Transport properties in spinel ferrite/graphene oxide nanocomposites for electromagnetic shielding

Herein, $\left({\text{Co}}_{0.5}{\text{Ni}}_{0.5}\right){\text{Cr}}_{0.3}{\text{Fe}}_{1.7}{\text{O}}_4$/graphene oxide nanocomposites were fabricated by ultrasonication technique, using pure spinel ferrite and graphene oxide synthesized by sol-gel method and modified Hummers' method, respectively. The effect of graphene incorporation with ferrite nanoparticles was studied by X-ray diffraction (XRD), electrical and dielectric measurements. XRD analysis revealed the spinel phase for the ferrite sample and confirmed the formation of graphene oxide. The crystallite size was found in the range of $37-43\text{ nm}$ and the porosity increased with the increase in the concentration of graphene oxide in the composites. The DC electrical resistivity of spinel ferrite was found equal to $3.83\times {10}^9\text{ Ω}.\text{cm}$ and it substantially decreased with the increase in the percentage of graphene oxide at room temperature. The real and imaginary part of relative permittivity followed the Maxwell-Wagner type of interfacial polarization. AC conductivity confirmed the conduction by hopping mechanism and increased on increasing the GO content. The coupling of magnetic ferrite with graphene oxide tunes the magneto-electrical properties for potential applications at high frequencies.     

Sputtered Fe1·5CoNi0.5 coating: An improved protective coating for SOFC interconnect applications

In an attempt to optimize the properties of FeCoNi coating for planar solid oxide fuel cell (SOFC) interconnect application, the coating composition is modified by increasing the ratio of Fe/Ni. An Fe_1·5CoNi_0.5 (Fe:Co:Ni = 1.5:1:0.5, atomic ratio) metallic coating is fabricated on SUS 430 stainless steel by magnetron sputtering, followed by oxidation in air at 800°C. The Fe_1·5CoNi_0.5 coating is thermally converted to (Fe,Co,Ni)₃O₄ and (Fe,Co,Mn,Ni)₃O₄ without (Ni,Co)O particles. After oxidation for 1680 h, no further migration of Cr is detected in the thermally converted coating region. A low oxidation rate of 5.9 × 10^?14 g² cm^?4 s^?1 and area specific resistance of 12.64 mΩ·cm² is obtained for Fe_1·5CoNi_0.5 coated steels.     

Salt-assisted solution combustion synthesis of NiFe2O4: Effect of salt type

The effects of three types of salt including NaF, KCl, and NaCl on the properties of NiFe₂O₄ nanoparticles using salt-assisted solution combustion synthesis (SSCS) have been investigated. The synthesized powders were evaluated by SEM, TEM, FTIR, XRD, and VSM analysis. Also, the specific surface area (SSA), as well as size distribution and volume of the porosities of NiFe₂O₄ powders were determined by the BET apparatus. The visual observations showed that the intensity and time of combustion synthesis of nanoparticles have been severely influenced by the type of salt. The highest crystallinity was observed in the synthesized powder using NaCl. The SSA has also been correlated completely to the type of salt. The quantities of SSA was achieved about 91.62, 64.88, and 47.22 m²g^-1 for the powders synthesized by KCl, NaCl, and NaF respectively. Although the magnetic hysteresis loops showed the soft ferromagnetic behavior of the NiFe₂O₄ nanoparticles in all conditions, KCl salt could produce the particles with the least coercivity and remanent magnetization. Based on the present study, the salt type is a key parameter in the SSCS process for the preparation of spinel ferrites. Thermodynamic evaluation also showed that the melting point and heat capacity are important parameters for the proper selection of the salt.     

Mg0.5NixZn0.5-xFe2O4 spinel as a sustainable magnetic nano-photocatalyst with dopant driven band shifting and reduced recombination for visible and solar degradation of Reactive Blue-19

Focussing on visible light active ferrites for high performance removal of noxious pollutants, we report the synthesis of Mg_0.5Ni_xZn_0.5-xFe₂O₄ (x = 0.1, 0.2, 0.3, 0.4, & 0.5) ferrite nanoparticle for degradation of reactive blue-19 (RB-19). Lattice parameters calculated using intense X-ray diffraction (XRD) peaks and Nelson-Riley plots (N-R plot) are in well agreement with each other. The sample Mg_0.5Ni_0.4Zn_0.1Fe₂O₄ (M5N4) exhibits best performance with 99.5% RB-19 degradation in 90 min under visible light. Photoluminescence (PL) results confirm that recombination of charge carriers is highly reduced in the photocatalyst. Scavenging experiments suggest that O₂⁻ radicals were the dominant species responsible for photocatalytic performance. The photocatalytic mechanism was explained in terms of dopant driven shifting of conduction bands and valence bands (calculated by Mott-Schottky plots). The thermodynamic probability of radical generation along with role of redox cycles of metal ions has been discussed in the mechanism. The dye degradation was ascertained by detection of intermediates via mass spectrometry analysis and a possible degradation route was also predicted. The findings in this work provide intriguing opportunities to modify the electronic band structure of spinel ferrites for visible and solar light photocatalytic activity for environmental detoxification.     

Structural,magnetic, thermal and optical properties of Sn2+ cation doped magnetite nanoparticles

Tin doped nanomagnetites, Sn_xFe_3-xO₄, were synthesized with various concentrations of Sn²⁺ ion (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0) by co-precipitation method. XRD, VSM, TG-DTA, SEM-EDX and UV–Vis were used to characterize and study the structural, magnetic, thermal, and optical properties of Sn_xFe_3-xO₄ nanoparticles. XRD confirmed the presence of cubic structure and spinel phase of tin doped magnetites. The d-spacing, lattice parameter, density, crystallite size and cation distribution were derived from the XRD analysis. The M − H curves exhibited changes in saturation magnetization (M_s), coercive field (H_c), remanent magnetization (M_r) and susceptibility (χ), with increasing concentration of non-magnetic Sn²⁺ ions. Differential thermal analysis was used to study the thermal stability of Sn_xFe_3-xO₄ nanoparticles. The SEM images revealed the surface morphology of the nanoparticles and the EDX spectra showed an increase in the Sn content and a corresponding decrease in the Fe content for the tin doped samples. The optical bandgap was found to be centered at 3.9 eV for the synthesized materials. This systematic study may be the first comprehensive report on synthesis and characterization of tin doped magnetites.     

Distribution of carbon contamination in MgAl2O4 spinel occurring during spark-plasma-sintering (SPS) processing: I – Effect of heating rate and post-annealing

Carbon contamination from the carbon paper/dies during spark-plasma-sintering (SPS) processing was examined in the MgAl₂O₄ spinel. The carbon contamination sensitively changes with the heating rate during the SPS processing. At the high heating rate of 100 °C/min, the carbon contamination having organized structures occurred over almost the entire area from the surface to deep inside the SPSed spinel disk. In contrast, at the slow heating rate of 10 °C/min, the carbon contamination having disordered structures occurred only around the surface area. The carbon phases transform into high pressure CO/CO₂ gases by post-annealing in air and lead to pore formation along the grain junctions. The pore formation significantly occurs at the high heating rate due to the large amount of the contaminant carbon phases. This suggests that if once the carbon contamination was formed in the materials, it is very difficult to remove the carbon phases from the materials.     

Effect of waste serpentine on the properties of basic insulating refractories

Basic insulating refractories were fabricated by the pressing route using dead-burned magnesia, pure calcined alumina, expanded perlite, and calcined waste serpentine as starting raw materials in four compositions from F1 to F4. Periclase and forsterite were major phases in F1 and F2 compositions, while spinel was also detected in the XRD patterns of F3 and F4 samples. Quantitative phase analysis showed that F4 sample sintered at 1450?°C has the highest forsterite content among all other samples. On the other hand, it has lower thermal conductivity compared to F1 to F3, and even lower than aluminosilicate IFBs with the same bulk density. It is concluded that forsterite is a highly insulating material, compared to periclase, corundum, periclase-spinel, aluminosilicates, such as mullite, etc.     

Kinetic analysis of magnesium aluminate spinel formation: Effect of MgO:Al2O3 ratio and titania dopant

The mechanistic pathway of MgO-Al₂O₃ reaction in solid state to form MgAl₂O₄ spinel was investigated to correlate the kinetic parameters with ratio of reactants (MgO:Al₂O₃) and with the presence of a doping agent, TiO₂. The time-temperature-expansion data of oxide compacts was analyzed using several model free analyses and model based (linear and non-linear) kinetic algorithms. These indicated that spinel formation process can be best described by single step with n-dimensional Avrami equation for every MgO:Al₂O₃ ratio, irrespective of titania dopant. The activation energy (E_a) of the process was proportional to % spinel formed in each system and validated with quantitative XRD analysis. The higher value of Avrami coefficient (n) in 90 wt% Al₂O₃ compositions has been explained with geometric considerations of powder packing. Incorporations of 1% TiO₂ in the MgO: Al₂O₃ oxide compact did not markedly affect the reaction model, frequency factor and Activation energy.     

Formation and properties of high entropy oxides in Co-Cr-Fe-Mg-Mn-Ni-O system: Novel (Cr,Fe,Mg,Mn,Ni)3O4 and (Co,Cr,Fe,Mg,Mn)3O4 high entropy spinels

Possibility of formation of quinary and senary equimolar high entropy oxides from the Co-Cr-Fe-Mg-Mn-Ni-O system is presented. Different proposed compositions are synthesized using the solid-state reaction route at high temperatures (900−1100 °C) and quenched to room temperature. Phase composition of the samples is studied, showing tendency toward formation of two main phases: rock salt-structured Fm-3 m and spinel-structured Fd-3 m. It is documented that the annealing temperature has a profound effect on stability of both structures, and at 1100 °C usually the highest content of Fm-3 m phase is usually observed. Three different oxides, namely, (Co,Cr,Fe,Mn,Ni)₃O₄, (Co,Cr,Fe,Mg,Mn)₃O₄ and (Cr,Fe,Mg,Mn,Ni)₃O₄ are obtained as single-phase materials, which structure can be described as the high entropy Fd-3 m spinel one. The latter two compounds have not been previously reported in the literature. Activated character of the electrical conductivity dependence on temperature is observed, with relatively high total conductivity at high temperatures and corresponding high absolute values of Seebeck coefficient.     

Mg-doped LiNi0.5Mn1.5O4 spinel for cathode materials

Lithium-ion batteries are becoming more and more important not only for portable electronic devices, but also in prevision of high power electric vehicles. In such an optic, deep studies regarding all the components of a secondary battery are in development. In this study, high voltage cathode materials have been selected. Crystals with spinel structure have a 3D vacancy pathway suitable for Li-ions transport. The material under study was LiNi_0.5Mn_1.5O₄ doped with magnesium replacing the nickel. Various samples were synthesized via three different routes: a solid-state method, a modified sol–gel method and a xerogel method. The structure and morphology of the powders were analyzed with HRTEM and XRD. Electrochemical tests were also performed. A wide range of particle sizes (from micro to nanosize) was the result of the different synthesis routes. Unfortunately pure materials were not always obtained. The electrochemical tests showed improvement of the material's cyclability, by reducing the particle size. The electrochemical tests further confirmed the existence of a Li_1+dMn_2−dO₄ impurity. The results are quite promising, however, further improvement of the purity of the electrode composition are needed.