Preparation and microstructural characterization of (Nd1−xGdx)2(Ce1−xZrx)2O7 solid solutions

(Nd_1−xGd_x)₂(Ce_1−xZr_x)₂O₇ (0 ≤ x ≤ 1.0) powders with an average particle size of 100 nm were synthesized with chemical-coprecipitation and calcination method, and were characterized by X-ray diffractometry and scanning electron microscopy. The sintering behaviour of (Nd_1−xGd_x)₂(Ce_1−xZr_x)₂O₇ powders was studied by pressureless sintering at 1600–1700 °C for 10 h in air. The relative densities of (Nd_1−xGd_x)₂(Ce_1−xZr_x)₂O₇ solid solutions increase with increasing the sintering temperature, and gradually decrease with increasing the content of neodymium and cerium at identical temperature levels. (Nd_1−xGd_x)₂(Ce_1−xZr_x)₂O₇ solid solutions have a single phase of defect fluorite-type structure among all the composition combinations studied. The lattice parameters of (Nd_1−xGd_x)₂(Ce_1−xZr_x)₂O₇ solid solutions agree well with the Vegard's rule.     

Comparison of the microwave-induced combustion and solid-state reaction for the synthesis of LiMn2O4 powder and their electrochemical properties

In the current research, we proposed a new method called microwave-induced combustion synthesis to produce LiMn₂O₄ powders. The microwave-induced combustion synthesis entails the dissolution of metal nitrates, and urea in water, and then heating the resulting solution in a microwave oven. Spinel LiMn₂O₄ powders were successfully synthesized by microwave-induced combustion. The microwave-heated LiMn₂O₄ powders annealed at various temperatures in the range of 600–800 °C were determined. The resultant powders were characterized by X-ray diffractometer (XRD), and scanning electron microscopy (SEM). The annealed samples were used as cathode materials for lithium-ion battery, for which their discharge capacity and electrochemical characteristic properties in terms of cycle performance were also investigated. The LiMn₂O₄ cell provides a high initial capacity of 133 mAh/g and excellent reversibility. The excellent capacity and reversibility were attributed to LiMn₂O₄ powders with small and uniform particle size produced by microwave-induced combustion synthesis.     

Low-temperature synthesis of ZnNb2O6 powders via hydrothermal method

ZnNb₂O₆ powder was successfully synthesized via hydrothermal method with Nb₂O₅ and Zn(NO₃)₂·6H₂O as raw materials and cyclohexane as solvent. Phase composition, morphology, and chemical composition were determined via a combination of XRD, SEM, TEM and EDS techniques. The effects of synthesis temperature and reaction time on phase composition and particle morphology were investigated in this paper. The results showed that fine ZnNb₂O₆ powders could be obtained at a hydrothermal temperature of 190 °C or above under different reaction time.     

Synthesis of negative thermal expansion materials ZrW2−xMoxO8 (0 ≤ x ≤ 2) using hydrothermal method

Negative thermal expansion materials ZrW_2−xMo_xO₈ (0 ≤ x ≤ 2) have been successfully synthesized by the reaction of a mixture of ammonium tungstate and ammonium molybdate with zirconium oxynitrate using a hydrothermal method. Effect of substituted ion Mo on the microstructure, α-to-β and cubic to trigonal phase transition in resulting ZrW_2−xMo_xO₈ powders was examined by the XRD experiments. It was found that the structural phase transition temperature decreased slightly with increasing substituted content. The cubic to trigonal phase transition was also influenced by substituted content. The resulting products decomposed to WO₃/MoO₃ and ZrO₂ as temperature increasing when x ≤ 0.5 and while x > 0.5, the cubic phase transited to trigonal phase. The effect of substituted Mo on the morphology of resulting products was also investigated by SEM experiments.     

Mechanochemical synthesis of Ti1−xZrxB2 and Ti1−xHfxB2 solid solutions

Solid solutions of TiB₂-ZrB₂ and TiB₂-HfB₂ were obtained under an inert atmosphere by high-energy ball-milling mixtures of Ti/Zr/B and Ti/Hf/B, respectively. Milling promoted mechanically induced self-sustaining reactions (MSR), and the ignition time was dependent on the initial composition of the mixture. The stoichiometry of Ti_1−xZr_xB₂ and Ti_1−xHf_xB₂ solid solutions was controlled by adjusting the atomic ratio of the reactants. The solid solutions were characterised by X-ray diffraction, transmission electron microscopy, electron diffraction, and energy dispersive X-ray spectroscopy. The results revealed that TiB₂-ZrB₂ possessed a nanometric microstructure and good chemical homogeneity. However, in the TiB₂-HfB₂ system, an inhomogeneous solid solution was obtained when a Ti-rich mixture was employed. The solid solutions showed good thermal stability; thus, can be used as raw materials for the development of technological materials for structural applications.     

Synthesis and photoluminescence properties of La1−xAlO3:xTb green phosphors for white LEDs

Tb³⁺-doped La_1−xAlO₃ phosphor powders are successfully synthesized by the solution combustion method, using citric acid as the combustion fuel. The crystal structure and photoluminescence properties of La_1−xAlO₃:xTb³⁺ phosphors are studied, depending on Tb³⁺ content. The strongest emission peak is found at 543 nm, which originates from the ⁵D₄→⁷F₅ transition of Tb³⁺ ions, indicating green emission. Among the fabricated phosphors, the La_0.9AlO₃:0.1Tb³⁺ phosphor emits the strongest green light. The excellent luminescent properties make it a possible candidate for white light-emitting diodes and various photonic applications.     

Nanocrystalline BaAl2O4 powders prepared by aqueous combustion synthesis

In order to achieve BaAl₂O₄ formation via combustion synthesis, two types of recipes were designed: single fuel recipes (urea, glycine, β-alanine or hexamethylenetetramine) and innovative fuel mixture recipes (urea+glycine, urea+β-alanine and urea+hexamethylenetetramine respectively). No combustion reactions were noticed in the case of single fuel recipes based on urea or hexamethylenetetramine. The only crystalline phase present in the case of the powders obtained in such a way was unreacted Ba(NO₃)₂. Glycine and β-alanine generated smoldering reactions, leading to the formation of black powders, which consist of Ba(NO₃)₂, BaCO₃ and traces of BaAl₂O₄ (in the case of β-alanine). Fuel mixture recipes proved to be better than single fuel recipes, yielding BaAl₂O₄ as main crystalline phase. The specific surface area of the resulted powders ranges between 2.0 and 3.9 m²/g. The urea and glycine fuel mixture was the most efficient yielding BaAl₂O₄ with an average crystallite size of 60 nm.     

VUV photoluminescence properties of Y1−xGdxVO4:Eu phosphors prepared by ultrasonic spray pyrolysis

The red-emitting (Y_1−xGd_x)_0.94Eu_0.06VO₄ (0 ≤ x ≤ 1.0) phosphors were synthesized by ultrasonic spray pyrolysis. The (Y_1−xGd_x)_0.94Eu_0.06VO₄ (0 ≤ x ≤ 1.0) phosphors had the tetragonal xenotime structure with a space group of I4₁/amd (1 4 1). The calculated crystallite sizes of the annealed phosphors ranged from 58 to 68 nm. In this study, we discussed the photoluminescence properties of the (Y_1−xGd_x)_0.94Eu_0.06VO₄ phosphors under VUV excitation, depending on Gd content. The emission intensity of the (Y_1−xGd_x)_0.94Eu_0.06VO₄ phosphors increased with increasing Gd content up to x = 0.5, and then decreased with a further increase in Gd content. The purest red color was obtained for the (Y_0.5Gd_0.5)_0.94Eu_0.06VO₄ phosphors.     

Synthesis of CuGa2O4 nanoparticles by precursor and self-propagating combustion methods

Copper gallate spinels, CuGa₂O₄, have been synthesized by two wet chemical routes: precursor method and self-propagating combustion involving a glycine-nitrate system. All complex precursors have been characterized by chemical analysis, infrared spectroscopy (IR), ultraviolet visible spectroscopy (UV–vis), electron paramagnetic resonance spectroscopy (EPR), thermal analysis and scanning electron microscopy (SEM). The copper gallate spinel oxides have been further investigated by X-ray diffraction (XRD), SEM, IR, UV–vis, magnetic measurements and EPR. The crystallite size of the copper gallate was found about 280 Å.     

Synthesis of LaB6 powders from La2O3, B2O3 and Mg blends via a mechanochemical route

This study reports a room temperature mechanochemical route for the synthesis of LaB₆ powders from La₂O₃–B₂O₃–Mg blends. The synthesis reaction was driven by high-energy ball milling and was gradually examined in terms of milling duration and process control agent. Following the mechanochemical synthesis, unwanted MgO phase and Fe contamination worn off from the milling vial/balls were removed with HCl acid leaching under the effect of ultrasonic stirring. Pure LaB₆ powders were obtained after repeated centrifuging, repeated washing and drying. Subsequent annealing was performed in a tube furnace at 800 °C for 5 h under Ar atmosphere in order to reveal residual elements. Phase and microstructural characterizations of the milled, leached and annealed powders were performed using X-ray diffractometry (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. A novel route for producing fine-grained LaB₆ powders was accomplished with shorter reaction times resulting in higher purity.     

One-step hydrothermal synthesis and microwave electromagnetic properties of RGO/NiFe2O4 composite

The reduced graphene oxide (RGO)/NiFe₂O₄ composite was synthesized by a facile one-pot hydrothermal route, which avoided the usage of chemical reducing agent. The reduction of graphene oxide (GO) and the crystallization of NiFe₂O₄ crystals happened in a one-step hydrothermal process. The morphology, microstructure and magnetic properties of the composite were detected by means of XRD, XPS, TEM, EDX, TG-DSC and VSM. The maximum R_L of the RGO/NiFe₂O₄ composite is −39.7 dB at 9.2 GHz with the thickness of 3.0 mm, and the absorption bandwidth with the R_L below −10 dB is up to 5.0 GHz (from 12.7 to 17.7 GHz) with a thickness of 1.9 mm. The introduction of RGO signally enhanced microwave absorption performance of the NiFe₂O₄ NPs. It is believed that such composite will be applied widely in microwave absorbing area.     

Impedance spectroscopic studies on NiFe2O4 with different morphologies: Microstructure vs. dielectric properties

NiFe₂O₄ powders were prepared by combustion synthesis, polyol-mediated and sol–gel methods. Morphological characterization of sintered disks was carried out using scanning electron microscopy (SEM). Dielectric properties of NiFe₂O₄ synthesized by different routes were investigated over the frequency range of 100 Hz–5 MHz at room temperature. A difference in dielectric constant (ε_r) and dissipation factor (tan δ) of NiFe₂O₄ samples obtained by different synthesis methods has been observed. The observed dissimilarity in the behavior originates from the variation in the microstructure of the samples that is evident in the Cole–Cole plot results.     

One-pot hydrothermal synthesis of MoS2 nanosheets/C hybrid microspheres

Uniform MoS₂ nanosheets/C hybrid microspheres with mean diameter of 320 nm have been successfully synthesized via a facile one-pot hydrothermal route by sodium molybdate reacting with sulfocarbamide in d-glucose solutions. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). XRD patterns showed that the MoS₂ was kept as a two-dimensional nanosheet crystal and C was retained as amorphous even after their annealing treatment at 800 °C. TEM and SEM images indicated that the MoS₂ nanosheets were uniformly dispersed in the amorphous carbon. The experiment results also revealed that the appropriate amount of d-glucose had an obvious effect on the formation of uniform MoS₂ nanosheets/C hybrid microspheres. A possible formation process of MoS₂ nanosheets/C hybrid microspheres was preliminarily presented.     

Structure and magnetic properties of multi-morphological CoFe2O4/CoFe nanocomposites by one-step hydrothermal synthesis

Multi-morphological CoFe₂O₄/CoFe nanocomposites have been synthesized using a facile hydrothermal process. The effects of hydrazine hydrate amount during hydrothermal reaction on the structure and magnetic property of the specimens were studied. With increasing hydrazine hydrate amount, the CoFe₂O₄ transformed to CoFe and the morphology of the specimen changed from granular particles to faceted particles. The saturation magnetization monotonically increased and the coercivity monotonically decreased with increasing hydrazine hydrate amount. The magnetic interactions, determining the magnetic properties of the composites, result from the dominant dipole coupling and relative weak exchange coupling between CoFe₂O₄ and CoFe nanoparticles. The CoFe₂O₄/CoFe nanocomposite prepared with 2?mL hydrazine hydrate exhibited the optimal magnetic properties, with the saturation magnetization of 81?emu/g and coercivity of 636?Oe.     

Fabrication of Yb-doped Lu2O3-Y2O3-La2O3 solid solutions transparent ceramics by self-propagating high-temperature synthesis and vacuum sintering

A comparative analysis of sintering and grain growth processes of lutetium oxide and lutetium-yttrium-lanthanum oxides solid solutions, as well as optical properties, luminescence and laser generation of (Lu_xY_0.9-xLa_0.05Yb_0.05)₂O₃ transparent ceramics are reported. Fabrication of highly dispersed initial powders of these compounds was performed via nitrate-glycine self-propagating high-temperature synthesis (SHS) method. The powders were compacted at 300?MPa and vacuum sintered at temperatures up to 1750?°С. Optical ceramics of (Lu_0.65Y_0.25La_0.05Yb_0.05)₂O₃ elemental composition were shown to have the highest in-line transmittance, which achieved 78% at the wavelength of 800?nm. Generation of laser radiation at a wavelength of 1032?nm with the differential efficiency of 20% was demonstrated in the (Lu_0.65Y_0.25La_0.05Yb_0.05)₂O₃ ceramics.     

Effect of La substitution on the structural and electrical properties of BaBi4−xLaxTi4O15

Pure and lanthanum doped barium bismuth titanate BaBi_4−xLa_xTi₄O₁₅ (BBLT, x=0, 0.05, 0.15, 0.30) ceramics were prepared utilizing solid state method. The X-ray diffraction (XRD) data confirmed formation of single-phase Aurivillius compounds while SEM micrographs did not show evident grain size change of doped ceramics. Dielectric properties were investigated in 1.21 kHz to 1 MHz frequency range and in the temperature range of 20 to 727 °C. When Bi³⁺ is substituted with La³⁺, a significant disorder was induced and the material exhibited broadening of the phase transition. Impedance analysis confirmed the presence of two semicircular arcs in doped samples suggesting the existence of grain and grain-boundary conduction. The dc-conductivity and activation energies were evaluated for all compositions.     

Adjustable dielectric properties of Li2CuxZn1−xTi3O8 (x=0 to 1) ceramics with low sintering temperature

Single-phase dielectric ceramics Li₂Cu_xZn_1−xTi₃O₈ (x=0–1) were synthesized by the conventional solid-state ceramic route. All the solid solutions adopted Li₂MTi₃O₈ cubic spinel structure in which Li/M and Ti show 1:3 order in octahedral sites whereas Li and M are distributed randomly in tetrahedral sites with the degree of Li/M cation mixing varying from 0.5 to 0.3. The substitution of Cu for Zn effectively lowered the sintering temperatures of the ceramics from 1050 to 850 °C and significantly affected the dielectric properties. As x increased from 0 to 0.5, τ_f gradually increased while the dielectric constant (ε_r) and quality factor value (Q×f) gradually decreased, and a near-zero τ_f of 1.6 ppm/°C with ε_r of 25.2, Q×f of 32,100 GHz could be achieved for Li₂Cu_0.1Zn_0.9Ti₃O₈ ceramic sintered at 950 °C, which make it become an attractive promising candidate for LTCC application. As x increases from 0.5 to 1, the dielectric loss significantly increases with AC conductivity increasing up to 2.3×10⁻⁴ S/cm (at 1 MHz).     

Hydrothermal synthesis of NaNbO3 with low NaOH concentration

NaNbO₃ fine powders were prepared by reacting niobium pentoxide with low NaOH concentration solution under hydrothermal conditions at 160 °C. The reaction ruptured the corner-sharing of NbO₆ octahedra in the reactant Nb₂O₅, yielding various niobates, and the structure and composition of the niobates depended on the [OH⁻] and reaction time. The fine Nb₂O₅ powder first aggregated to large particles and then turned to metastable intermediates with multifarious morphology. The reaction was fast for the situation of [OH⁻] = 2 M. The [OH⁻] determined the structure of final products, and three types of NaNbO₃ powder with the orthorhombic, tetragonal and cubic symmetries were obtained, respectively, depending on the [OH⁻]. The low [OH⁻] was propitious to yield orthorhombic NaNbO₃. The present work demonstrated that higher [OH⁻] was not favored to synthesize NaNbO₃ powders and the conversion speed in this reaction was not in proportion to the [OH⁻].     

Characterization of Mg1−xNixAl2O4 solid solutions prepared by combustion synthesis

Mg_1−xNi_xAl₂O₄ (x = 0, 0.25, 0.5, 0.75 and 1) solid solutions have been prepared by combustion synthesis. After annealing the combustion synthesized powders at 1000 °C for 3 h single-phase Mg_1−xNi_xAl₂O₄ was obtained over the entire range of compositions. The lattice parameter of Mg_1−xNi_xAl₂O₄ gradually increased from 8.049 Å (NiAl₂O₄) to 8.085 Å (MgAl₂O₄), which certified the formation of the spinel solid solutions. All samples prepared by combustion synthesis had blue color shades, denoting the inclusion of Ni²⁺ in the spinel structure in octahedral and tetrahedral configuration. The crystallite size of Mg_1−xNi_xAl₂O₄ was in the range of 35-39 nm and the specific surface area varied between 5.8 and 7.0 m²/g.     

Synthesis,structural analysis and dielectric properties of Ba8(Mg1−xZnx)Nb6O24 hexagonal perovskites

Ba₈(Mg_1−xZn_x)Nb₆O₂₄ (x=0, 0.2, 0.4, 0.6, 0.8 and 1) ceramics were prepared through the conventional solid-state route. The materials were calcined at 1250 °C and sintered at 1375–1425 °C. The structure of the system was analyzed using X-ray diffraction and vibrational spectroscopic studies. The microstructure of the sintered pellet was analyzed using scanning electron microscopy. The dielectric constant (ε_r), temperature coefficient of resonant frequency (τ_f) and the unloaded quality factor (Q_u) were measured in the microwave frequency region. The τ_f values of the compositions were reduced by varying the value of x from 0 to 1. The dielectric responses to frequency were also studied in the radio frequency region. The compositions have good microwave dielectric properties and hence are suitable for dielectric resonator applications.