Synthesis of (1 − x)Ca2/5Sm2/5TiO3-xLi1/2Nd1/2TiO3 ceramic powder via ethylenediaminetetraacetic acid precursor

(1 − x)Ca_2/5Sm_2/5TiO₃-xLi_1/2Nd_1/2TiO₃ (CSLNT) ceramic powder was prepared by a liquid mixing method using ethylenediaminetetraacetic acid (EDTA) as the chelating agent. TG, DTA, XRD and TEM characterized the precursors and derived oxide powders. When x = 0.3, perovskite CSLNT was synthesized at 1000 °C for 3 h in air. The CSLNT (x = 0.3) ceramics sintered at 1200 °C for 3 h show excellent microwave dielectric properties of ?_r = 99, Q_f = 6200 GHz and τ_f = 9 × 10⁻⁶ °C⁻¹.     

A non-solvent approach for high-stiffness all-cellulose biocomposites based on pure wood cellulose

All-cellulose composites are commonly prepared using cellulose solvents. In this study, moldable all-cellulose I wood fiber materials of high cellulose purity (97%) were successfully compression molded. Water is the only processing aid. The material is interesting as a “green” biocomposite for industrial applications. Dissolving wood fiber pulps (Eucalyptus hardwood and conifer softwood) are used and the influence of pulp origin, beating and pressing temperature (20–180 °C) on supramolecular cellulose nanostructure is studied by solid state CP/MAS ¹³C NMR. Average molar mass is determined by SEC to assess process degradation effects. Mechanical properties are determined in tensile tests. High-density composites were obtained with a Young’s modulus of up to 13 GPa. In addition, nanoscale cellulose fibril aggregation was confirmed due to processing, and resulted in a less moisture sensitive material.     

Die drawn wood polymer composites. II. Micromechanical modelling of tensile modulus

The Cox–Krenchel micromechanical model was applied to give predictions for the tensile moduli of isotropic and oriented wood polymer composites (WPC). The oriented WPC were produced by the Leeds die-drawing process using polypropylene filled with softwood and hardwood powders. The wood particles were extracted from the composites to determine their density and aspect ratio by dissolving in hot decalin. To measure particle shape and size, image analysis was employed. These experimental parameters were then introduced to the Cox–Krenchel model which was found to give prediction of tensile modulus in very good agreement with the experimental values.     

Preparation and properties of negative thermal expansion Zr2WP2O12 ceramics

Using solid-state reaction method, Zr₂WP₂O₁₂ powder was synthesized for this study. The optimum heating condition was 1200 °C for 4 h. The obtained powder was compacted and sintered. The relative density of the Zr₂WP₂O₁₂ ceramics with no sintering additive was 60%. That of samples sintered with more than 0.5 mass% MgO was about 97%. The average grain size (D₅₀), as estimated from the polished surface of a sample sintered at 1200 °C for 4 h was about 1 μm. The obtained ceramics showed a negative thermal expansion coefficient of about −3.4 × 10⁻⁶ °C⁻¹. Young's modulus, Poisson's ratio, three-point bending strength, Vickers microhardness, and fracture toughness of the obtained ceramics were, respectively, 74 GPa, 0.25, 113 ± 13 MPa, 4.4 GPa and 2.3 MPa m^1/2.     

Study on properties of CaO-SiO2-B2O3 system glass-ceramic

Low temperature co-fired ceramic (LTCC) is prepared by sintering a glass selected from CaO-SiO₂-B₂O₃ system, and its sintered bodies are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). It is found that the optimal sintering temperature for this glass-ceramic is 820 °C for 15 min, and the major phases of this material are CaSiO₃, CaB₂O₄ and SiO₂. The glass-ceramic possesses excellent dielectric properties: ?_r = 6.5, tan δ < 2 × 10⁻³ at 10 MHz, temperature coefficient of dielectric constant about −51 × 10⁻⁶ °C⁻¹ and coefficient of thermal expansion about 8 × 10⁻⁶ °C⁻¹ at 20-400 °C. Thus, this material is supposed to be suitable for the tape casting process and be compatible with Ag electrode, which could be used as the LTCC materials for the application in wireless communications.     

Elaboration, by tape casting, and thermal characterization of a solid oxide fuel half-cell for low temperature applications

In the past years, a major interest has been devoted to decrease the working temperature of solid oxide fuel cell (SOFC) down to about 700 °C. In this respect, materials with a high ionic conduction at intermediate temperature have to be found and the processes to elaborate fuel cells, using these new materials, have to be developed.Apatite materials (La_10−xSr_x(SiO₄)₆O_2±δ) are attractive candidates for solid electrolyte working at intermediate temperature. The ceramic powder was produced by solid state reaction and was tape cast to obtain green sheets.Concerning the cathode, a perovskite oxide (La_1−xSr_xMn_1−yCo_yO_3−δ) has been chosen. The perovskite powder was also shaped by tape casting with the introduction of a pore forming agent (corn-starch) to obtain the required porosity in the sintered cathode.The co-firing of the electrolyte/cathode half-cell in air at 1400 °C-2 h gives a flat sample with a dense apatite (98.2%), a 42.7% porous cathode and neither delamination nor chemical reactivity between electrolyte and cathode materials.The dimensional behaviour of the electrolyte material is stable for an oxygen partial pressure ranging from 10⁻¹⁰ to 0.21 atmosphere, from room temperature to 700 °C. The thermal expansion coefficients of the electrolyte and cathode materials are rather close (Δα = 2.8 × 10⁻⁶ K⁻¹) under air.     

Tropical wood polymer nanocomposite (WPNC): The impact of nanoclay on dynamic mechanical thermal properties

In this study, wood polymer nanocomposites (WPNCS) were manufactured from five Malaysian tropical wood species by vacuum-impregnation attended by in situ polymerization using phenol–formaldehyde resin and montmorillomite nanoclay. Percentage weight gain and density of wood polymer nanocomposites depended on wood species. Thermo-mechanical properties of wood samples were investigated by the dynamic mechanical thermal analysis (DMTA) over the temperature range of −100 °C to 200 °C. The intrinsic properties of the components, morphology of the system and the nature of interface between the phases were also determined through DMTA test. Storage modulus (E′) of WPNC samples exhibited significant improvement over the temperature range, in both glassy region and rubbery plateau in relation to their corresponding raw wood samples and wood polymer composites (WPCs). Furthermore, damping (loss tan δ) peaks of all wood species were lowered by PF-Nanoclay system treatment, an indication of improved surface interphase of wood. Dynamic Young’s modulus (E_d) of wood was also calculated using free–free vibration testing. A significant increment was obtained for the PF-Nanoclay impregnated WPNC samples.     

Thermal expansion coefficient of ZnSe crystal between 17 and 1080 °C by interferometry

The thermal expansion of ZnSe was measured by Fabry-Perot interferometry from 17 to 1080 °C during the heat-up of a seeded crystal growth experiment of ZnSe. The measured thermal expansion follows the two-step heating schedule very well. A single linear interpolation between the measured thermal expansion at 17 and 1080 °C gives a value for the thermal expansion coefficient, a as 4.95 × 10^− 6 °C^− 1. The estimated errors associated with a give its range of 4.60 to 4.99 × 10^− 6 °C^− 1.     

Thermal stability and transport studies of (100 − 2x)TeO2-xAg2O-xWO3 (7.5 ≤ x ≤ 30) glass system

Differential scanning calorimetry (DSC), infrared (IR) and direct current (DC) conductivity studies have been carried out on (100 − 2x)TeO₂-xAg₂O-xWO₃ (7.5 ≤ x ≤ 30) glass system. The IR studies show that the structure of glass network consists of [TeO₄], [TeO₃]/[TeO₃₊₁], [WO₄] units. Thermal properties such as the glass transition (T_g), onset crystallization (T_o), thermal stability (ΔT), glass transition width (ΔT_g), heat capacities in the glassy and liquid state (C_pg and C_pl), heat capacity change (ΔC_p) and ratios C_pl/C_pg of the glass systems were calculated. The highest thermal stability (237 °C) obtained in 55TeO₂-22.5Ag₂O-22.5WO₃ glass suggests that this new glass may be a potentially useful candidate material host for rare earth doped optical fibers. The DC conductivity of glasses was measured in temperature region 27-260 °C, the activation energy (E_act) values varied from 1.393 to 0.272 eV and for the temperature interval 170-260 °C, the values of conductivity (σ) of glasses varied from 8.79 × 10⁻⁹ to 1.47 × 10⁻⁶ S cm⁻¹.     

Synthesis of nanocrystalline magnesium titanate by an auto-igniting combustion technique and its structural, spectroscopic and dielectric properties

Nanocrystalline magnesium titanate was synthesized through an auto-ignited combustion method. The phase purity of the powder was examined using X-ray diffraction, thermo gravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy and Raman spectroscopy. The transmission electron microscopy study showed that the particle size of the as-prepared powder was in between 20 and 40 nm. The nanopowder could be sintered to 98% of the theoretical density at 1200 °C for 3 h. The microstructure of the sintered surface was examined using scanning electron microscopy. The dielectric constant (?_r) of 16.7 and loss factor (tan δ) of the order of 10⁻⁴ were obtained at 5 MHz when measured using LCR meter. The quality factor (Q_u × f) 73,700 and temperature coefficient of resonant frequency (τ_f) −44.3 ppm/°C, at 6.5 GHz are the best reported values for sintered pellets obtained from phase pure nanocrystalline MgTiO₃ powder.     

Low temperature photoluminescence and infrared dielectric functions of pulsed laser deposited ZnO thin films on silicon

C-axis oriented ZnO thin films were grown on silicon (100) and (111) substrates by pulsed laser deposition. Low temperature photoluminescence spectra show besides the peaks of free excitons, of defect bound excitons, and of a donor-acceptor pair transition a new doublet at 3.328/3.332 eV. The doublet seems to originate from the columnar textured ZnO film structure. A corresponding structural dependence of the broadening parameter of the infrared dielectric functions was derived from spectroscopic ellipsometry in the spectral range from 380 to 1200 cm^− 1. The wave numbers of the E₁ transverse optical and A₁ longitudinal optical phonon modes of the ZnO films on silicon are determined to be 406 and 573 cm^− 1, respectively. These values are slightly smaller than those of single-crystalline ZnO thin films on sapphire.     

Preparation, structure and dielectric properties of Ba4LaMNb3O15 (M = Ti, Sn ) ceramics

Two new cation-deficient hexagonal perovskites Ba₄LaMNb₃O₁₅ (M = Ti, Sn) ceramics were prepared by high temperature solid-state reaction route. The phase and structure of the ceramics were characterized by X-ray diffraction, scanning electron microscopy (SEM). The microwave dielectric properties of the ceramics were studied using a network analyzer. The Ba₄LaTiNb₃O₁₅ has high dielectric constant of 52, high quality factors (Q) 3500 (at 4.472 GHz), and temperature variation of resonant frequency (τ_f) +93 ppm °C⁻¹ at room temperature; Ba₄LaSnNb₃O₁₅ has dielectric constant of 39 with high Q value of 2510 (at 5.924 GHz), and τ_f −29 ppm °C⁻¹.     

Forming behavior and workability of 6061/B4CP composite during hot deformation

Compression tests of 6061/B₄C_P composite have been performed in the compression temperature range from 300 °C to 500 °C and the strain rate range from 0.001 s⁻¹ to 1 s⁻¹. The flow behavior and processing map have been investigated using the corrected data to elimination of effect of friction. The processing maps exhibited two deterministic domains, one was situated at the temperature between 300 °C and 400 °C with strain rate between 0.003 s⁻¹ and 0.18 s⁻¹ and the other was situated at the temperature between 425 °C and 500 °C with strain rate between 0.003 s⁻¹ and 0.18 s⁻¹.The estimated apparent activation energies of these two domains, were 129 kJ/mol and 149 kJ/mol, which suggested that the deformation mechanisms were controlled by cross-slip and lattice self-diffusion respectively. The optimum parameters of hot working for the experimental composite were 350 °C - 0.01 s⁻¹ and 500 °C - 0.01 s⁻¹. In order to exactly predict dangerous damaging mechanism under different deformation conditions exactly, Gegel’s criterion was applied to obtain processing map in the paper. The result showed that the processing map used Gegel’s criterion can be effectively to predict the material behavior of the experimental composite.     

Materials with layered structures XIII: electrical and optical properties of layered chalcogenides in the system CoIn2S4-CoIn2Se4

The system CoIn₂S_4xSe_4(1−x) has been investigated by X-ray powder methods on samples quenched at 700 °C. The spinel type phase has a phase width of 1≥x>0.9. A new layered compound is formed for 0.9>x>0.45 which crystallizes with the α-FeGa₂S₄-type with a=392.6 pm and c=1270.3 pm (x=0.5) for the hexagonal cell. Platelike crystals of the layered phase are obtained by transport reactions with iodine in a temperature gradient 750→700 °C. The band gaps of these crystals measured by optical absorption vary from 1.2 to 1.4 eV. The electrical conductivities of the crystals are found in the order of 10⁻⁵ Ω⁻¹ cm⁻¹.     

Piezoelectric and ferroelectric properties of K0.5Na0.5NbO3 ceramics synthesized by spray drying method

Potassium-sodium niobate was synthesized at 800 °C for 1 h using dried precursors in a powder form obtained by the spray drying method. Different samples were sintered from 1060 to 1120 °C for 2 h reaching a relative density as high as 96% of the theoretical value. Piezoelectric and ferroelectric properties were studied for these samples and some of the most prominent results are: k_p, d₃₁, 2P_r, and 2E_C of 0.36, 39 pC/N, 29 μC/cm² and 16.5 kV/cm, respectively, for the sample sintered at 1080 °C. The methodology presented in this study can be used to synthesize submicrometer powders.     

Hydrothermal synthesis and study of an inorganic-organic hybrid vanadate of a nickel(II) coordination complex with pyrazine, Ni3(C4H4N2)3(V8O23)

The three-dimensional hybrid compound Ni₃(C₄H₄N₂)₃(V₈O₂₃) has been synthesized by mild hydrothermal methods under autogenous pressure at 170 °C. The structure of the phase is stable until 380 °C. The removal of the pyrazine molecules from the structure induces its collapse. The IR spectrum shows the vibration modes of the pyrazine molecule and those of the [VO₄]³⁻ groups. A UV-visible spectrum shows the characteristic bands of the Ni(II) d⁸-high-spin cation in a slightly distorted octahedral coordination. Magnetic measurements indicate the existence of antiferromagnetic interactions that can be fitted with a chain model to give g = 2.31, J/k = −5.3, and zJ′/k = −5.5.     

Synthesis and characterization of a new organic dihydrogen phosphate-arsenate: [H2(C4H10N2)][H2(As, P)O4]2

Chemical preparation, crystal structure, calorimetric and spectroscopic investigations (IR and RMN) are given for a new non-centrosymmetric organic-cation dihydrogen phosphate-arsenate [H₂(C₄H₁₀N₂)][H₂(As, P)O₄]₂. This compound is triclinic P1 with the following unit-cell parameters: a = 7.082(2) Å, b = 7.796(1) Å, c = 12.05(3) Å, α = 95.37(2)°, β = 98.38(3)°, γ = 62.98(1)°, Z = 2, V = 586.2(1) Å³ and D_x = 1.836 g cm⁻³. The crystal structure has been solved and refined to R = 0.03 using 2328 independent reflections. The structure can be described as infinite (H₂XO)_n chains spreading parallel to the b direction. These chains are themselves interconnected by a set of NH?O hydrogen bonds generated by the organic entities, alternating with the chains. Solid-state ¹³C, ¹⁵N and ³¹P MAS NMR spectroscopies are in agreement with the X-ray structure.     

Investigation of SmBaCuCoO5+δ double-perovskite as cathode for proton-conducting solid oxide fuel cells

SmBaCuCoO_5+δ, a double-perovskite oxide, was synthesized by the modified Pechini method and developed as cathode material for proton-conducting solid oxide fuel cells. The SmBaCuCoO_5+δ powders calcined at 800 °C, show the double-perovskite structure in powder XRD pattern. SmBaCuCoO_5+δ has a more suitable thermal expansion coefficient than SmBaCo₂O_5+δ for BaCe_0.7Zr_0.1Y_0.2O_3−δ electrolyte-based solid oxide fuel cells. The single cell was tested with humidified hydrogen (∼3% H₂O) as the fuel and static air as the oxidant. The performance of the cell was characterized by DC Electronic Load and AC impedance spectroscopy. The peak power densities reached 355-86 mW cm⁻² in the range of 700-550 °C and the interfacial polarization resistance decreased with increasing operation temperature, from 3.1 Ω cm² at 550 °C to 0.22 Ω cm² at 700 °C. The high power density and low polarization demonstrate that SmBaCuCoO_5+δ is a potential candidate for proton-conducting solid oxide fuel cells.     

Transport characteristics of ZrO2 dispersed mixed (BaCl2)1−x-(KCl)x solid electrolytes

Composite solid electrolytes in the system [(BaCl₂)_1−x:(KCl)_x]_1−y:(ZrO₂)_y were prepared following the conventional ceramic powder processing route. In the mixed matrix system prepared by melt quench technique, a nominal increase in conductivity (σ) was found in (BaCl₂)_0.9:(KCl)_0.1. On ZrO₂ particle dispersion in this mixed matrix, the maximum conductivity (∼90 times that of base matrix value) was found to occur with 50 m/o of ZrO₂. Conductivity increases monotonically over the temperature range from 100 to 300 °C studied and attains the value of 10 × 10⁻⁶ S cm⁻¹ at 300 °C. The mobility (μ) of the charge carriers at room temperature was found to be 18.5 × 10⁻² cm² V⁻¹ s⁻¹ and the increase in μ with temperature was not very significant. The transference ionic number determination showed that the electrical conductivity of the electrolyte is predominantly due to ions. This study indicates that the conductivity is governed by mobile ion concentration.     

Order-disorder phase transitions and high-temperature oxide ion conductivity of Er2+xTi2−xO7−δ (x = 0, 0.096)

The Er_2+xTi_2−xO_7−δ (x = 0.096; 35.5 mol% Er₂O₃) solid solution and the stoichiometric pyrochlore-structured compound Er₂Ti₂O₇ (x = 0; 33.3 mol% Er₂O₃) are characterized by X-ray diffraction (phase analysis and Rietveld method), thermal analysis and optical spectroscopy. Both oxides were synthesized by thermal sintering of co-precipitated powders. The synthesis study was performed in the temperature range 650-1690 °C. The amorphous phase exists below 700 °C. The crystallization of the ordered pyrochlore phase (P) in the range 800-1000 °C is accompanied by oxygen release. The ordered pyrochlore phase (P) exists in the range 1000−1200 °C. Heat-treatment at T ≥ 1600 °C leads to the formation of an oxide ion-conducting phase with a distorted pyrochlore structure (P2) and an ionic conductivity of about 10⁻³ S/cm at 740 °C. Complex impedance spectra are used to separately assess the bulk and grain-boundary conductivity of the samples. At 700 °C and oxygen pressures above 10⁻¹⁰ Pa, the Er_2+xTi_2−xO_7−δ (x = 0, 0.096) samples are purely ionic conductors.