Improvement in hydrogen sorption properties of Mg by reactive mechanical grinding with Cr2O3, Al2O3 and CeO2

We tried to improve the hydrogen sorption properties of Mg by mechanical grinding under H₂ (reactive mechanical grinding) with oxides Cr₂O₃, Al₂O₃ and CeO₂. The hydriding rates of Mg are reportedly controlled by the diffusion of hydrogen through a growing Mg hydride layer. The added oxides can help pulverization of Mg during mechanical grinding. A part of Mg is transformed into MgH₂ during reactive mechanical grinding. The Mg+10wt.%Cr₂O₃ powder has the largest transformed fraction 0.215, followed in order by Mg+10wt.%CeO₂ and Mg+10wt.%Al₂O₃. The Mg+10wt.%Cr₂O₃ powder has the largest hydriding rates at the first and fifth hydriding cycle, followed in order by Mg+10wt.%Al₂O₃ and Mg+10wt.%CeO₂. Mg+10wt.%Cr₂O₃ absorbs 5.87wt.% H at 573 K, 11 bar H₂ during 60 min at the first cycle. The Mg+10wt.%Cr₂O₃ powder has the largest dehydriding rates at the first and fifth dehydriding cycle, followed by Mg+10wt.%CeO₂ and Mg+10wt.%Al₂O₃. It desorbs 4.44 wt.% H at 573 K, 0.5 bar H₂ during 60 min at the first cycle. All the samples absorb and desorb less hydrogen at the fifth cycle than at the first cycle. It is considered that this results from the agglomeration of the particles during hydriding–dehydriding cycling. The average particle sizes of the as-milled and cycled powders increase in the order of Mg+10wt.%Cr₂O₃, Mg+10wt.%Al₂O₃ and Mg+10wt.%CeO₂. The quantities of hydrogen absorbed or desorbed for 1 h for the first and fifth cycles decrease in the order of Mg+10wt.%Cr₂O₃, Mg+10wt.%Al₂O₃ and Mg+10wt.%CeO₂. The quantities of absorbed or desorbed hydrogen increase as the average particle sizes decrease. As the particle size decreases, the diffusion distance shortens. This leads to the larger hydriding and dehydriding rates. The Cr₂O₃ in the Mg+10wt.%Cr₂O₃ powder is reduced after hydriding–dehydriding cycling. The much larger chemical affinity of Mg than Cr for oxygen leads to a reduction of Cr₂O₃ after cycling.     

Morphology and texture evolution of FeCrAlTi-Y2O3 foil fabricated by EBPVD

An electron beam physical vapor deposition method was used to fabricate freestanding Y₂O₃ dispersive strengthened FeCrAlTi foils for high-temperature applications. The vapor incidence mode was found to have great impact on the morphology and crystallographic orientation of the foils. Under symmetric vapor incidence mode, an out-of-plane < 100> fiber texture was formed. While under asymmetric vapor incidence mode, both out-of-plane preference of < 111> direction and several in-plane preferences were developed. As the deposition proceeded, the extent of in-plane orientation increased, and the preferred out-of-plane orientation increasingly deviated from the surface normal. The vapor incidence mode played a role on the growth rate of < 100> direction and < 110> direction, by which the morphology and crystallographic orientation of grains were modified.     

Microstructural and mechanical properties of Al-Mg/Al2O3 nanocomposite prepared by mechanical alloying

The effect of milling time on the microstructure and mechanical properties of Al and Al-10 wt.% Mg matrix nanocomposites reinforced with 5 wt.% Al₂O₃ during mechanical alloying was investigated. Steady-state situation was occurred in Al-10Mg/5Al₂O₃ nanocomposite after 20 h, due to solution of Mg into Al matrix, while the situation was not observed in Al/5Al₂O₃ nanocomposite at the same time. For the binary Al-Mg matrix, after 10 h, the predominant phase was an Al-Mg solid solution with an average crystallite size 34 nm. Up to 10 h, the lattice strain increased to about 0.4 and 0.66% for Al and Al-Mg matrix, respectively. The increasing of lattice parameter due to dissolution of Mg atom into Al lattice during milling was significant. By milling for 10 h the dramatic increase in microhardness (155 HV) for Al-Mg matrix nanocomposite was caused by grain refinement and solid solution formation. From 10 to 20 h, slower rate of increasing in microhardness may be attributed to the completion of alloying process, and dynamic and static recovery of powders.     

Synthesis, structural and microwave dielectric properties of Al2W3−xMoxO12 (x = 0-3) ceramics

Low dielectric ceramics in the Al₂W_3−xMo_xO₁₂ (x = 0-3) system have been prepared through solid state ceramic route. The phase purity of the ceramic compositions has been studied using powder X-ray diffraction (XRD) studies. The microstructure of the sintered ceramics was evaluated by Scanning Electron Microscopy (SEM). The crystal structure of the ceramic compositions as a result of Mo substitution has been studied using Laser Raman spectroscopy. The microwave dielectric properties of the ceramics were studied by Hakki and Coleman post resonator and cavity perturbation techniques. Al₂Mo_xW_3−xO₁₂ (x = 0-3) ceramics exhibited low dielectric constant and relatively high unloaded quality factor. The temperature coefficient of resonant frequency of the compositions is found to be in the range −41 to −72 ppm/°C.     

Novel photoluminescent properties of LiGaO2 nanoflakes

The luminescence properties of LiGaO₂ microflakes synthesized using the sol-gel process are investigated. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and photoluminescence (PL) and absorption spectra. The PL spectra excited at 325 nm have a broad and strong emission band with a peak at 383 nm, which corresponds to the self-activated luminescence of the tetrahedral gallium group. The optical absorption spectra of the sample annealed at 600 °C exhibited a band-gap energy of 3.38 eV.     

Electrochemical properties of ordered TiO2 nanotube loaded with Ag nano-particles for lithium anode material

Self-organized TiO₂ nanotube array was grown on titanium (Ti) thin film by anodizing in glycerol solution containing low concentration of NH₄F, and Ag/TiO₂ nanotube was then prepared from TiO₂ nanotube array by thermal decomposition. The physical properties of the synthesized TiO₂ and Ag/TiO₂ nanotubes were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The synthesized two samples were used as negative materials for lithium-ion battery, and their charge–discharge property, cyclic voltammetry, electrochemical impedance spectroscopy, and cycle performance were investigated. The results indicated that the addition of Ag to TiO₂ nanotube could significantly improve the electronic conductivity, charge–discharge capacity, and cycle stability of TiO₂ nanotube.     

A facile route to VN and V2O3 nanocrystals from single precursor NH4VO3

V₂O₃ and VN nanocrystals have been synthesized by the decomposition of the precursor NH₄VO₃ and following nitridation in an autoclave with metallic Na flux at 450–600 °C. X-ray powder diffraction (XRD) recorded the evolution process of the reaction from precursor NH₄VO₃ to hexagonal V₂O₃ and then to NaCl-type VN. In addition, the products were characterized by X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM).     

CTAB-assisted hydrothermal synthesis of NiFe2O4 and its magnetic characterization

A simple hydrothermal route is demonstrated for the synthesis of nickel ferrite nanocrystals, NiFe₂O₄, using cetyltrimethylammonium bromide (CTAB) as the surfactant and NH₃ and NaOH as hydrolyzing agents. Synthesized materials have been characterized by XRD, FTIR, ESR, and TEM techniques. It was found that crystallization in both hydrolyzing agent led to nanometric in size. Average particle size of prepared samples was calculated from TEM micrographs and varied significantly between samples prepared using different hydrolyzing agents; it was 12 nm when conc. NH₃ was used and 50 nm when 2 M NaOH was used. Crystallite size obtained using Scherrer equation agreed well with the TEM observations with the respective values of 15 and 55 nm. ESR analysis showed single broad bands which might indicate the phase homogeneity of the materials. Furthermore, linewidths were observed to differ due to the difference in magnetization that depends on the particle size; NiFe₂O₄ sample hydrolysed with NH₃ has a larger linewidth revealing its smaller particle size as confirmed by XRD and TEM techniques.     

Solution processing of V2O5-WO3 composite films for enhanced Li-ion intercalation properties

We have employed a simple and novel solution processing method to prepare V₂O₅-WO₃ composite films which demonstrate enhanced Li-ion intercalation properties for applications in lithium-ion batteries or electrochromic displays. This solution processing method employs precursors that only contain the elements of V, W, O and H, which avoids impurity elements such as Na that has been commonly used in other solution methods (e.g. using precursors of sodium metavanadate and sodium tungstate solution). The V₂O₅-WO₃ composite films show enhanced Li-ion intercalation properties compared to pure V₂O₅ and WO₃ films. For example, at a high current density of 1.33 A/g, V₂O₅-WO₃ film with a V₂O₅/WO₃ molar ratio of 10/1 exhibits the highest capacities of 200 mA h/g at the first cycle and 132 mA h/g after 50 cycles, while pure V₂O₅ film delivers discharge capacities of 108 mA h/g at the first cycle and 122 mA h/g after 50 cycles. The enhanced Li-ion intercalation properties of the composite films are ascribed to the reduced crystallinity, the increased porosity and thus the enhanced surface area. Both the cyclic voltammogram and chronopotentiometric curves of the V₂O₅-WO₃ film with a molar ratio of 10:1 are distinctively different from those of pure oxide films, suggesting a different Li-ion intercalation process in the V₂O₅-WO₃ film with the molar ratio of 10:1.     

Synthesis and optical studies of gamma irradiated Eu doped nanocrystalline CaF2

Europium (Eu) doped Calcium fluoride (CaF₂) nanoparticles are synthesized by co-precipitation method and characterized by powder X-ray diffraction (PXRD), Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). Also, optical absorption and photoluminescence (PL) results on gamma irradiated Eu doped CaF₂ nanoparticles are presented. The PXRD patterns confirmed the cubic crystallinity of the samples and the particle size is found to be ∼25 nm. The purity of the synthesized nanoparticles is confirmed from FTIR spectrum. The morphological features studied using SEM revealed that nanoparticles are agglomerated and porous. Optical absorption spectrum shows that γ-rayed Eu doped CaF₂ nanoparticles exhibit absorption bands at ∼279, 360 and 434 nm. The PL studies showed emission at ∼420, 525 and 552 nm.     

Magnetic properties of Pr1−xGdxMn2Ge2 compounds

The structure and magnetic properties of the Pr_1−xGd_xMn₂Ge₂ (0.0≤x≤1.0) compounds have been investigated by means of X-ray diffraction (XRD), differential scanning calorimetry (DSC) techniques and AC magnetic susceptibility measurements. All compounds crystallize in the ThCr₂Si₂-type structure with the space group I4/mmm. The lattice constants and the unit cell volume obey Vegard’s law. Samples in this alloy system exhibit a crossover from ferromagnetic ordering for PrMn₂Ge₂ to antiferromagnetic ordering for GdMn₂Ge₂ as a function of Gd concentration x. At low temperatures, the rare earth sublattice also orders and reconfigures the ordering in the Mn sublattice. The results are summarized in the x–T magnetic phase diagram.     

Studies on Y2O3:Eu phosphor with different particle size prepared by wet chemical method

Europium activated yttrium oxide phosphors were prepared by reagent simultaneous addition technique, using oxalic acid as precipitating reagent. The aim of the paper is to establish the flux influence and thermal regime on photoluminescence and morpho-structural characteristics of phosphor powders. In this respect different mineralising agents such as sodium/lithium carbonate, sodium tetraborate ans sodium pyrophosphate were used during the thermal synthesis stage. Thermal analysis, X-ray diffraction, scanning electron microscopy, infrared spectroscopy and photoluminescence measurements were used to investigate precursor and phosphor powders. The correlation between the phosphor properties and precursor quality enabled us to select the optimal synthesis conditions.     

Magnetic properties of Al2O3-Cr2O3 solid solutions

Solid solution ceramics (Al₂O₃)_x(Cr₂O₃)_1−x with different x in the range of 0 < x < 1 were synthesized via traditional ceramic production method. X-ray diffraction results and Rietveld refinements indicated that all samples possessed rhomb-centered structure and continuous solid solutions were synthesized. The samples were composed of irregular grains with several micrometers in diameter. Temperature dependence of magnetization measurements showed monotonous decreasing Néel temperature with increasing x and percolation effect happened with threshold of x = 0.65. As x became higher, weak ferromagnetism was observed in the samples. Field dependence of magnetization measurements further confirmed the weak ferromagnetism in the samples with x = 0.7, 0.8 and 0.9.     

Crystal structure, thermal expansion and electrical properties of the new Al0.32ErGe2 compound

A new ternary compound Al_0.32ErGe₂ has been synthesized and studied from 298 K to 773 K using X-ray powder diffraction technique. Its structure has been determined at room temperature by Rietveld refinement of X-ray powder diffraction data. The ternary compound Al_0.32ErGe₂ crystallizes in the orthorhombic with the defect CeNiSi₂ structure type (space group Cmcm, a = 0.40701(2) nm, b = 1.60401(9) nm, c = 0.39240(2) nm, Z = 4 and D_calc = 8.326 g/cm³). The average thermal expansion coefficients , and of Al_0.32ErGe₂ are 1.72 × 10⁻⁵ K⁻¹, 1.11 × 10⁻⁵ K⁻¹ and 1.52 × 10⁻⁵ K⁻¹, respectively. The bulk thermal expansion coefficient is 4.35 × 10⁻⁵ K⁻¹. Electrical resistivity of Al_0.32ErGe₂ was measured between 5 K and 300 K.     

Effects of Al and Al4C3 contents on combustion synthesis of Cr2AlC from Cr2O3-Al-Al4C3 powder compacts

Preparation of the ternary carbide Cr₂AlC was conducted by combustion synthesis in the mode of self-propagating high-temperature synthesis (SHS) from the Cr₂O₃-Al-Al₄C₃ powder compact. Effects of the contents of Al and Al₄C₃ on the product composition and combustion behavior were studied by formulating the reactant mixture with a stoichiometric proportion of Cr₂O₃:Al:Al₄C₃ = 3:5x:y, where x and y varied from 1.0 to 1.5. When compared to those of the powder compact with Cr₂O₃:Al:Al₄C₃ = 3:5:1 (i.e., x = y = 1.0), the combustion temperature and reaction front velocity increased with content of Al, but decreased with that of Al₄C₃. Besides Cr₂AlC and Al₂O₃, the final products always contained a secondary phase Cr₇C₃ that was substantially reduced by adopting additional Al and Al₄C₃ in the reactant compacts. For the sample with Cr₂O₃:Al:Al₄C₃ = 3:7.5:1 (x = 1.5), solid state combustion reached a peak temperature of 1245 °C and yielded Cr₂AlC with a trivial amount of Cr₇C₃. Although Cr₇C₃ was lessened by introducing extra Al₄C₃, the increase of Al₄C₃ from y = 1.1 to 1.5 produced almost no further reduction of Cr₇C₃ in the final product. This is partly attributed to the low combustion temperature in the range of 1065-1095 °C for the samples with additional Al₄C₃, and in part, due to the role of Al₄C₃ which might react with Cr to form Cr₇C₃, Cr₂Al, and Cr₂AlC.     

Preparation of nano-sized SrAl2O4 using an amorphous hetero-nucleus complex as a precursor

Nano-crystalline SrAl₂O₄ with spinel structure was successfully prepared at 700 °C using amorphous SrAl₂(diethylenetriaminepentaacetic acid (DTPA)_1.6)(H₂O)₄ as precursor. The precursor was synthesized by a simple inorganic reaction and decomposed into SrAl₂O₄ at temperatures above 500 °C, which was proved by DTA–TGA and X-ray photoelectron spectroscopy (XPS) analysis. X-ray diffraction (XRD) results illustrated that a crystalline SrAl₂O₄ phase can form at 700 °C, which is about 600 °C lower than that used in the traditional method. The crystalline SrAl₂O₄ prepared at 900 °C for 2 h had a crystal size of about 28 nm and a grain size of about 80 nm, and its BET surface area can reach 28.056 m²/g. Calcination temperature and time had a weak effect on crystal size.     

SEM and TEM characterization of magnesium hydride catalyzed with Ni nano-particle or Nb2O5

The microstructures of MgH₂ catalyzed with Ni nano-particle or Nb₂O₅ mesoporous powders are examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations. For MgH₂ catalyzed with Ni, the Ni particles with the diameter smaller than 1 μm were detected on the MgH₂ particles with the diameter smaller than 5 μm by the back scattering electron (BSE) microscopy. In details, the TEM micrograph indicates that the Ni particles distribute 20 nm in diameter on MgH₂ uniformly, which was the same size as the additive doped in MgH₂ before milling. On the other hand, for MgH₂ catalyzed with Nb₂O₅, the additive particles could not be found anywhere in the BSE image. Even in the TEM micrograph by much larger magnification than the SEM micrograph, the particles corresponding to the additive cannot be observed at all. Furthermore, an energy dispersive X-ray (EDX) analysis in spots with a diameter of 20 nm indicated that the existing ratio of Mg to Nb was evaluated to 98:2, being the same as the starting ratio before milling. Therefore, the metal oxide Nb₂O₅ becomes extremely small particle that could not be observed by the present work after milling compared to metal Ni^nano.     

Synthesis, structure, and properties of Li2Pb2CuB4O10 with isolated [CuB4O10] units

The copper borate Li₂Pb₂CuB₄O₁₀ has been synthesized in air by the standard solid-state reaction at temperature in the range 550-650 °C and the structure of Li₂Pb₂CuB₄O₁₀ was determined by single-crystal X-ray diffraction. Li₂Pb₂CuB₄O₁₀ crystallizes in the monoclinic space group C2/c (no. 15) with a = 16.8419(12), b = 4.7895(4), c = 13.8976(10) Å, and β = 125.3620(10)°, V = 914.22(12) Å³, and Z = 4, as determined by single-crystal X-ray diffraction. The Li₂Pb₂CuB₄O₁₀ structure exhibits isolated units of stoichiometry [CuB₄O₁₀]⁶⁻ that are built from CuO₄ distorted square planes and triangular BO₃ groups. The IR spectroscopy and thermal analysis investigations of Li₂Pb₂CuB₄O₁₀ are also presented.     

Morphology and structure of LiNb0.6Ti0.5O3 particles by molten salt synthesis

M-phase LiNb_0.6Ti_0.5O₃ (LNT) plate-like particles with large anisometric shape were firstly fabricated by molten salt synthesis (MSS) method in LiCl flux. Effects of reaction temperature, holding time and the weight ratio of LiCl salt to the original powders on the phase structure and morphology of the synthesized particles were investigated. The LiNb_0.6Ti_0.5O₃ powders generally showed a multi-layer structure, exhibiting irregular hexagonal or triangle morphology. The reaction temperature showed a strong influence on the particle growth process, and pure LNT particles are obtained at 950 °C. Further increasing the reaction temperature and holding time could increase the average size of the particles. It revealed that the thickness of the plat-like particles was increased as the contents of the chloride salts increased. The synthesis process, the relation between crystal structure and morphology of particles were also discussed.