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D. Czekaj, J. Micior and A. Lisińska-Czekaj

Abstract

Goal of the present research was to fabricate and study two-phase BiNbO4//PVDF composites with 0-3 connectivity. Such composite consists of there-dimensionally connected polymer matrix loaded with dielectric ceramic particles. In the present case BiNbO4 powder acted as an active phase (dispersed phase) whereas polyvinylidene fluoride (PVDF) acted as a non-active (passive) phase (matrix). BiNbO4//PVDF composites with the volume fraction of the ceramic phase cν =2, 4, 6, 8, 10, 16 and 20 vol. % were prepared. Average grain size of BiNbO4 powder was <d>=1.86 μm. It was found that BiNbO4 powder exhibited orthorhombic symmetry with Pnna (52) space group and PVDF polymer powder was α-phase. Minimum of dielectric losses at room temperature were found within the frequency range Δν =103-104 Hz. It was found that composite with cν =10% of ceramic powder exhibited lower values of dielectric permittivity.

Open access

D. Czekaj and A. Lisińska-Czekaj

Abstract

Bismuth niobate (BiNbO4) has attracted attention as a low-fired ceramics with promising microwave application potential. BiNbO4 ceramics was fabricated by mixed oxide method and sintered at temperature T<1000°C. As the sintering aids a small amount of CuO oxide was used. The crystalline structure of the ceramic samples was examined by X-ray diffraction method at room temperature. The Rietveld refinement method was used for analysis of diffraction data. As a result an influence of dopants on crystal structure of bismuth niobate (BiNbO4) ceramics was revealed. It was found that fabricated BiNbO4 ceramics adopted the orthorhombic symmetry (α-BiNbO4 phase, Pnna (52) space group). Small differences in elementary cell parameters were found.

Open access

J. Dzik, A. Lisinska-Czekaj, A. Zarycka and D. Czekaj

Abstract

In the present paper studies on Bi1-xNdxFeO3 for x =0.1-0.4 are reported. The mixed oxide method followed with pressureless sintering was employed for ceramics fabrication. Thermal behavior of stoichiometric mixtures of simple oxide powders, viz. Bi2O3, Nd2O3 and Fe2O3 was studied by simultaneous thermal analysis. It was found that with an increase in neodymium content the weight loss increased from 0.75% to 3.16% for x =0.1 and x =0.4, respectively. It was found that weight loss took place mainly within two temperature ranges, namely ΔT1 ≈(300-400)0C and ΔT2 ≈(600-800)°C. Bi1-xNdxFeO3 ceramics was studied in terms of its phase composition (X-ray phase analysis) and chemical composition (EDS method) at room temperature. It was found that Bi1-xNdxFeO3 suffered structural phase transition from rhombohedral to orthorhombic symmetry with an increase in neodymium concentration x within the range x =(0.2-0.3).

Open access

A. Lisińska-Czekaj, D. Czekaj, K. Osińska and M. Adamczyk

Abstract

Goal of the present research was to investigate the influence of V2O5 additive on the structure and dielectric properties of BiNbO4 ceramics. To fabricate BiNbO4 ceramics with V2O5 added the solid state reaction route and pressureless sintering was utilized. Thus obtained ceramics was characterized in terms of its microstructure (SEM), chemical composition (EDS), phase composition and crystalline structure (X-ray phase and structural analysis, respectively). Also dielectric properties in both temperature and frequency domains were investigated. The impedance spectroscopy was utilized for dielectric characterization and the measurements of complex impedance were performed within the frequency range ν =10Hz-1MHz and temperature range T =RT-550°C. It was found that V2O5 additive changed slightly lattice parameters of BiNbO4 ceramics, decreased porosity of samples and revealled relaxation phenomena within the frequency ranges ν =102-103 Hz and ν =105-106 Hz at temperature T>285°C.

Open access

D. Czekaj, A. Lisińska-Czekaj, K. Osińska and K. Biernacki

Abstract

Goal of the present research was to fabricate BiNbO4 ceramics from the mixture of powders by the solid state reaction route and pressureless sintering at various temperatures (TS =8700C and TS =9100C) and study microstructure, phase composition and crystalline structure of BiNbO4 ceramics. Four batches were fabricated and examined, namely the one fabricated from the stoichiometric mixture of reagent - grade oxide powders, viz. Bi2O3 and Nb2O5 as well as the ones with an excess of 3%, 5% and 10% by mole of Bi2O3. It was found that apart from the main orthorhombic -BiNbO4 phase additional phases, namely tetragonal Bi5Nb3O15, and cubic Bi3NbO7 are possible to form from the mixture of bismuth oxide and niobium oxide. It was found that -BiNbO4 ceramics exhibited the orthorhombic symmetry identified as Pnna (52). However, small differences in elementary cell parameters were found for the samples sintered from stoichiometric and non-stoichiometric mixture of initial powders.

Open access

A. Lisińska-Czekaj, M. Rerak, D. Czekaj, M. Lubina, B. Garbarz-Glos and W. Bąk

Abstract

In the present research the tool of broadband dielectric spectroscopy was utilized to characterize dielectric behavior of Bi6Fe2Ti3O18 (BFTO) Aurivillius-type multiferroic ceramics. Dielectric response of BFTO ceramics was studied in the frequency domain (Δν=0.1Hz – 10MHz) within the temperature range ΔT=-100°C – 200°C. The Kramers-Kronig data validation test was employed to validate the impedance data measurements and it was found that the measured impedance data exhibited good quality justifying further analysis. The residuals were found to be less than 1%, whereas the “chi-square” parameter was within the range χ2~10−7−10−5. Experimental data were analyzed using the circle fit of simple impedance arc plotted in the complex Z”-Z’ plane (Nyquist plot). The total ac conductivity of the grain boundaries was thus revealed and the activation energy of ac conductivity for the grain boundaries was calculated. It was found that activation energy of ac conductivity of grain boundaries changes from EA=0.20eV to EA=0.55eV while temperature rises from T=-100°C up to T=200°C. On the base of maxima of the impedance semicircles (ωmτm=1) the relaxation phenomena were characterized in terms of the temperature dependence of relaxation times and relevant activation energy was calculated (EA=0.55eV).

Open access

D. Czekaj, A. Lisińska-czekaj and J. Plewa

Abstract

In the present research technology of compositionally graded barium strontium titanate Ba1-xSrxTiO3 thin films deposited on stainless steel substrates by sol-gel spin coating followed with thermal annealing at T = 650°C is reported. Results of thermal behavior of the sol-gel derived powders with compositions used for fabrication of graded structure (i.e. with Sr mole fraction x = 0.5, 0.4 and 0.3) are described. X-ray diffraction studies of the phase composition and crystal structure of such complex thin film configuration are given. It was found that gel powders exhibited a large total weight loss of about Δm ≈ 44-47%. Three stages of weight loss took place at temperature ranges: below T ≈ 300°C, at ΔT ≈ 300-500°C and between T = 600°C and T = 800°C. Phase analysis has shown that the dominating phase is Ba0.67Sr0.33TiO3 compound while the second phase is Ba0.7Sr0.3TiO3 or Ba0.5Sr0.5TiO3 for “up-graded” and “down-graded” structure, respectively.

Open access

H. Bernard, A. Lisińska-Czekaj, J. Dzik, K. Osińska and D. Czekaj

Fabrication, Structural and AC Impedance Studies of Layer-Structured Bi4Ti3O12 Ceramics

In the present research bismuth titanate Bi4Ti3O12 (BiT) ceramics was synthesized by the standard solid-state reaction method from the mixture of oxides, followed by free sintering at temperature T=1000°C. BiT ceramics was studied in terms of its chemical composition (EDS), crystalline structure (X-ray), microstructure (SEM) and dielectric properties (ac technique of complex impedance spectroscopy) over a range of frequency (ƒ=100Hz to ƒ=1MHz) and temperature (T=200-500°C). Experimental results confirmed the phase formation. It was found that BiT ceramics crystallized in orthorhombic symmetry, best described with Fmmm space group and the following elementary cell parameters: a=5.409(6)°A, b=5.449(2)°A and c=32.816(2)°A. It was also found that BiT ceramics exhibited the plate-like microstructure and stoichiometric chemical composition. Impedance spectroscopy measurements showed contribution of three overlapping relaxation processes (three semicircles in the complex impedance diagrams were observed) ascribed to bulk, grain boundary and electrode/interface polarization phenomena. Impedance data were fitted to the corresponding equivalent circuit using the complex nonlinear least squares (CNLS) method. The ac conductivity for grains, grain boundaries and electrode processes was calculated from CNLS fit of the impedance data and thus the activation energy of ac conductivity (σAC) and relaxation (τ) was calculated for the three revealed components of the impedance spectra from the slopes of σAC and τ versus 1000/T plots (semi log scale) in the range of ΔT=200-500°C.

Open access

B. Garbarz-Glos, A. Lisińska-Czekaj, D. Czekaj and W. Bąk

Abstract

The investigated ceramics were prepared by a solid-state reaction from simple oxides and carbonates with the use of a mixed oxide method (MOM). The morphology of BaTi0.96Si0.04O3 (BTSi04) ceramics was characterised by means of a scanning electron microscopy (SEM). It was found that Si+4 ion substitution supported the grain growth process in BT-based ceramics. The EDS results confirmed the high purity and expected quantitative composition of the synthesized material. The dielectric properties of the ceramics were also determined within the temperature range (ΔT=130-500K). It was found that the substitution of Si+4 ions had a significant influence on temperature behavior of the real (ε’) and imaginary (ε”) parts of electric permittivity as well as the temperature dependence of a.c. conductivity. Temperature regions of PTCR effect (positive temperature coefficient of resistivity) were determined for BTSi04 ceramics in the vicinity of structural phase transitions typical for barium titanate. No distinct maximum indicating a low-temperature structural transition to a rhombohedral phase in BTSi04 was found. The activation energy of conductivity was determined from the Arrhenius plots. It was found that substitution of Si ions in amount of 4wt.% caused almost 50% decrease in an activation energy value.

Open access

A. Lisińska-Czekaj, M. Lubina, D. Czekaj, M. Rerak, B. Garbarz-Glos and W. Bąk

Abstract

Aim of the present research was to apply a solid state reaction route to fabricate Aurivillius-type ceramics described with the formula Bi6Fe2Ti3O18 (BFTO) and reveal the influence of processing conditions on its crystal structure. Pressureless sintering in ambient air was employed and the sintering temperatures were 850 and 1080 °C. It was found that the fabricated BFTO ceramics were multiphase ones. They consisted of two Bim+1Fem-3Ti3O3m+3 phases, namely the phase with m=5 (i.e. the stoichiometric phase) and m=4 (i.e. the phase with a reduced number of layers in the slab). Detailed X-ray diffraction patterns analysis showed that both phases adopted the same orthorhombic structure described with Fmm2 (42) space group. The ratio of weight fractions of the constituent phases (m=5): (m=4) was ~30:70.