Re-examination of phase relations between solid solutions in R4Al2O9-R4Si2N2O7-R4Si2O10 (R=Y,Gd, Yb) systems

Samples in Si–Al-R-O-N (R = Y, Gd, Yb) systems were prepared by solid-state reactions using R₂O₃, Al₂O₃, SiO₂ and Si₃N₄ powders as starting materials. X-ray diffraction was done to investigate RAM-J(R) solid solutions [RAM = R₄Al₂O₉, J(R) = R₄Si₂N₂O₇] formation and their equilibrium with RSO (R₄Si₂O₁₀). Phase relations between RAM, J(R) and RSO at 1700 °C were summarized in a phase diagram. It was determined that a limited solid solution of RAM and RSO could be formed along RAM-RSO tie-line, while RAM and J(R) form a continuous solid solution along RAM-J(R) tie-line. In RAM-J(R)-RSO ternary systems, the RAM-J(R) tie-lines were extended towards the RSO corner to form a continuous solid solution area of JRAMss (R = Y, Gd, Yb). The established phase relations in the Si–Al-R-O-N (R = Y, Gd, Yb) systems may facilitate compositional selections for developing JRAMss as monolithic ceramics or for SiC/Si₃N₄ based composites using the solid-solutions as a second refractory phase.     

In-vitro evaluation of wollastonite nanopowder produced by a facile process using cheap precursors for biomedical applications

Wollastonite nanopowder (β-CaSiO₃) is the most nanoceramic powder that is most frequently applied in biomedical applications due to its good bioactivity and biocompatibility. Although the preparation of wollastonite in a solid-state is distinguished as a simple and cheap method with large-scale production, it requires high temperatures (=1400 °C) and consumes quite a long time. The wet methods are considered the best when it comes to preparing the wollastonite nanopowders. However, it has some drawbacks such as its extravagant raw materials and its shorting in preparation which inhibits successful coverage for large-scale production. Herein facile, one-pot modified co-precipitation approach with an easy procedure, shorter reaction time, and in-expensive precursor sodium meta-silicate-pentahydrate and CaCO₃ has been utilized for large-scale production of wollastonite nano-powders (76–150 nm). The precipitated product was calcined at different temperatures (800, 900, 1000, and 1100 °C). The phase composition and microstructure of the calcined powders were investigated. They were analyzed by XRD, FTIR, FESEM, and HRTEM. The in-vitro bioactivities of the calcined powders at 1000 &1100 °C were investigated by analyzing their abilities to form apatite on their surface after 21 days in SBF. The apatite mineralization of the powder surfaces was examined through FESEM, EDX, and Raman spectra. The results show that a single-phase wollastonite got formed at all calcined temperatures with a unique silkworm texture. SBF in-vitro test states the formation of HA on the powder surface. Therefore, these powders are expected to be valuable and promising for biomedical applications such as coating and bio cement.     

Structural Aspects of P2-Type Na0.67Mn0.6Ni0.2Li0.2O2 (MNL) Stabilization by Lithium Defects as a Cathode Material for Sodium-Ion Batteries

A known strategy for improving the properties of layered oxide electrodes in sodium-ion batteries is the partial substitution of transition metals by Li. Herein, the role of Li as a defect and its impact on sodium storage in P2-Na_0.67Mn_0.6Ni_0.2Li_0.2O₂ is discussed. In tandem with electrochemical studies, the electronic and atomic structure are studied using solid-state NMR, operando XRD, and density functional theory (DFT). For the as-synthesized material, Li is located in comparable amounts within the sodium and the transition metal oxide (TMO) layers. Desodiation leads to a redistribution of Li ions within the crystal lattice. During charging, Li ions from the Na layer first migrate to the TMO layer before reversing their course at low Na contents. There is little change in the lattice parameters during charging/discharging, indicating stabilization of the P2 structure. This leads to a solid-solution type storage mechanism (sloping voltage profile) and hence excellent cycle life with a capacity of 110 mAh g^-1 after 100 cycles. In contrast, the Li-free compositions Na_0.67Mn_0.6Ni_0.4O₂ and Na_0.67Mn_0.8Ni_0.2O₂ show phase transitions and a stair-case voltage profile. The capacity is found to originate from mainly Ni³⁺/Ni⁴⁺ and O^2-/O^2-δ redox processes by DFT, although a small contribution from Mn⁴⁺/Mn⁵⁺ to the capacity cannot be excluded.     

Multiferroic behaviour in ‘Bi’ doped solid solution SmFeO3-BaTiO3 perovskite system

The solid solution of (Sm_0.75Bi_0.25FeO₃)_0.5 (BaTiO₃)_0.5 perovskite system is developed through conventional solid state reaction route. Prepared compound is thoroughly analyzed for its multipurpose use by studying its multiferroic character. The XRD spectra verifies the synthesized material is crystallize in tetragonal structure (space group = P4mm). The identification of the involved elements and their actual oxidation states are inspected through X-ray photoelectron spectroscopic (XPS) technique. Dielectric studies reveal the material has high dielectric constant at room temperature for possible storage devices. The relaxation process in the system is related to the short-range portability of charge transporters as studied from modulus spectra. Material can be beneficial for memory devices according to the room temperature multiferroic studies.     

Experimental investigation of Co and Fe-Doped CuO nanostructured electrode material for remarkable electrochemical performance

The current research work presents a facile and cost–effective co-precipitation method to prepare doped (Co & Fe) CuO and undoped CuO nanostructures without usage of any type of surfactant or capping agents. The structural analysis reveals monoclinic crystal structure of synthesized pure CuO and doped-CuO nanostructures. The effect of different morphologies on the performance of supercapacitors has been found in CV (cyclic voltammetry) and GCD (galvanic charge discharge) investigations. The specific capacitances have been obtained 156 (±5) Fg^?1, 168(±5) Fg^?1 and 186 (±5) Fg^?1 for CuO, Co-doped CuO and Fe-doped CuO electrodes, respectively at scan rate of 5 mVs^?1, while it is found to be 114 (±5) Fg^?1, 136 (±5) Fg^?1 and 170 (±5) Fg^?1 for CuO, Co–CuO and Fe–CuO, respectively at 0.5 Ag^-1 as calculated from the GCD. The super capacitive performance of the Fe–CuO nanorods is mainly attributed to the synergism that evolves between CuO and Fe metal ion. The Fe-doped CuO with its nanorods like morphology provides superior specific capacitance value and excellent cyclic stability among all studied nanostructured electrodes. Consequently, it motivates to the use of Fe-doped CuO nanostructures as electrode material in the next generation energy storage devices.     

Optimization of structural,electrical, and magnetic properties of ytterbium substituted W-type hexaferrite for multi-layer chip inductors

The rare earth (Yb³⁺) substituted W-type hexagonal ferrites with composition CaPb_2-xYb_xFe₁₆O₂₇ (x = 0.0, 0.5, 1.0, 1.5, 2.0) were synthesized by a facile and cost-effective sol-gel auto combustion method with post heat treatment. The synthesized hexagonal ferrites were characterized by a variety of analytical techniques, and an impedance analyzer was used to investigate the effects of Ytterbium on structural, magnetic, spectral and dielectric properties. The relationship between their impedance, structure and dielectric properties was investigated. The X-ray diffraction patterns verify the presence of single-phase W-type hexagonal ferrites. Physical properties such as D_bulk (bulk density), D_xrd (X-ray density), and P (porosity) of the CaPb_2-xYb_xFe₁₆O₂₇ W-type hexagonal ferrites were calculated. The bulk density of all the samples was decreased, and X-ray intensity was increased with the Ytterbium replacement in the W-type hexaferrite. By adding Yb³⁺ ions, the lattice parameters, cell volume and X-ray density were reduced due to the substitution of ytterbium with smaller ionic radii compared to the lead ion with large ionic radii. The AC-conductivity was increased from (1.523 × 10^?5 to 6.699 × 10^?5) Ωcm^?1. The dielectric constant and tangent loss was found to decrease substantially. The magnetic properties were found to enhance by the substitution of Yb³⁺. The low coercivity value of Yb³⁺ substituted W-type hexagonal ferrites are suitable for magnetic recording media operated at a high-frequency regime. The enhancement of electrical, dielectric and magnetic characteristics suggests these materials as promising for multi-layer chip inductors (MLCIs) circuit applications.     

Impact of Co doping on physical,structural, microstructural and magnetic features of MgZn nanoferrites for high frequency applications

Cobalt (Co) doped MgZn spinel nanoferrites with composition Mg_0.5Zn_0.5Co_x Fe_2-xO₄ at x = 0.0, 0.10, 0.20, 0.30, 0.40, 0.50 were prepared using sol-gel auto ignition method. The characterizations techniques such as FESEM, FTIR, XRD and VSM were used to determine the morphology, force constants, phase, structure and magnetic features of the samples. Lattice parameters, FWHM, d-spacing, crystallite size, micro strains and volume were investigated using high score plus software. Materials analysis using diffraction (MAUD) software was also used to study the Rietveld refinement properties of the Co doped MgZn ferrites. Physical properties such as porosity, X-ray and bulk density were also determined. Force constants of their respective absorption bands were calculated from FTIR of the Co doped MgZn nanoferrites. Single phase structure with cubic phase were observed for MgZn and Co doped MgZn at x = 0.0 whereas second phase was observed at higher Co concentrations respectively. FESEM show regular shape of the particles at low Co concentrations whereas agglomerations were observed at higher Co concentrations respectively. The magnetic properties of the Co doped MgZn ferrites were also investigated from VSM study. Magnetic remanence, coercivity, initial permeability, saturation magnetization, Bohr magneton and anisotropy constant were determined from VSM analysis. The coercivity, saturation magnetization, remanence, anisotropy constant and initial permeability were enhanced with the doping of ‘Co’ in MgZn nanoferrites. Response of the Co doped MgZn nanoferrites at high frequency regime was also evaluated. It can be seen that the response from all the Co doped MgZn nanoferrites was 2.84 GHz–5.96 GHz respectively and suggested the use of these nanoferrites for the operation of nanodevices in the X-band high frequency regime.     

Effect of the acid type on clinoptilolite-rich tuff for hydrogen storage

Clinoptilolite from Gördes (Turkey) was treated with HCl, HNO₃ and H₂SO₄ solutions of varying concentrations (from 2.0 M to 6.0 M) at 90 °C for 4 h to evaluate its potential for possible applications in hydrogen storage. X-ray diffraction, X-ray fluorescence and nitrogen adsorption techniques were applied for characterization of the zeolites. Hydrogen adsorption capacities of clinoptilolite samples were found in the range between 1.609 and 2.391 mmol/g. The effects of the acid modification process on the structure and hence hydrogen adsorption was evaluated according to the obtained results.     

On processing of Ni-WC based functionally graded composite clads through microwave heating

Present study focuses on the development of four layered functionally graded clads (FGC) of Ni-WC based composite material on AISI 304 substrate through microwave heating route. Experimental trials were conducted inside a microwave applicator of domestic type at frequency range of 2.45?GHz. The optimal exposure time of 900?W microwave power was varied with compositional gradient and it was from 300 to 360?s. The mechanism of FGC formation through microwave heating was explained and developed FGC was subjected to mechanical and microstructure characterizations. The results of micro-structural analysis revealed that the FGC of ～1.8?mm thickness was produced and was free from any type of interfacial cracks and visible porosity. It was observed that WC particles were randomly dispersed in the nickel matrix. XRD study revealed the formation of inter-metallics, such as NiW₄, NiSi, and Cr₂₃C₆. Maximum value of microhardness was observed in the top FGC layer and was 880?±?30?HV.     

Synthesis of Novel Tetra(µ3-Methoxo) Bridged with [Cu(II)-O-Cd(II)] Double-Open-Cubane Cluster: XRD/HSA-Interactions,Spectral and Oxidizing Properties

A new double-open-cubane core Cd(II)-O-Cu(II) bimetallic ligand mixed cluster of type [Cl₂Cu₄Cd₂(NNO)₆(NN)₂(NO₃)₂].CH₃CN was made available in EtOH/CH₃CN solution. The 1-hydroxymethyl-3,5-dimethylpyrazole (NNOH) and 3,5-dimethylpyrazole (NNH) act as N,O-polydentate anion ligands in coordinating the Cu(II) and Cd(II) centers. The structure of the cluster in the solid state was proved by XRD study and confirmed in the liquid state by UV-vis analysis. The XRD result supported the construction of two octahedral and one square pyramid geometries types around the four Cu(II) centers and only octahedral geometry around Cd(II) two centers. Interestingly, NNOH ligand acts as a tetra-µ³-oxo and tri-µ²-oxo ligand; meanwhile, the N-N in NNH acts as classical bidentate anion/neutral ligands. The interactions in the lattice were detected experimentally by the XRD-packing result and computed via Hirschfeld surface analysis (HSA). The UV-vis., FT-IR and Energy Dispersive X-ray (EDX), supported the desired double-open cubane cluster composition. The oxidation potential of the desired cluster was evaluated using a 3,5-DTB-catechol 3,5-DTB-quinone as a catecholase model reaction.