photocatalytic efficiency within three times of recycling process.     

Fabrication of Al2O3 Coatings on Metal Substrates by Electrophoretic Deposition by the Addition of Polydimethylsiloxane-Based Organic-Inorganic Hybrid Materials as Binders

Polydimethylsiloxane (PDMS)-based organic-inorganic hybrids have been studied because of their high dielectric strength, heat resistivity, and flexibility. In this study, we fabricated Al₂O₃ coatings on metal substrates with sufficient electrical insulation, heat conductivity, and thermal stability by electrophoretic deposition (EPD) using PDMS-based hybrid binders. The scratch hardness, thermal conductivity, and electrical breakdown strength of the Al₂O₃ coating before and after heat treatment at 300 °C for 500 h were 2.0 N, 3.1 W/mK, and 60 kV/mm, respectively. These results demonstrate the usefulness of EPD using PDMS-based hybrid binders for fabricating flexible heat dissipative substrates used in high-temperature environments.     

Electrical properties of Bi3.15Nd0.85Ti2.8-xZr0.2MnxO12 thin films with different Mn content synthesized by chemical solution deposition (CSD)

Bi_3.15Nd_0.85Ti_2.8-xZr_0.2Mn_xO₁₂ (BNTZM) thin films with various Mn content (x = 0, 0.005, 0.01, 0.03, and 0.05) have been prepared on Pt/Ti/SiO₂/Si (100) substrates by a chemical solution deposition (CSD) technique. The crystal structures of BNTZM thin film have been analyzed by X-ray diffraction (XRD). The dependence of Mn contents on the ferroelectric, dielectric properties, and leakage current of these BNTZM films have been thoroughly investigated. The XRD analysis demonstrated that all the BNTZM thin films were of typical bismuth-layer-structured ferroelectrics (BLSF) polycrystalline structure and exhibited a highly preferred (117) orientation. Among these BNTZM films, the BNTZM thin film with Mn content equal to 0.01 exhibits the maximum remnant polarization (2P_r) of 48μC/cm² and a low coercive field (2E_c) of 177 kV/cm. In addition, the BNTZM thin film with x = 0.01 (Mn) showed a fatigue-free behavior up to 1 × 10¹⁰ read/write cycles.     

Enhanced persistent photoconduction in CuInS2–ZnIn2S4 alloys single crystals and processes of its relaxation

ABSTRACT

Photoelectrical response in CuInS₂–ZnIn₂S₄ alloys single crystals was analysed in the low temperature region from 30 K up to 100 K. The molar ratio of ZnIn₂S₄ in the alloys was varied in the range 0 mol%?16 mol%. The crystals with up to 12 mol% were the single-crystalline, meanwhile those with 16 mol% were the two phase ones. We have analysed spectral distribution of their photocurrent at different temperatures and the following relaxation towards the stationary values. The photo-induced photoconductivity phenomena were identified. Moreover the long-lasting relaxations with characteristic times exceeding 1.5×10³ sec were observed at lowest temperatures. They used to shorten exponentially with increasing temperature showing thermally activated behaviour. The main parameters of the photoconductivity kinetics and their temperature dependencies were determined. The observed behaviour was explained by the slow multicenter recombination due to the combined effect of different trapping and recombination centers. The effects of both – “fast” and “slow” recombination centers were taken into account.     

Structural and magnetic properties of nanometric Zn0.5Co0.5Fe2O4 prepared by hydrothermal method

ABSTRACT

The study of the structural, morphology and magnetic properties of Zn_0.5Co_0.5Fe₂O₄ ferrite is the objective of this work. The sample was prepared by hydrothermal method and was characterized by X-ray diffraction (XRD), (SEM) and (TEM) micrographs and magnetization measurements.

The magnetic hysteresis loops, field cooling (FC) and zero field cooling (ZFC) curves, in temperature range (0-400K), were measured using XL-SQUID magnetometer and the values of blocking temperatures (T_B) were determined. The results indicated that Zn_0.5Co_0.5Fe₂O₄ sample were formed in a single spinel phase and gives the value for the lattice parameter (8.3952 Å) and nanosizes of particles (13.8 nm) were compared with these obtained from ZnFe₂O₄ sample prepared also by synthesis method (8.4261 Å and 14 nm). Although, the superparamagnetic behaviour for Co-Zn ferrite has observed at 350K with a blocking temperature (T_B = 300K), that is maximum at the value obtained in the case of Zn-ferrite (T_B = 12K).     

Transport and Electrochemical Properties of Bi2Sr2CaCu2O8 Superconductors

Abstract

Electrical conductivity and thermoelectric power measurements (77–300K) of both the pure and electrochemically doped with lithium Bi₂Sr₂CaCu₂O₈ system, are presented. Clear correlation between transport and electrochemical properties of Li_xBi₂Sr₂CaCu₂O₈ was shown.     

Preparation and Characterization of [Zn(H2O)6][Zn2V10O28(H2O)10]?·?6H2O Single Crystals with a Novel Metallic Heteropolyoxoanion

Abstract  The compound investigated in this study contains a novel centrosymmetric heteroanion [Zn₂V₁₀O₂₈(H₂O)₁₀]²⁻. This cluster results from the connection between a V₁₀O₂₈ group and two Zn(2)O(OH₂)₅ octahedra. The Zn(1)O₆ octahedron and three water molecules associated with it are located between the different layers. The [Zn(H₂O)₆][Zn₂V₁₀O₂₈(H₂O)₁₀] · 6H₂O compound belongs to P-1 space group, with a = 8.967(2) ?, b = 10.390(4) ?, c = 12.338(13) ?, α = 108.31(7)°, β = 100.68(7)°, γ = 103.00(3)°, V = 1022(1) ?³ and Z = 1. Refinement gave R = 0.035 and wR(F²) = 0.098 for 3837 unique observed reflexions [I > 2σ(I)]. Index Abstract  The compound investigated in this study contains a novel centrosymmetric heteroanion [Zn₂V₁₀O₂₈(H₂O)₁₀]²⁻. This cluster results from the connection between a V₁₀O₂₈ group and two Zn(2)O(OH₂)₅ octahedra.      

Intercalation of O2 and its Effect on the Properties of C60 and C70 Solids

Abstract

The intercalation of O₂ in C₆₀ and C₇₀ solids have been studied. In both gas effusion spectra of C₆₀ and C₇₀ powder exposed to O₂ at room temperature, two evolution peaks of O₂ are found near 80 and 150°C. In both C₆₀ and C₇₀ powder, the peak near 80°C does not depend on a heating ratio and the peak near 150°C shifts to higher temperature with the heating ratio. The activation energy on diffusion of O₂ in C₆₀ and C₇₀ solids are ～0.27eV and ～0.46eV, respectively. The number of O₂ intercalated in C₇₀ powder is larger than that in C₆₀ powder. Electron spin density of 02-intercalated C₆₀ film is larger than that of C₇₀ film. The effect on the properties of C₆₀ and C₇₀ solids by the intercalation of O₂ are discussed.     

Crystal structure, vibrational spectra, and thermal decomposition and nitrogen adsorption behaviour of a new tetramanganese(II) dipyrophosphate decahydrate, Mn4(P2O7)2·10H2O

A new manganese(II) pyrophosphate, Mn₄(P₂O₇)₂·10H₂O, has been synthesized and characterized by single-crystal X-ray diffraction [orthorhombic space group Pnma, with unit cell parameters of a=9.3288(3) ?, b=25.9532(9) ?, c=8.4783(3) ?; Z=4]. All the pyrophosphate anions show non-linear P–O–P bonds with an average angle of 128.60°. The framework of this new pyrophosphate is made up of packed layers of MnO₆ octahedra connected by double-tetrahedra P₂O₇ groups and a layer of Mn(H₂O)₆ units. The [P₂O₇]⁴⁻ anions adopt a bent, near-staggered conformation. The absence of coincidences for the majority of the IR and Raman bands is in accord with the centrosymmetric structure of the material. The vibrational spectra have been interpreted in part on the basis of factor group effects. The structural changes occurring during heating have been investigated by TG-ATD. When Mn₄(P₂O₇)₂ ^.10H₂O is gradually heated, it decomposes into an intermediate hydrated salt at 96°C and then to anhydrous Mn₂P₂O₇ at 325°C. This thermal behaviour is different from that of Zn₄(P₂O₇)₂·10H₂O. The crystal structure of the new managenese(II) pyrophosphate is compared with the known structures of Zn₄(P₂O₇)₂·10H₂O, Mn₂P₂O₇·2H₂O and anhydrous Mn₂P₂O₇. The adsorption and desorption isotherms of Mn₄(P₂O₇)₂·10H₂O, Zn₄(P₂O₇)₂·10H₂O and MnKHP₂O₇·2H₂O have been investigated by BET measurements and the results show that the capacity for N₂ sorption of the Mn(II) salt is two times lower than is that of the Zn(II) isotype and two or three times higher than is that of MnKHP₂O₇·2H₂O.     

A novel Zn(II) coordination polymer based on tetra-carboxylates ligand and N-donor ligand: synthesis,structure and photocatalytic properties

Abstract

Novel film polymeric composites based on the non-photoconducting polyvinyl butyral with heterometallic complexes (NH₄)_4n{[Cu(en)(H₂O)][P₂Mo₅O₂₃]}_n·3.5nH₂O (1) and (NH₄)_2n{[Cu(en)₂][Cu(en)(H₂O)][P₂Mo₅O₂₃]}_n·3nH₂O (2) [en?=?ethylenediamine] have been prepared. Both compounds are similar and contain Strandberg anions [P₂Mo₅O₂₃]^6– linked to Cu-diamine species. The main structural difference between complexes is the presence of additional bridging [Cu(en)₂] fragments in 2, which provide an extra connectivity between the neighboring polyoxometalates. However, the different saturations and relaxation times of the photoresponse, as well as different activation energies, are shown. The variability of the photoconducting properties can be explained by the influence of a chain rigidity on the transport of non-equilibrium charge carriers.     

X-Ray diffractometry of metamorphic nanoheterostructures

Elastic strains in active regions of metamorphic transistor nanoheterostructures In_0.7Al_0.3As/In_0.7Ga_0.3As/In_0.7Al_0.3As on GaAs substrates with a metamorphic buffer (MB) having different complex designs have been determined by X-ray diffractometry. The objects of study are linear-graded MBs with different thicknesses, including those with internal strain-balanced superlattices or internal inverse steps, and a step-graded MB. All MBs are completed with an inverse step. The experimental results are compared with model predictions for hypothetical linear-graded MBs with the same average compositional gradients as for the samples under study.     

Investigation of the structure evolution process in sol-gel derived CaO-B2O3-SiO2 glass ceramics

A sol-gel method was used to prepare CaO-B₂O₃-SiO₂ (CBS) glass powder for making low-temperature cofired ceramics. This paper was focused on the mechanism of hydrolysis and polymerization and also on the structural evolution of xerogel at various temperatures. The xerogel was transformed into glass ceramics containing CaSiO₃ and CaB₂O₄ crystalline phases through nucleation and crystallization processes. The results indicated that the xerogel exhibits [BO₄] or [SiO₄] based three-dimensional network structure whose interstices Ca ions fill in, which becomes more orderly and stable after heat treatments. The CBS glass ceramics through controlled crystallization have a potential as electronic packaging materials.     

Synthetic nanodiamonds (SNDs) containing bimetallic Ni(Co)–Fe composites: preparation,characterization and catalytic performance in the reaction of CO2 methanation

Abstract

In this article, we present the preparation, characterization, and catalytic performance of bimetallic Co₉₃Fe₀₇ and Ni₈₀Fe₂₀ active mass loaded on synthetic nanodiamonds (SNDs) in the carbon dioxide (CO₂) methanation. The pristine SNDs possessing a developed specific surface are thermally stable and inert to the reaction mixture of CO₂ and dihydrogen. However, it is shown that 100% conversion of CO₂ into methane can be reached at the lower temperature than that for a massive Co₉₃Fe₀₇ or Ni₈₀Fe₂₀ catalyst when 20?wt.% of the catalyst mass was loaded on the surface of SNDs. The catalytic activity of the prepared bimetallic/SNDs composites is estimated as the minimum temperature at the maximum conversion of CO₂ at atmospheric pressure: it is 325 and 290?°C for Co₉₃Fe₀₇/SNDs and Ni₈₀Fe₂₀/SNDs, respectively. Thermal desorption studies showed that the methanation over Co-Fe/SNDs and Ni-Fe/SNDs catalysts run through the stage of CO₂ dissociation into carbon and oxygen atoms and their subsequent interaction with hydrogen to form methane and water molecules. Scanning electron microscopy studies have shown that the presence of transition metal-rich sites on the surface of the carrier contributes to the improvement of efficiency of the Ni₈₀Fe₂₀ catalyst action.     

Effect of alkaline earth oxides on ceramization of LaF3 in aluminosilicate glass: F MAS-NMR study

Local environment of fluorine atoms in the lanthanum oxyfluoride aluminosilicate glasses and glass-ceramics modified by alkaline earth oxides, i.e. MgO, CaO and BaO, was studied by solid state ¹⁹F MAS-NMR spectroscopy. The effect of the type and concentration of the modifier on the formation of crystalline LaF₃ phase was determined, as a function of heat treatment conditions. In all series of glasses studied, the F-Me(n), but no Na-F species were observed. The presence of F-La,Ba(n) units, in which fluorine is coordinated both by lanthanum and barium, was detected in the Ba-glass. Supplementary XRD analysis of this series confirmed that an increase of barium contents leads to the formation of Ba_0.3La_0.7O_0.7F_1.3, instead of pure LaF₃ only.