Synthesis and magnetic properties of hard magnetic (CoFe2O4)-soft magnetic (Fe3O4) nano-composite ceramics by SPS technology

CoFe₂O₄/Fe₃O₄ nano-composite ceramics were synthesized by Spark Plasma Sintering. The X-ray diffraction patterns show that all samples are composed of CoFe₂O₄ and Fe₃O₄ phases when the sintering temperature is below 900 °C. It is found that the magnetic properties strongly depend on the sintering temperature. The two-step hysteresis loops for samples sintered below 500 °C are observed, but when sintering temperature reaches 500 °C, the step disappears, which indicates that the CoFe₂O₄ and Fe₃O₄ are well exchange coupled. As the sintering temperature increases from 500 to 800 °C, the results of X-ray diffractometer indicate the constriction of crystalline regions due to the ion diffusion at the interfaces of CoFe₂O₄/Fe₃O₄ phases, which have great impact on the magnetic properties.     

Effect of microstructural characteristics on the magnetic properties of sol-gel synthesized ZnMnO

In this paper we report the effect of microstructural characteristics on the magnetic properties of sol-gel synthesized Mn-doped ZnO. The microstructural characteristics of the samples (e.g., grain sizes and their distribution) have been varied by changing the sintering temperature (T_S) and sintering duration (T_H). Weak room temperature ferromagnetism (RTFM) has been observed in the samples sintered for ∼8 h at 500, 600, 700, 800 and 900 °C. The ferromagnetic fraction and the saturation magnetization, however, first increase as T_S increases from 500 to 600 °C and after that both start decreasing. On the other hand, the samples sintered for ∼12 h at the same temperatures show paramagnetic behavior at room temperature. Field emission scanning electron microscope (FESEM) results show enhancement in the grain sizes with the increase in both T_S and T_H. Energy dispersive X-ray (EDAX) results show increase in the oxygen content in the sample with increase in both T_S and T_H. X-ray diffractometer (XRD) measurements reveal that the basic crystal structure of all the samples corresponds to the wurtzite structure of pure ZnO together with some minor impurities. The correlation between the observed magnetic properties and the microstructural characteristics of the samples has been discussed in this paper.     

Fabrication of solid oxide fuel cell based on doped ceria electrolyte by one-step sintering at 800 °C

Ce_0.8Gd_0.05Y_0.15O_1.9 (GYDC) electrolyte was prepared by a carbonate co-precipitation method. Lithium nitrate at 1, 1.5, 2 and 3 mol% was added to GYDC as sintering additive. 96% relative density was achieved for GYDC at sintering temperature of 800 °C with addition of 1.5 mol% LiNO₃. The conductivities of GYDC with sintering aids LiNO₃ were measured by a.c. impedance spectroscopy and showed comparable values to that of pure GYDC sample sintered at 1400 °C. A single cell with 1.5 mol% LiNO₃ infiltrated GYDC electrolyte was fabricated by sintering at 800 °C for only 2 h. Lithiated NiO was synthesized by the glycine-nitrate combustion method and employed as cathode material. The cell was tested at temperatures from 500 to 575 °C and a maximum power density of 73 mW cm^− 2 was obtained at 575 °C. These preliminary results indicate that LiNO₃ is a very effective sintering additive for intermediate temperature solid oxide fuel cell fabrication.     

Structural studies of annealed neodymia-silica composite synthesized by solgel technique

Nd₂O₃-SiO₂ binary oxide was prepared by solgel technique using tetra-ethoxysilane and neodymium nitrate as precursor materials and HCl as a catalyst. The prepared samples were subjected to heat treatment in the temperature range from 600 to 1100 °C for different time duration. Characterization of heat treated samples was carried out by using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The effect of sintering temperature and time on structural changes of Nd-doped silica has been discussed. The sample sintered at 1100 °C for 12 h shows the formation of monoclinic Nd₂O₃ nanocrystallites in silica matrix with average grain size ∼18 nm.     

Post-sintering annealing effect on the diffuse phase transition in (Pb1−xBax)(Yb0.5Ta0.5)O3 ceramics

The effect of post sintering annealing on the dielectric response of (Pb_1−xBa_x)(Yb_0.5Ta_0.5)O₃ ceramics in the diffuse phase transition range (x=0.2) has been investigated. The samples are prepared by conventional solid-state reaction method. The samples are sintered at 1300 °C for 2 h and annealed at different temperatures (800, 900 and 1000 °C) for 8 h and at 800 °C for different time durations (8, 12 and 24 h). A significant change in the dielectric response has been observed in all the samples. The dielectric constant increases remarkably and the dielectric loss tangent decreases. The dielectric peaks of the annealed samples are observed to be more diffused with noticeable frequency dispersion compared to the as sintered sample.     

Effects of V2O5 addition on NiZn ferrite synthesized using two-step sintering process

The combined influence of a two-step sintering (TSS) process and addition of V₂O₅ on the microstructure and magnetic properties of NiZn ferrite was investigated. As comparison, samples prepared by the conventional single-step sintering (SSS) procedure were also studied. It was found that with 0.3 wt% V₂O₅ additive, the sample sintered by the two-step sintering process at a high temperature of 1250 °C for 30 min and a lower temperature of 1180 °C for 3 h exhibited more homogeneous microstructure and higher permeability with a high Q-factor. The results showed that the TSS method with suitable additive brought positive improvement of the microstructure and magnetic properties of NiZn ferrite.     

Effect of annealing temperature on structure, magnetic properties and optical characteristics in Zn0.97Cr0.03O nanoparticles

The Cr-doped zinc oxide (Zn_0.97Cr_0.03O) nanoparticles were successfully synthesized by sol-gel method. The relationship between the annealing temperature (400 °C, 450 °C, 500 °C and 600 °C) and the structure, magnetic properties and the optical characteristics of the produced samples was studied. The results indicate that Cr (Cr³⁺) ions at least partially substitute Zn (Zn²⁺) ions successfully. Energy dispersive spectroscopy (EDS) measurement showed the existence of Cr ion in the Cr-doped ZnO. The samples sintered in air under the temperature of 450 °C had single wurtzite ZnO structure with prominent ferromagnetism at room temperature, while in samples sintered in air at 500 °C, a second phase-ZnCr₂O₄ was observed and the samples were not saturated in the field of 10000 Oe. This indicated that they were mixtures of ferromagnetic materials and paramagnetic materials. Compared with the results of the photoluminescence (PL) spectra, it was reasonably concluded that the ferromagnetism observed in the studied samples was originated from the doping of Cr in the lattice of ZnO crystallites.     

Effects of sintering temperature and atmosphere on magnetism in Mn-doped TiO2 bulk samples

Magnetic properties have been investigated on Mn doped TiO₂(Ti_0.98Mn_0.02O₂) bulk samples prepared by solid state reaction, which were sintered at different temperature ranging from 450 ^°C to 900 ^°C in air and argon atmosphere, respectively. The results show that the magnetic properties were strongly dependent on the sintering temperature and atmosphere. For samples sintered in air, the magnetization initially increase with the increase of sintering temperature up to 600 ^°C and thereafter it decrease. While the magnetization of samples sintered in argon atmosphere decreases monotonically with the increase of sintering temperature. Furthermore, for samples sintered at 600 ^°C in air, the magnetic susceptibility exhibits a dominant Curie-Weiss behaviour and no magnetic transition is observed over the temperature range from 10 to 300 K. In contrast, for samples sintered in argon atmosphere, besides the magnetic transition near 45 K perhaps caused by Mn₃O₄, another magnetic transition appears near room temperature.     

Solid state reaction synthesis of NiFe2O4 nanoparticles

Ni-ferrite (NiFe₂O₄) nanoparticles have been synthesized via a solid state reaction process. Ni and Fe bi-metallic nanoparticles in the form of Ni₃₃Fe₆₇ alloy nanopowder are first synthesized by simultaneous evaporation of the required amounts of pure Ni and Fe metals followed by rapid condensation of the evaporated metal flux into solid state by means of an inert gas, helium, using the process of inert gas condensation (IGC). In order to form the NiFe₂O₄ structure, as-synthesized samples (Ni₃₃Fe₆₇) are annealed for 12 h in ambient conditions at different annealing temperatures. Structural analyses show that NiFe₂O₄ starts to form at around 450 °C and gets progressively well defined with increasing annealing temperatures yielding particle with size ranging between 15 and 50 nm. Besides successfully forming NiFe₂O₄, NiO/Fe₃O₄ core/shell nanoparticles have also been synthesized by adjusting the annealing conditions. Three different structures, Ni₃₃Fe₆₇, NiO/Fe₃O₄, and NiFe₂O₄, obtained in this study are compared with respect to their structural and magnetic properties.     

Effect of zinc concentration on the structural,electrical and magnetic properties of mixed Mn–Zn and Ni–Zn ferrites synthesized by the citrate precursor technique

Mixed manganese-zinc and nickel-zinc ferrites of composition Mn_0.2Ni_0.8−xZn_xFe₂O₄ where x=0.4$x=0.4$, 0.5 and 0.6 have been synthesized by the citrate precursor technique. Decomposition of the precursor at temperatures as low as 500 °C gives the ferrite powder. The ferrites have been investigated for their electrical and magnetic properties such as saturation magnetization, initial permeability, Curie temperature, AC-resistivity and dielectric constant as a function of sintering temperature and zinc content. Structural properties such as lattice parameter, grain size and density are also studied. The mixed compositions exhibited higher saturation magnetizations at sintering temperatures as low as 1200 °C. While the Curie temperature decreased with zinc content, the permeability was found to increase. The AC-resistivity ranged from 10⁵–10⁷ Ω cm and decreased with zinc content and sintering temperature. The dielectric constants were lower than those normally reported for the Mn–Zn ferrites. Samples sintered at 1400 °C densified to about 94% of the theoretical density and the grain size was of the order of about 1.5 μm for the samples sintered at 1200 °C and increased subsequently with sintering temperature.     

Immiscibility in the nickel ferrite-zinc ferrite spinel binary

Immiscibility in the trevorite (NiFe₂O₄)-franklinite (ZnFe₂O₄) spinel binary is investigated by reacting 1:1:2 molar ratio mixtures of NiO, ZnO and Fe₂O₃ in a molten salt solvent at temperatures in the range 400-1000 °C. Single phase stability is demonstrated down to about 730 °C (the estimated consolute solution temperature, T_cs). A miscibility gap/solvus exists below T_cs. The solvus becomes increasingly asymmetric at lower temperatures and extrapolates to stoichiometric parameters = 0.15, 0.8 at 300 °C. A thermodynamic analysis, which accounts for changes in configurational and magnetic ordering entropies during cation mixing, predicts solvus phase compositions at room temperature in reasonable agreement with those determined by extrapolation of experimental results. The delay between disappearance of magnetic ordering above (for NiFe₂O₄) and disappearance of a miscibility gap at T_cs is explained by the persistence of long-range ordering correlations in a quasi-paramagnetic region above T_C.     

Effect of high magnetic field annealing on the microstructure and magnetic properties of Co-Fe layered double hydroxide

The effects of high magnetic field (10 T) on the products obtained by calcination of Co-Fe LDH precursors at different temperatures were investigated. The XRD results indicated that Fe^III substituted for Co^III in Co₃O₄ to yield Co^IICo^IIIFe^IIIO₄ under the calcination of Co-Fe LDH precursors at 400 °C. The products obtained by magnetic field annealing at 400 °C had a porous plate-like morphology, whereas the products without magnetic field annealing were composed of nanoparticles. It was seen that CoFe₂O₄ phase could be formed at low temperature (about 500 °C) under the magnetic field annealing. The grain size of products obtained by magnetic field annealing at 800 °C was larger than that of zero magnetic field. It was found that the saturation magnetization was significantly enhanced after magnetic field annealing, especially at lower temperature (≤600 °C). The possible reason for the effects on the microstructure and magnetic properties of products obtained by magnetic field annealing was discussed.     

The effect of B2O3 addition to the microstructure and magnetic properties of Ni0.4Zn0.6Fe2O4 ferrite

The effects of 0.01 and 0.1 mol B₂O₃ addition to the microstructure and magnetic properties of a Ni–Zn ferrite composition expressed by a molecular formula of Ni_0.4Zn_0.6Fe₂O₄ were investigated. The toroid-shaped samples prepared by pressing the milled raw materials used in the preparation of the composition were sintered in the range of 1000–1300 °C. The addition of 0.01 mol B₂O₃ increased the grain growth and densification giving rise to reduced intergranular and intragranular porosity due to liquid-phase sintering. The sintered toroid sample at 1300 °C gave the optimum magnetic properties of B_r=170 mT, H_c=0.025 kA/m and a high initial permeability value of μ_i=4000. The increment of the B₂O₃ content to 0.1 mol resulted in a pronounced grain growth and also gave rise to large porosity due to the evaporation of B₂O₃ at higher sintering temperatures. Hence, it resulted in an air-gap effect in the hysteresis curves of these samples.     

Effects of precursor types of Fe and Ni components on the properties of NiFe2O4 powders prepared by spray pyrolysis

The effects of the precursor types of Ni and Fe components on the morphology, mean size, and magnetic property of NiFe₂O₄ powders prepared by spray pyrolysis from the spray solution, with citric acid were studied. The precursor powders with hollow and thin wall structure turned to the nano-sized NiFe₂O₄ powders after post-treatment at a temperature of 800 °C. The nickel ferrite powders obtained from the spray solution with ferric chloride had nanometer sizes and narrow size distributions irrespective of the types of nickel precursor. The nickel ferrite powders obtained from the spray solution with ferric nitrate and nickel chloride also had nanometer size and narrow size distribution. The saturation magnetizations of the NiFe₂O₄ powders changed from 37 to 42 emu/g according to the types of the Fe and Ni precursors. The saturation magnetizations of the NiFe₂O₄ powders increased with increasing the Brunauer-Emmett-Teller (BET) surface areas of the powders.     

Effects of sintering temperature on grain growth and the complex permeability of Co0.2Ni0.3Zn0.5Fe2O4 material prepared using mechanically alloyed nanoparticles

Nanoparticle-sized Co_0.2Ni_0.3Zn_0.5Fe₂O₄ was prepared using mechanical alloying and sintering. The starting raw materials were milled in air and subsequently sintered at various temperatures from 600 to 1300 °C. The effects of sintering temperature on physical, magnetic and electrical characteristics were studied. The complex permittivity and permeability were investigated in the frequency range 10 MHz to 1.0 GHz. The results show that single phase Co_0.2Ni_0.3Zn_0.5Fe₂O₄ could not be formed during milling alone and therefore requires sintering. The crystallization of the ferrite sample increases with increasing sintering temperature; which decrease the porosity and increase the density, crystallite size and the shrinkage of the material. The maximum magnetization value of 83.1 emu/g was obtained for a sample sintered at 1200 °C, while both the retentivity and the coercivity decrease with increasing the sintering temperature. The permeability values vary with both the sintering temperature and the frequency and the absolute value of the permeability decreased after the natural resonance frequency. The real part of the permittivity was constant within the measured frequency, while the loss tangent values decreased gradually with increasing frequency.     

Sintering temperature dependence of room temperature magnetic and dielectric properties of Co0.5Zn0.5Fe2O4 prepared using mechanically alloyed nanoparticles

Co_0.5Zn_0.5Fe₂O₄ nanoparticles were prepared using mechanical alloying (MA) and sintering. The crystallite size, coercivity, retentivity and saturation magnetization were also measured. The frequency dependence of dielectric and the magnetic parameters, namely, real permittivity ε′, loss tanget tan δ, real permeability μ′ and loss factor μ″ were measured at room temperature for samples sintered from 600 to 1000 °C, in the frequency range 10 MHz to 1.0 GHz. The results show that the crystallite size of the resulting products ranges between 16 and 67 nm for as-milled sample and the sample sintered at 1000 °C, respectively. The sample sintered at 1000 °C, measured at room temperature exhibited a saturation magnetization of 37 emu g⁻¹. The values of permittivity remain constant within the measured frequency, but vary with sintering temperature. The permeability values, on the other hand however vary with both the sintering temperature and the frequency, thus, the absolute value of the permeability decreased after the natural resonance frequency.     

Wear behavior of sintered hexagonal boron nitride under atmosphere and water vapor ambiences

Hexagonal boron nitride was pressed and sintered at 2000 °C with CaB₂O₄ as an additive to promote its crystallization, which was used as an abradable sealing coating for aircraft turbo engines. Microstructures, phase compositions and tribological properties of the sintered hBN were tested, and the results show that CaB₂O₄ can effectively promote crystal growth of hBN at 2000 °C for 5 h in N₂ ambience. The friction coefficients of the sintered hBN under atmosphere ambience increase as the temperature increasing from room temperature to 400 °C, and then decrease with further increasing of temperature up to 800 °C. Under water vapor ambience, friction coefficients of the sintered hBN are much lower than those under atmosphere ambience, which are attributed to a lamella-slip of hBN and the solid lubrication effect of H₃BO₃.     

Bismuth zinc niobate (Bi1.5ZnNb1.5O7) ceramics derived from metallo-organic decomposition precursor solution

The preparation, microstructure development and dielectric properties of Bi_1.5ZnNb_1.5O₇ pyrochlore ceramics by metallo-organic decomposition (MOD) route are reported. Homogeneous precalcined ceramic powders of 13-36 nm crystallite size were obtained at temperatures ranging from 500 to 700 °C. The thermal decomposition/oxidation of the gelled precursor solution was chemically analyzed, TG/DTA, XRD, and SEM, led to the formation of a pure cubic pyrochlore phase with a stoichiometry close to Bi_1.5ZnNb_1.5O₇ which begins to form at 500 °C. The metallo-organic precursor synthesis method, where Bi, Zn and Nb ions are chelated to form metal complexes, allows the control of Bi/Zn/Nb stoichiometric ratio on a molecular scale leading to the rapid formation of bismuth zinc niobate (Bi_1.5ZnNb_1.5O₇) ceramic fine powders with pure pyrochlore structure. The powders were pressed into pellets and can be sintered at temperatures as low as 800-1000 °C. Fine crystalline ceramics with the grain size in the range of 200-500 nm have been obtained at the sintering temperature of 800 °C. The dielectric properties in high frequency to microwave range were measured and discussed.     

Simple recipe to synthesize single-domain BaFe12O19 with high saturation magnetization

We report a new synthesis route for preparation of single-domain barium hexaferrite (BaFe₁₂O₁₉) particles with high saturation magnetization. Nitric acid, known as a good oxidizer, is used as a mixing medium during the synthesis. It is shown that formation of BaFe₁₂O₁₉ phase starts at 800 °C, which is considerably lower than the typical ceramic process and develops with increasing temperature. Both magnetization measurements and scanning electron microscope micrographs reveal that the particles are single domain up to 1000 °C at which the highest coercive field of 3.6 kOe was obtained. The best saturation magnetization of ≈60 emu/g at 1.5 T was achieved by sintering for 2 h at 1200 °C. Annealing at temperatures higher than 1000 °C increased the saturation magnetization, on the other hand, decreased the coercive field which was due to the formation of multi-domain particles with larger grain sizes. It is shown that the best sintering to obtain fine particles of BaFe₁₂O₁₉ occurs at temperatures 900-1000 °C. Finally, magnetic interactions between the hard BaFe₁₂O₁₉ phase and impurity phases were investigated using the Stoner-Wohlfarth model.     

NiO+YSZ anode substrate for screen-printing fabrication of YSZ electrolyte film in solid oxide fuel cell

Anode substrate has a great effect on screen-printing fabrication of yttria-stabilized zirconia (YSZ) electrolyte film and cell performance. In this work, NiO+YSZ anode substrate was prepared by a conventional ceramic sintering method, on which dense YSZ electrolyte film was successfully fabricated by screen-printing method. Microstructure of the anode substrate and cell performance were investigated. The optimal amount of addition of starch to the anode substrate was 20 wt%. The optimal temperature for pre-sintering of NiO powder was 800 °C. A single cell with the NiO powder pre-sintered at 800 °C exhibited the highest power density of 0.95 W cm⁻² at 700 °C.