The effect of heat treatment and re-calcination on magnetic properties of BaFe12O19/Fe3O4 nano-composite

In this study a mixture of barium hexaferrite (BaFe₁₂O₁₉) and graphite was subjected to intensive milling in a planetary ball mill in order to synthesize BaFe₁₂O₁₉/Fe₃O₄ magnetic nano-composite. The effects of milling time and post-synthesis heat treatment on the powder characteristics were investigated using XRD, VSM and HRTEM techniques. XRD results showed that barium hexaferrite partially reduced during high-energy ball milling and nano-composite of BaFe₁₂O₁₉/Fe₃O₄ was obtained after 15 h milling of the initial mixture. Analysis of the 40 h milled and then heat-treated samples revealed that reduction of iron oxides proceeded at temperatures above 650 °C. The most intensive peaks of α-Fe were observed in XRD patterns of the samples heat treated at 850 and 950 °C. Magnetic property measurements showed that saturation magnetization of the milled sample increased considerably and coercivity decreased by heat treating at 950 °C. Re-calcination of the aforementioned sample resulted in an increase in coercivity value to 3444.62 Oe. HRTEM image showed nano-crystalline Fe₃O₄ in the structure of 40 h milled sample.     

Ni4Nb2O9 ceramics prepared by the reaction-sintering process

Fabrication of Ni₄Nb₂O₉ ceramics via a reaction-sintering process was investigated. A mixture of raw materials was sintered into ceramics by bypassing calcination and subsequent pulverization stages. Ni₄Nb₂O₉ phase appeared at 1300 °C and increased with increasing soak time. Ni₄Nb₂O₉ content was found >96% in 1350 °C/2 h sintering pellets. A density of 5.71 g/cm³ was obtained for pellets sintered at 1350 °C for 2 h. This reaches 96.5% of the theoretical density. As the sintering temperature increased to 1350 °C, an abnormal grain growth occurred and grains >100 μm could be found. ?_r of 15.4–16.9 are found in pellets sintered at 1200–1300 °C. Q × f increased from 9380 GHz in pellets sintered at 1200 °C to 14,650 GHz in pellets sintered at 1250 °C.     

Development of novel magnetic-dielectric ceramics for enhancement of reflection loss in X band

The purpose of this research was to develop BaFe_9.5Al_1.5CrO₁₉-xCaCu₃Ti₄O₁₂ nanocomposites (x=10%, 20%, 30%, 40%, 50%) and investigate their structural and magnetic features. The substituted barium hexaferrite (BaFe_9.5Al_1.5CrO₁₉) nanoparticles and calcium copper titanate (CaCu₃Ti₄O₁₂) particles were synthesized by the auto-combustion sol-gel method. The structural, chemical composition and morphology of CaCu₃Ti₄O₁₂ (CCTO) and the nanocomposites were investigated by X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy, respectively. The magnetic and microwave properties of nanocomposites were also investigated by vibrating sample magnetometer and vector network analyzer, respectively. The results confirmed that 1100 °C is the optimum synthesis temperature for CCTO, the mean particles size of the CCTO particles changing from 220 nm (at 850 °C) to 2.18 µm (1250 °C). The SEM micrograph revealed that in all of the BaM-xCCTO nanocomposites (x=10%, 20%, 30%, 40%, 50%), the CCTO dielectric particles were attached to the substituted barium hexaferrite nanoparticles, indicating the effectiveness of the adopted synthesis method. Due to the presence of a dielectric phase in the nanocomposites the saturation magnetization decreases from 22 emu/g to 12 emu/g. The coercive field was a slightly larger than substituted barium hexaferrite and increased from 5.558 kOe for substituted barium hexaferrite to 5.813 kOe for BaM-50CCTO due to hindered motion of the domain walls by the dielectric phase and also to the collective behavior of agglomerated barium ferrite nanoparticles. The BaM-30CCTO nanocomposite shows the highest value of reflection loss compared to other nanocomposites. The reflection dip frequency of BaM-30CCTO nanocomposite was −48.85 dB at 10.93 GHz.     

Effects of Bi2O3–Li2CO3 additions on dielectric and pyroelectric properties of Mn doped Pb(Zr0.9Ti0.1)O3 thick films

Pb(Zr_0.9Ti_0.1)O₃ pyroelectric thick films adding various amounts of the sintering aids Bi₂O₃–Li₂CO₃ have been deposited on the substrates Al₂O₃ by the screen-printing process, and the dependence of microstructure, dielectric and pyroelectric properties on the content of sintering aids has been studied. When the amount of Bi₂O₃–Li₂CO₃ increases from 0 wt% to 5.4 wt%, the sintering temperature of the thick films decreases from 1100 °C to 900 °C, and the grain size and the lattice constant decrease either, but the density and the dielectric constant increase. The Pb(Zr_0.9Ti_0.1)O₃ thick film with 5.4 wt% of Bi₂O₃–Li₂CO₃ sintered at 900 °C has the maximum pyroelectric coefficient 10.51×10^?8 C/cm^?2 K^?1 and the highest figure-of-merit 10.58×10^?5 Pa^?0.5.     

Far infrared and microstructural studies of mechanically activated nickel manganite

Nickel manganite powder synthesized by calcination of a stoichiometric mixture of manganese (MnO Aldrich 99.9%) and nickel oxide (NiO Merck, 99.5%) containing 0.5 wt% CoO and Fe₂O₃, was additionally mechanically activated in a high energy planetary ball mill for 5–60 min. The resulting powders were uniaxially pressed into disc shape pellets and then sintered for 60 min at 900 °C, 1050 °C and 1200 °C. Morphological changes of the obtained nickel manganite ceramics induced by mechanical activation were monitored using scanning electron microscopy, while changes in structural characteristics were followed using X-ray powder diffraction. Room temperature far infrared reflectivity spectra for all sintered samples were recorded in the frequency range between 50 cm^?1and 1200 cm^?1. The observed spectra for all samples showed the presence of the same oscillators, but their intensities depended on the sintering temperature and the time of mechanical acivation. Transversal and longitudinal optical modes were calculated for six ionic oscillators (four strong, and two shoulders) belonging to the nickel manganite partially inverse spinel structure.     

Preparation of barium hexaferrite coatings using atmospheric plasma spraying

Thick coatings of barium hexaferrite with the compositions BaFe₁₂O₁₉ and BaCoTiFe₁₀O₁₉ were prepared using atmospheric plasma spraying (APS) technology. The coatings were prepared from pre-reacted powders of the desired composition. The as-deposited coatings were poorly crystallized, but their crystallinity was improved with a subsequent annealing. The crystallization mechanism of the sprayed hexaferrites was studied during annealing up to 1300 °C, using X-ray powder diffraction combined with thermal analysis and with electron microscopy including microanalysis. Single-phase coatings were obtained after annealing treatments at 1100–1300 °C. Their magnetic properties showed that they would be suitable for absorbers at microwave and mm-wave frequencies, depending on the coating phase's composition, the crystallinity and the thicknesses.     

Effect of calcination temperature on the fabrication of transparent lutetium titanate by spark plasma sintering

Transparent lutetium titanate (Lu₂Ti₂O₇) bodies were fabricated by spark plasma sintering using Lu₂O₃ and TiO₂ powders calcined from 700 °C to 1200 °C. No solid-state reaction was identified after calcination at 700 °C, whereas single-phase Lu₂Ti₂O₇ powder was prepared at 1100 and 1200 °C. The calcination at 700 °C promoted densification at the early stages of sintering, whereas residual pores at grain boundaries resulted in Lu₂Ti₂O₇ bodies with low transparency. Low-density and opaque Lu₂Ti₂O₇ bodies formed owing to the coarsening of the powder calcined at 1200 °C. The Lu₂Ti₂O₇ body sintered using the powder calcined at the moderate temperature of 1100 °C had a density of 99.5% with the highest transmittances of 41% and 74% at wavelengths of 550 nm and 2000 nm, respectively.     

Morphological and magnetic properties of BaFe12O19 nanoferrite: A promising microwave absorbing material

In this work, ultrapure hexagonal BaFe₁₂O₁₉ nanoferrite was synthesized by a facile co-precipitation method. Formation of single phase was analyzed by using wide angle X-ray diffraction. Crystallite size was found to increase from 50 nm to 78 nm when annealing temperature increased from 800 °C to 1000 °C, respectively. Ferrimagnetic behavior with moderate value of saturation magnetization and coercivity were studied at room temperature with the help of vibrating sample magnetometer (VSM). The electromagnetic radiation (EMR) absorption properties were studied in the frequency range of 2–18 GHz by using Vector Network analyzer (VNA). The maximum EMR absorption of −26.52 dB was observed at a frequency of 5.79 GHz. The FTIR spectra confirm tetrahedral and octahedral sites in BaFe₁₂O₁₉ structure. The surface morphology was analyzed by scanning electron microscopy (SEM), which reveals that the particles are agglomerated into irregular shapes. Particle size was measured with transmission electron microscopy (TEM), which was in correlation with the already calculated size from x-ray diffraction (XRD) spectra.     

Electrochemical and microstructural characteristics of nanoperovskite oxides Ba0.2Sr0.8Co0.8Fe0.2O3−δ (BSCF) for solid oxide fuel cells

Nanoperovskite oxides, Ba_0.2Sr_0.8Co_0.8Fe_0.2O_3?δ (BSCF), were synthesized via the co-precipitation method using Ba, Sr, Co, and Fe nitrates as precursors. Next, half cells were fabricated by painting BSCF thin film on Sm_0.2Ce_0.8O_x (samarium doped ceria, SDC) electrolyte pellets. X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and electrochemical impedance spectroscopy (EIS) measurements were carried out on the BSCF powders and pellets obtained after sintering at 900 °C. Investigations revealed that single-phase perovskites with cubic structure was obtained in this study. The impedance spectra for BSCF/SDC/BSCF cells were measured to obtain the interfacial area specific resistances (ASR) at several operating temperatures. The lowest values of ASR were found to be 0.19 Ω cm², 0.14 Ω cm² 0.10 cm², 0.09 Ω cm² and 0.07 Ω cm² at operating temperatures of 600 °C, 650 °C, 700 °C, 750 °C and 800 °C, respectively. The highest conductivity was found for cells sintered at 900 °C with an electrical conductivity of 153 S cm^?1 in air at operating temperature of 700 °C.     

Influence of heat treatment of powder mixture on the microstructure and optical transmission of Nd:YAG transparent ceramics

Transparent Nd:YAG ceramics were fabricated by solid-state reactive sintering of Y₂O₃, α-Al₂O₃ and Nd₂O₃ powders with TEOS and MgO as sintering aids. The powders were ball-milled, dried, sieved and calcined at different temperatures. Samples sintered at 1745 °C for 10 h were utilized to observe the microstructure and the optical transmission. It is found that heat treatments of the powder mixtures above 600 °C for 1 h are necessary to remove the carbon contamination but below 800 °C for 4 h can avoid strong aggregation of the powder. So there is a room for heat-treatment, between 600 °C and 800 °C that can obtain Nd:YAG ceramics with almost pore-free microstructures and high transparency. Highly transparent Nd:YAG ceramic with 84.3% in-line transmission at 1064 nm was fabricated by sintering the 800 °C-1 h-heat-treated powder mixture at 1745 °C for 50 h. Even at wavelength of 400 nm, the transmittance of the sample reached 82.9% and the optical scattering coefficient was as low as 0.71% cm⁻¹.     

Enhanced sintering behavior of LSGM electrolyte and its performance for solid oxide fuel cells deposited by vacuum cold spray

How to obtain dense La_0.8Sr_0.2Ga_0.8Mg_0.2O₃ (LSGM) electrolyte at low sintering temperature (<1300 °C) is a challenge to improve solid oxide fuel cell (SOFC) performance at intermediate operation temperature. In this study, a double-layer design method for vacuum cold spray (VCS) prepared-LSGM electrolyte assisted with two-step sintering at a low temperature was proposed. The sintering behavior of VCS deposited LSGM layers at 1200 °C was investigated. The LSGM layers became denser in most regions except the appearance of some cracks. Subsequently, the effect of a second LSGM layer on the sintered top layer was studied to block cracks. Results showed that the co-sintered layer with a thickness of approximately 5 μm presented a maximum open circuit voltage of ∼0.956 V at 650 °C and a maximum power density of 592 mW/cm² at 750 °C. Result indicates that the sintering assisted VCS is a promising method to prepare the LSGM electrolyte applied in intermediate temperature SOFCs.     

Structural and electrical properties of Sr2NaNb4O13 thin film grown by electrophoretic method using nanosheets synthesized from K(Sr2Na)Nb4O13 compound

Sr₂NaNb₄O₁₃⁻ (SNNO⁻) nanosheets were exfoliated from the K(Sr₂Na)Nb₄O₁₃ compound that was synthesized at 1200 °C. The SNNO⁻ nanosheets were deposited on a Pt/Ti/SiO₂/Si substrate at room temperature by the electrophoretic method. Annealing was conducted at various temperatures to remove organic defects in the SNNO film. A crystalline SNNO phase without organic defects was formed in the film annealed at 500 °C. However, a SrNb₂O₆ secondary phase was formed in the films annealed above 600 °C, probably due to the evaporation of Na₂O. The SNNO thin film annealed at 500 °C showed a dielectric constant of 74 at 1.0 MHz with a dielectric loss of 2.2%. This film also exhibited a low leakage current density of 9.0 × 10⁻⁸ A/cm² at 0.6 MV/cm with a high breakdown electric field of 0.72 MV/cm.     

Nanosized barium ferrite powders prepared by spray pyrolysis from citric acid solution

Highly crystalline nanosized barium ferrite (BaFe₁₂O₁₉) powders were prepared by spray pyrolysis from a spray solution containing a high concentration of the metal components. The precursor powders obtained from the spray solution containing citric acid were amorphous with a porous and hollow structure. Purely crystalline and fine BaFe₁₂O₁₉ powders were obtained after post-treatment between 700 and 1000 °C and subsequent mechanical grinding in an agate mortar. The mean sizes of the powders post-treated at 700 and 1000 °C were 125 and 550 nm, respectively. The specific magnetization of the powders prepared from the spray solution containing citric acid was 57 emu/g.     

The low-temperature sintering of M-type hexaferrites

The sintering of the M-type hexaferrites, AFe₁₂O₁₉ (A = Ba, Sr), was studied. The effects of the A cation type, the partial CuO substitution for Fe₂O₃ and the Fe deficiency on the sintering were examined. Samples with nominal compositions of Ba_1?zSr_zCu_xFe_y?xO_19?δ (z = 0 or 0.5, x = 0–1.0 and y = 11–12) were prepared with a solid-state reaction at 1000 °C. The CuO addition enhanced significantly the sintering rate of the hexaferrites at temperatures below 1100 °C, while a moderate effect on the sintering was caused by a partial substitution of Sr for Ba. The diffusion studies showed that the CuO addition enabled the reactive liquid-phase sintering of hexaferrites at 1000 °C. The relative sintered densities of the Cu-containing hexaferrite ceramics sintered at 1000 °C for 3 h were around 90%. The addition of CuO had a strong effect on the coercivity, but only a moderate effect on the magnetization of the studied ceramics.     

Characterization of IT-SOFC non-symmetrical anode sintered through conventional furnace and microwave

This work investigated the mechanical and electrical properties of NiO–SDC/SDC anode sintered by two different methods: in a microwave at about 1200 °C for 1 h and in a conventional furnace at 1200 °C with a holding time of 1 h (total sintering time of 21 h). Nano-powders Sm_0.2Ce_0.8O_1.9 (SDC) and NiO were mixed using a high-energy ball mill, followed by the co-pressing technique at a compaction pressure of 400 MPa. No binder was used between the layers. The electrical behaviors of all sintered samples were studied using electrochemical impedance spectra in the frequency range of 0.01–10⁵ Hz under 97% H₂–3% H₂O, an amplitude of 10 mV, and at high temperature range of 600–800 °C. Results indicate that the non-symmetrical NiO–SDC/SDC anode achieved through microwave sintering has finer grain size and higher electrochemical performance. However, hardness and Young׳s modulus increased in the samples sintered through a conventional furnace.     

Pb(Zr0.95Ti0.05)O3 powders and porous ceramics prepared by one-step pyrolysis process using non-aqueous Pechini method

Using non-aqueous Pechini method, Pb(Zr_0.95Ti_0.05)O₃ powders were prepared at low temperature by one-step pyrolysis process. The polymeric gels and powders were characterized using a range of techniques, such as DTG, XRD, SEM, Raman spectroscopy, and laser particle size distribution. The perovskite phase was formed at about 350–400 °C and some oxocarbonate impurities can be detected in all samples after calcining at 400–850 °C by one-step pyrolysis process. Phase pure and porous Pb(Zr_0.95Ti_0.05)O₃ ceramics were obtained without pore formers from the powders by one-step pyrolysis process at 500 °C for 4 h. The relative densities were 87%, 91% and 94% for the ceramics sintered at 1100, 1150 and 1200 °C for 2 h, respectively. The porous ceramics sintered at 1200 °C for 2 h have homogeneously dispersed pores and fine-grain structures with an individual grain size of 0.7–2 μm.     

Study of strontium ferrites substituted by lanthanum on the structural and magnetic properties

M-type strontium ferrites, Sr_0.8La_0.2Fe₁₂O₁₉ have been synthesized by conventional ceramic process. The effects of lanthanum addition and sintering temperature on microstructures and magnetic properties of SrFe₁₂O₁₉ and Sr_0.8La_0.2Fe₁₂O₁₉ samples were investigated. Microstructural analysis of the SrFe₁₂O₁₉ and Sr_0.8La_0.2Fe₁₂O₁₉ specimens, sintered at different temperatures revealed that average grain sizes of SrFe₁₂O₁₉ ferrites were larger than that of Sr_0.8La_0.2Fe₁₂O₁₉ ferrite and increased with increasing sintering temperature. The X-ray diffraction (XRD) results confirmed the strontium hexagonal ferrite phase of SrFe₁₂O₁₉ and Sr_0.8La_0.2Fe₁₂O₁₉ compounds. A maximum coercivity value of 4850 Oe and maximum saturation magnetization value of 102 emu/g were obtained for the SrFe₁₂O₁₉ ferrite sintered at 1150 °C and for the SrFe₁₂O₁₉ and Sr_0.8La_0.2Fe₁₂O₁₉ ferrites sintered at 1300 °C, respectively. The remanence (Mr) of Sr_0.8La_0.2Fe₁₂O₁₉ sample sintered at 1200 °C possesses the maximum value of 60 emu/g.     

Synthesis of BaCeO3 and BaCe0.9Y0.1O3−δ from mixed oxalate precursors

An oxalate precipitation route is proposed for the synthesis of BaCe_1−xY_xO₃ (x = 0 and 0.1) after calcination at 1100 °C. The precipitation temperature (70 °C) was a determinant parameter for producing a pure perovskite phase after calcination at 1100 °C for 1 h. TG/DTA measurements showed that the co-precipitated (Ba, Ce and Y) oxalate had a different thermal behaviour from single oxalates. Despite a simple grinding procedure, sintered BaCe_0.9Y_0.1O_3−δ pellets (1400 °C, 48 h) presented 90.7% of relative density and preliminary impedance measurements showed an overall conductivity of around 2 × 10⁻⁴ S cm⁻¹ at 320 °C.     

Preparation of ultra-fine Sm0.2Ce0.8O1.9 powder by a novel solid state reaction and fabrication of dense Sm0.2Ce0.8O1.9 electrolyte film

A novel solid state reaction was adopted to prepare Sm_0.2Ce_0.8O_1.9 (SDC) powder. A mixed oxalate Sm_0.2Ce_0.8(C₂O₄)_1.5·2H₂O was synthesized by milling a mixture of cerium acetate hydrate, samarium acetate hydrate, and oxalic acid for 5 h at room temperature. An ultra-fine SDC powder with the primary particle size of 5.5 nm was obtained at 300 °C. The ultra-low temperature for the formation of SDC phase was due to the atomic level mixture of the Sm³⁺ and Ce⁴⁺ ions. The crystal sizes of SDC powders at 300 °C, 550 °C, 800 °C, and 1050 °C were 5.5 nm, 11.4 nm, 24.1 nm and 37.5 nm, respectively. The sintering curves showed that the powder calcined at lower temperature was easier to be sintered owning to its smaller particle size. A solid oxide electrolytic cell (SOEC), comprising porous La_0.8Sr_0.2Cu_0.1Fe_0.9O_3−δ (LSCF) for substrate, LSCF–SDC for active electrode, SDC for electrolyte, and LSCF–SDC for symmetric electrode, was fabricated by dip-coating and co-sintering techniques. An extremely dense SDC film with the thickness of 20 μm was obtained at only 1200 °C, which was about 100–300 °C lower than the literatures׳ reports. The designed SOEC was proved to work effectively for decomposing NO (3500 ppm, balanced in N₂), 80% NO can be decomposed at 600 °C.     

The sintering behavior,microstructure, and electrical properties of gallium-doped zinc oxide ceramic targets

The properties of sputtering targets have recently been found to affect the performances of sputtered films and the sputtering process. To develop high-quality GZO ceramic targets, the influences of Ga₂O₃ content and sintering temperature on the sintering behavior, microstructure, and electrical properties of GZO ceramic targets were studied.The results showed that the increase in Ga₂O₃ content from 3 wt% (GZO-3Ga) and 5 wt% (GZO-5Ga) not only inhibited the densification but retarded grain growth. During sintering, ZnGa₂O₄ phase formed before 800 °C, and Zn₉Ga₂O₁₂ phase was found after sintering at 1000 °C. Moreover, after sintering at 1200 °C, the number of Zn₉Ga₂O₁₂ precipitates increased at the expense of ZnGa₂O₄ and ZnGa₂O₄ disappearing completely. The relative density, grain size, and resistivity of GZO-3Ga sintered at 1400 °C in air were 99.3%, 3.3 μm, and 2.8 × 10⁻³ Ω cm, respectively. These properties of GZO ceramics are comparable to properties reported in the literature for AZO sintered in air.