Microstructural,magnetic and electric properties of sol-gel synthesized Na0.5Bi0.5TiO3–CoFe2O4 composites

In this work, we presented investigations on the microstructural, magnetic, dielectric and conductive properties of (1-x)Na_0.5Bi_0.5TiO₃-xCoFe₂O₄ (NBT-CFO) composite ceramics (x = 0.1, 0.2, 0.3 and 0.5). The composites were synthesized using the in-situ sol-gel method, and the resulting CFO/NBT embedded structure was observed in the 0.9NBT–0.1CFO sample. Rietveld refinement confirmed that the embedded structure had remarkable effects on the c/a ratios of NBT-CFO composites. Increasing normalization saturation magnetizations were observed with increasing of CFO contents, thus revealing the influence of phase interfaces on magnetism. Dielectric relaxation anomalies were observed on both temperature dependent permittivity and loss spectra. Two sets of anomalies in these spectra were caused by space charges on the phase interfaces of embedded CFO grains and the NBT matrix. The conduction behavior of ceramics with and without the embedded structure obeyed the double power law and Jonscher's fraction power law, respectively, which inferred a transformation from the AC to the DC conduction mechanism with the disappearance of the embedded structure.     

Tuning the dielectric,ferroelectric and electromechanical properties of Ba0.83Ca0.10Sr0.07TiO3–MnFe2O4 multiferroic composites

We report the successful synthesis of Ba_0.83Ca_0.10Sr_0.07TiO₃–MnFe₂O₄ multiferroic composites showing significant improvement in electromechanical and magnetoelectric properties. All the composite samples have formed a diphasic perovskite-ferrite composite without the presence of any impurity or intermediate phase. The bare as well as composite samples have shown classical dielectric behavior even at higher ferrite substituted samples. The electrical characteristics of composite samples have shown slight deterioration, which is mainly attributed to non-ferroelectric MnFe₂O₄. However, the composites still exhibit high enough piezoelectric behavior and the modification in the electromechanical response of composites is mainly caused by a change in applied stress with MnFe₂O₄ addition. The M-H loops of composites have demonstrated a ferrimagnetic behavior with a substantial increase in saturation magnetization on increasing the ferrite concentration. Further, the composites have shown better coupling between the ferroelectric and ferrimagnetic phases, which has resulted in an improved magnetoelectric characteristic. The role of oxygen vacancies on ferroelectric and magnetic properties of prepared composites has been systematically studied.     

Effect of mechanical milling on structural,dielectric and magnetic properties of BaTiO3–Ni0.5Co0.5Fe2O4 multiferroic nanocomposites

The coexistence of ferroelectricity and ferromagnetism has triggered great interest in multiferroic materials. Multiferroic with strong room temperature magnetoelectric (ME) coupling can provide a platform for future technologies. In this paper, we have investigated the effect of mechanical milling on the properties of multiferroic nanocomposites synthesized by mixing barium titanate (BaTiO₃) (BT) and nickel cobalt ferrite (Ni_0.5Co_0.5Fe₂O₄) (NCF). This process has resulted into reliable disposal of a given quantity of NCF nanoparticles in BT grid and composite samples of different particle sizes (<500 nm) have been obtained by varying the duration of ball-milling for 12, 24, and 48 h. The presence of NCF within BT powder has been confirmed by X-ray Diffraction (XRD) and magnetization measurements (MH). Structural analysis was performed by using Reitveld refinement method that shows that the tetragonality of BaTiO₃ structure get reduced in submicron range. Variations in ferroelectric and dielectric properties with reduction in particle size/milling duration have been studied by P-E loop tracer and Impedance analyzer. The dielectric constant value of 400 has been observed for BT-NCF0 that increases to 9.7 K for composite sample ball mill at 48 h whereas remnant polarization increases to 4.2 μC/cm². These composites with high dielectric constant that changes with temperature and particles size find application in energy storage devices, sensor and memory devices.     

Room temperature multiferroic properties of BiFeO3–MnFe2O4 nanocomposites

The novel functionalities of multiferroic magneto-electric nanocomposites have spawned substantial scope for fast-paced memory devices and sensor applications. Following this, herein we report the development of nanocomposites with soft ferromagnetic MnFe₂O₄ and ferroelectric BiFeO₃ to fabricate a system with engineered multiferroic properties. A modified sol-gel route called Pechini method is demonstrated for the preparation of the (1-x) BiFeO₃-x MnFe₂O₄ (x = 10%, 30%, 50%, 70%) nanocomposites. The crystallographic phase, structure, and morphology are characterized by XRD, FESEM, and HRTEM. The accurate crystallite size and lattice strain are determined by Williamson-Hall plot method and a comparative study with Scherer's equation is carried out. TEM image evidences the interface between BiFeO₃ and MnFe₂O₄ nanoparticles in the composite. The room temperature magnetic response reveals the strong dependence of magnetic saturation, remanent magnetization, and coercivity of the nanocomposites on MnFe₂O₄ addition. The dielectric response and impedance analysis of the prepared nanocomposites are observed. The electrical performance of the composite is affected by grain, grain boundaries, and oxygen vacancies. The unsaturated P-E loops exhibit the leaky ferroelectric behavior for the nanocomposite. The intrinsic magnetoelectric coupling between ferroelectric BiFeO₃ and ferromagnetic MnFe₂O₄ has been determined by varying H_dc/H_ac and its maximum coupling coefficient (α) is found to be 25.39 mV/cmOe for 70% BiFeO₃ -30% MnFe₂O₄ nanocomposite. These distinctive and achievable characteristics of the nanocomposite would enable the designing of magnetic field sensors, spintronic devices, and multiferroic memory devices.     

Densification,microstructure and microwave dielectric properties of ultra-low fire BaTe4O9–TiTe3O8 ceramic composites

In this study, BaTe₄O₉–TiTe₃O₈ ceramic composites with various amounts of TiTe₃O₈ were prepared, and the densification, microstructural evolution, and dielectric properties of the ultra-low fire ceramic composites were characterized. With the addition of TiTe₃O₈, the ceramic composites were densified at 575 °C with the maximum densities ranging from 93% to 96% of theoretical density. Except the BaTe₄O₉ and TiTe₃O₈ phases, no other second phase was observed in the XRD results. The change in the microstructures caused by the increase of TiTe₃O₈ content appeared to be insignificant. Wide grain size distributions with angular grains in the range of 1–4 μm were observed for all cases. The best dielectric properties – ?_r value of 25, Q × f value of 19,340 GHz, and τ_f value of ?2.7 ppm/°C – were obtained for BaTe₄O₉–40 wt% TiTe₃O₈ ceramic composite sintered at 575 °C, qualifying the ultra-low fire composites for use in the application of ceramic resonators.     

Electrical properties of low-temperature-fired ferrite–dielectric composites

The effects of the BaO·(Nd_0.8Bi_0.2)₂O₃·4TiO₂ (BNBT) to NiCuZn ferrite ratio and addition of Bi₂O₃–B₂O₃–SiO₂–ZnO (BBSZ) glass on the sintering behavior, microstructure evolution, dielectric and magnetic properties of BNBT–NiCuZn ferrite composites were investigated in developing low-temperature-fired composites for high frequency electromagnetic interference (EMI) devices. The results indicate that these composites can be densified at 900 °C and exhibit superior dielectric and magnetic properties with the addition of BBSZ glass. The dielectric system used in the ferrite–dielectric composites reported in the previous studies mostly belong to the ferroelectricity group, which are not suitable for use in the high frequency range (>800 MHz) due to the selfresonance frequency limit. In this study, the dielectric constant remains nearly a constant over a wide range of frequencies (100 MHz to 1 GHz) and the magnetic resonance frequencies are larger than 100 MHz for the BNBT + BBSZ glass–NiCuZn ferrite composites. Therefore, the BNBT + BBSZ glass–NiCuZn ferrite composites can be a good candidate material for high frequency EMI device applications.     

Structural,dielectric and magnetic properties of Bi–Mn doped SmFeO3

We have studied the structural, magnetic, dielectric and impedance properties of the Sm_1-xBi_xFe_1-yMn_yO₃ [SmFeO₃ (SFO), Sm_0.9Bi_0.1FeO₃ (SBFO), Sm_0.9Bi_0.1Fe_0.9Mn_0.1O₃ (SBFMO)] polycrystalline samples synthesized by solid-state reaction method. Rietveld refinement of room temperature (RT) powder x-ray diffraction pattern confirms the orthorhombic crystal structure with Pnma/Pbnm space group. The average particle size of Bi doped and co-doped (Bi–Mn) samples determined from SEM analysis are 5.6 μm and 5.2 μm, respectively. Room temperature field-dependent magnetization increases, suggesting the presence of magnetic contribution due to the Rare earth-Fe ion interaction which persists even at RT. However, with co-doping of Bi and Mn, a decrease in magnetization is observed, which corresponds to the dilution of Fe³⁺-Fe³⁺ interactions due to the presence of Mn³⁺ ions. The observed values of magnetization at 90 kOe for Bi doped sample is (2.87 emu/g) approximately two times and for codoped (0.7 emu/g) sample is nearly half of that of pristine sample (1.51 emu/g). Dielectric measurements as a function of frequency/temperature and impedance analysis using equivalent circuit model reveal grain and grain boundary contributions of SBFO (at high temperature) and SBFMO (for all temperature) samples towards the electrical properties indicating the electrically heterogeneous nature of these samples. However, for SFO sample grain contribution is dominant. Observed value of dielectric constant varies from ~10³-10⁴ with Bi–Mn doping. The conduction mechanism of the studied samples has been explained by considering Jonscher power law. Arrhenius law fitting of AC conductivity data manifests two types of conduction mechanisms in these samples. The depressing nature of the semicircular arc observed in the Nyquist plot of all the samples indicates the presence of a non-Debye type of relaxation.     

Structural,thermal and dielectric properties of AlN–SiC composites fabricated by plasma activated sintering

Highly dense AlN–SiC composites with various SiC additions (0–50?wt-%) were fabricated at 1800°C by plasma activated sintering. The effect of SiC addition on structural, thermal and dielectric properties as well as microwave absorbing performance of the composites was investigated. The thermal conductivity decreases with increasing SiC addition, from 68.7 W (m?K)^?1 for 0?wt-% SiC to 19.38?W (m?K)^?1 for 50?wt-% SiC. On the contrary, the permittivity and dielectric loss increase gradually, from 7.6–8.5 to 22–26.7 and from 0.02–0.1 to 0.2–0.53, respectively. AlN–SiC composite with better thermal and dielectric properties in 30?wt-% SiC, whose thermal conductivity and dielectric loss are found to be 24.88?W (m?K)^?1 and 0.15–0.74, respectively. Furthermore, the composite exhibits microwave absorbing performance with the minimum reflection loss (RL) of ?16.5 dB at 15.5 GHz and the frequency range of 2.6 GHz for RL below ?10 dB (90% absorption).     

Crystal structure and dielectric properties of barium titanate–kaolinite composites

Barium Titanate–Kaolinite composites were prepared systematically by conventional solid-state method. The crystal structure and dielectric properties of samples were investigated by XRD and dielectric measurements, respectively. XRD results show that new phase BaAl₂Si₂O₈ was formed as kaolinite added into BaTiO₃. The 10 wt% kaolinite addition led to a considerable reduction in sintering temperature and a strong densification. The dielectric constant of BaTiO₃–Kaolinite composites tended to be stable with increasing of kaolinite content.     

Thermal properties of field-assisted-sintered SiCN–Y2O3 composites

Polymer-derived amorphous SiCN has excellent high-temperature stability and properties. To reduce the shrinkage during pyrolysis and to improve the high-temperature oxidation resistance, Y₂O₃ was added as a filler. In this study, polymer-derived SiCN–Y₂O₃ composites were fabricated by mixing a polymeric precursor of SiCN with Y₂O₃ submicron powders in different ratios. The mixtures were cross-linked and pyrolyzed in argon. SiCN–Y₂O₃ composites were processed using field-assisted sintering technology at 1350°C for 5 min under vacuum. Dense SiCN–Y₂O₃ composite pellets were successfully made with relative density higher than 98% and homogeneous microstructure. Due to low temperature and short time of the heat-treatment, the grain growth of Y₂O₃ was substantially inhibited. The Y₂O₃ grain size was ∼1 μm after sintering. The composites’ heat capacity, thermal diffusivity, and thermal expansion coefficients were characterized as a function of temperature. The thermal conductivity of the composites ceramics decreased as the amount of amorphous SiCN increased and the coefficient of thermal expansion (CTE) of the composites increased with Y₂O₃ content. However, the thermal conductivity and CTE did not follow the rule of mixture. This is likely due to the partial oxidation of SiCN and the resultant impurity phases such as Y₂SiO₅, Y₂Si₂O₇, and Y_4.67(SiO₄)₃O.     

Rietveld refined crystal structure,magnetic, dielectric,and electric properties of Li- substituted Ni–Cu–Zn ferrite and Sm,Dy co-doped BaTiO3 multiferroic composites

The conventional solid-state reaction technique is used to fabricate the multiferroic xLi_0.1Ni_0.3Cu_0.1Zn_0.4Fe_2.1O₄(LNCZFO)+(1-x)Ba_0.95Sm_0.05Ti_0.95Dy_0.05O₃(BSTDO) composites. To determine the ferrite and ferroelectric phases, the Rietveld refinement analysis is used. The excellent fit of experimental diffraction data is confirmed by the low values of reliability factors and the goodness of fit index, and so the crystal structure is perfect. Increasing the LNCZFO phase in the composites causes the formation of more ferrite grains and enhancement of magnetization values. The anisotropy field varies due to compressive stress created by a lattice mismatch between the BSTDO and LNCZFO phases. The dielectric peak shifts to higher temperatures as the ferrite phase increases, indicating that magnetoelectric interaction between the constituent phases exists in composites. At 100 kHz, the diffuseness exponent ranged from 1.01 to 1.79, indicating that a diffuse phase transition (DPT) occurred for some composites. As the ferrite content increases, the DPT effect decreases, resulting a narrower dielectric peak. The small polaron hopping mechanism is responsible for electrical conduction, which followed Jonscher's power law. The magnitude of the angular frequency exponent factor increases with frequency, indicating an increase in charge carrier mobility from long to short range.     

Phase evolution and microwave dielectric properties of SrTiO3 added ZnAl2O4–Zn2SiO4–SiO2 ceramics

Phase evolution and microwave dielectric properties of SrTiO₃ added ZnAl₂O₄–3Zn₂SiO₄–2SiO₂ ceramics system were investigated. With the addition of SrTiO₃, the sintering temperature for dense ceramic is reduced from 1320 °C to 1180–1200 °C. According to the nominal composition ZnAl₂O₄–3Zn₂SiO₄–2SiO₂-ySrTiO₃, phase evolution is revealed by XRD patterns and Back Scattering Electron images: Zn₂SiO₄, ZnAl₂O₄ and SiO₂ phases coexist at y = 0; SrTiO₃ reacts with ZnAl₂O₄ and SiO₂ to form SrAl₂Si₂O₈, TiO₂ and Zn₂SiO₄ at y = 0.2 to 0.8, and SiO₂ phase disappears at y = 0.8; new phase of Zn₂TiO₄ is obtained at y = 1. The existence of TiO₂ has important effect on the dielectric properties. The optimized microwave dielectric properties are obtained at y = 0.6 and the ceramics show low dielectric constant (7.16), high-quality factor (57, 837 GHz), and low temperature coefficient of resonant frequency (−30 ppm °C⁻¹).     

Microstructure and mechanical properties of Al2O3–YSZ spherical polycrystalline composites

The mechanical behavior and microstructure of highly densified, spherically shaped, polycrystalline Al₂O₃–YSZ composites, processed from pseudoboehmite powders by sol–gel is reported here. Processing was carried out by combining nanometric sized α-Al₂O₃ (120 nm) seeds and YSZ particles of tetragonal structure. The YSZ particles were homogeneously distributed in a coarse-grained matrix of alumina, both inside grains and along grain boundaries. Fracture surfaces, achieved by impact tests showed toughening effects of the zirconia particles. The tetragonality of the YSZ phase stability even after fracture events and fracture toughness measurements by Vickers indentation, where the crack tip interacts with YSZ particles, are all provided and discussed. The local mechanical properties, such as elastic modulus, indentation hardness and the onset of plastic deformation or fracture contact pressure of both YSZ particles and the Al₂O₃ matrix were quantified by nanoindentation. Evidence of coercive contact pressure was observed in YSZ from indentation stress–strain curves.     

Microwave hybrid sintering of Al2O3 and Al2O3–ZrO2 composites,and effects of ZrO2 crystal structure on mechanical properties,thermal properties,and sintering kinetics

Structural ceramics such as Al₂O₃ and Al₂O₃–ZrO₂ composites are widely used in harsh environment applications. The conventional sintering process for fabrication of these ceramics is time-consuming method that requires large amount of energy. Microwave sintering is a novel way to resolve this problem. However, to date, very limited research has been carried out to study the effects of different ZrO₂ crystal structures on Al₂O₃–ZrO₂ composites, especially on the sintering kinetics, when fabricated by microwave sintering.The microwave hybrid sintering of Al₂O₃ and Al₂O₃–ZrO₂ composites was performed in this study. Tetragonal zirconia and cubic zirconia were used as two different reinforcements for an α–alumina matrix, and the mechanical and thermal properties were studied. It was found that Al₂O₃ experienced a remarkable increase in fracture toughness of up to 42% when t-ZrO₂ was added. Al₂O₃–c-ZrO₂ also showed increased fracture toughness. The sintering kinetics were also thoroughly investigated, and the average activation energy values for the intermediate stage of sintering were estimated to be 246 ± 11 kJ/mol for pure Al₂O₃, 319 ± 71 kJ/mol for Al₂O₃–c-ZrO₂, and 342 ± 77 kJ/mol for Al₂O₃–t-ZrO₂. These values indicated that the activation energy was increased by the addition of either type of ZrO₂, with the highest value shown by Al₂O₃–t-ZrO₂.     

Influence of annealing treatment on magnetic properties of Fe2O3/SiO2 and formation of ε-Fe2O3 phase

Magnetic properties of Fe₂O₃/SiO₂ samples were studied after being produced by sol-gel synthesis and formation of ε-Fe₂O₃ polymorph. Samples were thermally treated, using different annealing temperatures and annealing times. The size and morphological characteristics of the iron oxide nanoparticles were examined using a TEM microscope. We used the “ellipticity of shapes”, which is a measure of how much the shape of a nanoparticle differs from a perfect ellipse, in order to quantitatively describe morphological properties of nanoparticles. Coercivity measurements were used to identify and monitor the formation of the epsilon-iron oxide phase during the thermal treatments (annealing). Coercivity values were in the range from 1.2 to 15.4 kOe, which is in accordance with previous experience regarding the existence of ε-Fe₂O₃. We have determined the optimal formation conditions for the ε-Fe₂O₃ polymorph (t=1050 °C for 7 h, H_C=15.4 kOe), as well as the narrow temperature interval (1050–1060 °C) in which the polymorph abruptly vanished (H_C=2300 Oe), on the basis of results of the magnetic properties. The threshold temperature for the ε-Fe₂O₃ phase transformation was measured as 1060 °C. We found that different annealing temperatures and annealing times significantly affected magnetic properties of the examined samples.     

Role of competing phases in the structural,magnetic and dielectric relaxation for (1−x)CoFe2O4+(x)BaTiO3 composites

Magnetoelectric composites of (1−x)CoFe₂O₄+(x)BaTiO₃ (0.0≤x≤1.0) were prepared by ball milling method. X-ray diffraction analysis revealed the presence of cubic spinel (CoFe₂O₄) and tetragonal perovskite (BaTiO₃) phases in the prepared composites. Scanning electron micrographs confirmed the homogeneous phase distribution in the obtained composites. The magnitude of saturation magnetization and linear magnetostriction decreased with increasing BaTiO₃ content in the composite. Significant reduction in the magnetostrictive behavior is attributed to different elastic constants of the constituents which affect the mechanical coupling. In order to identify the different electro-active regions in the prepared composites, the experimental impedance spectroscopic data have been analyzed using different equivalent circuit models. The analysis of the impedance data is carried out by calculating the impedance of conductive (CoFe₂O₄) phase, resistive (BaTiO₃) phase and interconnectivity between the two constituent phases. With increasing BaTiO₃ content ‘x’ in the system, the dielectric permittivity decreased at low frequencies and increased at high frequencies. The observed behavior is mainly ascribed to the polarization in the CoFe₂O₄ and BaTiO₃ phases at low and high frequencies, respectively. Moreover, the AC conductivity analysis suggested the mixed polaron hopping type of conduction mechanism in the prepared composites.     

Ferroelectric hysteresis behavior and dielectric properties of 1–3 lead zirconate titanate–cement composites

Lead zirconate titanate (PZT) ceramic was mixed with Portland cement (PC) to form 1–3 connectivity PZT–PC composite using a dice-and-fill technique. Ferroelectric hysteresis behavior and dielectric properties of these composites were investigated using PZT volume content of 60%, 70% and 80%. The results showed that the dielectric constant of the composite materials increased with PZT content and the dielectric constant (?_r) value is 781 for 80% PZT composite at 1 kHz. The dielectric loss tangent (tan δ) was found to decrease with increasing PZT content and the tan δ value of 80% PZT composite is 0.06. Parallel and series models were also compared to the dielectric measurement results. For the hysteresis measurements, the ferroelectric hysteresis loops can be seen for all composites. The “instantaneous” remnant polarization (P_ir) was found to increase with increasing PZT content from 3.20 to 4.28 μC/cm² at 90 Hz when PZT volume content used was 60% and 80% respectively.     

Preparation of AlN–Al2O3 composites exhibiting antibacterial and water purification properties

This study aimed to develop new antibacterial and water purification materials without heavy metal contamination. Herein, AlN–Al₂O₃ composites were prepared by changing the content of AlN in raw material. The results showed that AlN, Al₂O₃, aluminum oxynitride, and yttrium aluminum garnet phases were generated by adjusting the AlN: Al₂O₃ ratio. The difference in the ability of AlN and aluminum oxynitride to release substances such as ammonium ions and aluminum hydroxide when reacting with water resulted in remarkably different pH values of the sample immersion solution, which led to an increase in the material antibacterial efficiency with the addition of AlN. Similar results were also obtained with zinc ion absorption. Therefore, AlN–Al₂O₃ composite ceramics can potentially be used as novel antibacterial and water purification materials without heavy metal contamination through the release of ammonium ions for conferring antibacterial effects and of aluminum hydroxide for absorbing heavy metals and suspended impurities.     

Sonochemical synthesis and characterization of magnetic separable Fe3O4–TiO2 nanocomposites and their catalytic properties

A novel sonochemical method is described for the preparation of Fe₃O₄–TiO₂ photocatalysts in which nanocrystalline titanium dioxide particles are directly coated onto a magnetic core. The Fe₃O₄ nanoparticles were partially embedded in TiO₂ agglomerates. TiO₂ nanocrystallites were obtained by hydrolysis and condensation of titanium tetraisopropyl in the presence of ethanol and water under high-intensity ultrasound irradiation. This method is attractive since it eliminated the high-temperature heat treatment required in the conventional sol–gel method, which is important in transforming amorphous titanium dioxide into a photoactive crystalline phase. In comparison to other methods, the developed method is simple, mild, green and efficient. The magnetization hysteresis loop for Fe₃O₄–TiO₂ nanocomposites indicates that the hybrid catalyst shows superparamagnetic characteristics at room temperature. Photocatalytic activity studies confirmed that the as-prepared nanocomposites have high photocatalytic ability toward the photodegradation of RhB solution. Furthermore, the photodecomposition rate decreases only slightly after six cycles of the photocatalysis experiment. Thus, these Fe₃O₄–TiO₂ nanocomposites can be served as an effective and conveniently recyclable photocatalyst.     

Effects of graphite nano-flakes on thermal and microstructural properties of TiB2–SiC composites

In the last decades, the production of ultra-high temperature composites with improved thermo-mechanical properties has attracted much attention. This study focuses on the effect of graphite nano-flakes addition on the microstructure, densification, and thermal characteristics of TiB₂–25 vol% SiC composite. The samples were manufactured through spark plasma sintering process under the sintering conditions of 1800 °C/7 min/40 MPa. Scanning electron microscopy images demonstrated a homogenous dispersion of graphite flakes within the TiB₂–SiC composite causing a betterment in the densification process. The thermal diffusivity of the specimens was gained via the laser flash technique. The addition of graphite nano-flakes as a dopant in TiB₂–SiC did not change the thermal diffusivity. Consequently, the remarkable thermal conductivity of TiB₂–SiC remained intact. It seems that the finer grains and more interfaces obstruct the heat flow in TiB₂–SiC–graphite composites. Adding a small amount of graphite nano-flakes enhances the densification of the mentioned composite by preventing the grain growth.