Sintering of Fe-doped Bi0.5Na0.5TiO3 at < 1000 °C

Fe-doped Bi_0.5Na_0.5TiO₃ ceramics with Fe-ion content varied from 0 to 0.15 at.% were successfully prepared by conventional solid state reaction method. The sintering temperature used was between 850 and 1000 °C. X-ray diffraction patterns showed that all produced ceramics were single phase with a rhombohedral structure. SEM micrographs of the ceramics showed a dramatic change in densification behavior as a result of Fe-ion doping. At 850 °C, the undoped BNT ceramic had a very porous structure. As the Fe-ion concentration increased, the ceramics showed denser microstructures and, for the sample containing 0.15 at.% Fe, a very dense grain structure with almost no porosity was obtained. This microstructural observation agreed well with the measured density whose value increased with increasing Fe content. The relative density of at least 95% was achieved in 0.15 at.% Fe-doped BNT ceramics even when it was sintered at 850 °C. Increasing the sintering temperature only had an effect of increasing the grain size of this sample without appreciably affecting its density. The results of this investigation showed that addition of Fe₂O₃ in BNT could help improve the densification process and significantly reduced the sintering temperature of BNT ceramics.     

Grain growth,densification and electrical properties of lead-free piezoelectric ceramics from nanocrystalline (Ba0.85Ca0.15)(Ti0.90Zr0.10)O3 powder by sol–gel technique

The sintering behavior revealed in the sintering processes of the conventional and a two-step process and electrical properties of the (Ba_0.85Ca_0.15)(Ti_0.90Zr_0.10)O₃ ceramics from the nanocrystalline powders synthesized by a sol–gel technique were systematically studied. It was found that the sintering process of the (Ba_0.85Ca_0.15)(Ti_0.90Zr_0.10)O₃ ceramics made from nanocrystalline powders was significantly improved, the sintering temperature was reduced markedly from 1,540 to 1,280 °C, as well as a high relative density (>97 %) was obtained in the conventional sintering. Under the two-step sintering conditions, the full densification and the most suppression of grain growth was achieved simultaneously. The (Ba_0.85Ca_0.15)(Ti_0.90Zr_0.10)O₃ ceramics from nanocrystalline powders sintered by the two-step sintering technique (sintered at T ₁ of 1,300 °C for 1 min and T ₂ of 1,150 °C for 20 h) exhibited the optimum average grain size of 700 nm and a high relative density of 98 %. The electrical properties of the (Ba_0.85Ca_0.15)(Ti_0.90Zr_0.10)O₃ ceramics were greatly influenced by the grain size and phase structure formed under the both sintering conditions, with sintering temperature and grain size increased, the electrical properties of the (Ba_0.85Ca_0.15)(Ti_0.90Zr_0.10)O₃ ceramics, which made from nanocrystalline powders, shows an enhancing trend: d ₃₃ ~100 pC/N, k _p ~53.3 % for the specimen sintered at 1,300 °C for 1 min and 1,150 °C for 20 h, d ₃₃ ~310 pC/N, k _p ~53.3 % for the specimen sintered at 1,350 °C for 2 h respectively.     

Effect of CuO on the microstructure and electrical properties of Ba0.85Ca0.15Ti0.90Zr0.10O3 piezoceramics

In this study, the effect of CuO content on the microstructure and electrical properties of Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ (BCZT) ceramics was systematically studied. The addition of CuO effectively results in an increase of grain sizes in BCZT ceramics. BCZT ceramics endure a lattice distortion due to the Cu²⁺ part substitution for the Ti⁴⁺ site, and a low-sintering temperature of BCTZ ceramics is induced by the addition of CuO. With increasing CuO content, the dielectric constant and the dielectric loss of BCTZ ceramics decrease, together with the decrease of the remanent polarization and the coercive field. Effects of sintering temperature and dwell time on the microstructure and electrical properties of BCZT ceramics with x = 0.5 mol% CuO were also studied, and an optimum sintering condition helps to further improve its electrical properties. BCZT ceramics with x = 0.5 mol% CuO possess optimum electrical properties: d ₃₃ ~ 403 pC/N and k _p ~ 44.6% when sintered at a low temperature of 1400 °C for 6 h. As a result, BCZT ceramics with a sintering aid of CuO are a promising candidate for the transducer and transformer applications.     

Influence of sintering temperature on microstructure and electric properties of CuO doped alkaline niobate-based lead-free ceramics

In this work, microstructure characteristics, dielectric, piezoelectric and ferroelectric properties of lead-free (K_0.4425Na_0.52Li_0.0375)(Nb_0.87Ta_0.06Sb_0.07)O₃ (KNLNST) doped with 1?mol% copper oxide (CuO) piezoelectric ceramics prepared by a conventional solid-state reaction route are investigated with an emphasis on the influence of sintering temperature. The introduction of CuO could significantly improve the sinterability of KNLNST ceramics. It is found that the tetragonality of the ceramics increases with raising sintering temperature. A dense microstructure with increased grains is developed, probably due to liquid-phase sintering. Both the piezoelectric constant d ₃₃ and planar electromechanical coupling k _p increase with increasing relative density and grain size. The Curie temperature T _C values increase slightly when the sintering temperature is increased. In addition, the KNLNST ceramics doped with 1?mol% CuO show obvious dielectric relaxor characteristics, and the relaxor behavior of ceramics is strengthened by increasing the sintering temperature. The improved piezoelectric and dielectric properties of d ₃₃?=?241?pC/N, k _p?=?0.437, dielectric loss tanδ?=?0.0087, mechanical quality factor Q _m?=?138, dielectric constant ε _r?=?1,304 can be obtained for specimens sintered at 1,080?°C for 3?h.     

Effects of MnO2 and sintering temperature on microstructure, ferroelectric, and piezoelectric properties of Ba0.85Ca0.15Ti0.90Zr0.10O3 lead-free ceramics

Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ + xmol% MnO₂ lead-free ceramics have been prepared by a conventional sintering method and the effects of MnO₂ and sintering temperature on microstructure, ferroelectric, and piezoelectric properties of Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ lead-free ceramics have been studied. The addition of 0.25 mol% MnO₂ promotes grain growth, improves the ferroelectricity of the ceramics and strengthens ferroelectric tetragonal–ferroelectric orthorhombic phase transition near 40 °C. Because of the coexistence of tetragonal and orthorhombic phases and the combinatory effects of soft and hard doping of Mn ions, the ceramic with x = 0.25 exhibits the optimum piezoelectric properties (d ₃₃ = 306 pC/N and k _p = 42.2 %, respectively). Excess MnO₂ inhibits the grain growth and degrades the ferroelectric and piezoelectric properties of the ceramics. Sintering temperature has an important influence on the microstructure, tetragonal–orthorhombic phase transition near 40 °C, ferroelectric and piezoelectric properties of the ceramics. The increase in sintering temperature leads to large grains and more noticeable tetragonal–orthorhombic phase transition near 40 °C, enhances ferroelectricity and thus improves effectively the piezoelectricity of the ceramics. The Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ ceramic sintered at 1350 °C possesses the optimum piezoelectric constant d ₃₃ value of 373 pC/N.     

Improvement in the dielectric properties of Ba6?3x (Nd0.4Bi0.6)8+2x Ti18O54(x?=?1�C1.5) ceramics by LiBSi/BaLiF glass additives

To develop low-temperature-fired Ba_6?3x (Nd_0.4Bi_0.6)_8+2x Ti₁₈O₅₄(x = 1?C1.5, abbreviated as BNBT)-based ceramics, the effects of two kinds of glasses (LiBSi and BaLiF) addition on both the phase structure and dielectric properties of BNBT were investigated. The results indicate that LiBSi and BaLiF glasses can effectively wet the BNBT grain and be used as sintering aids to reduce the sintering temperature from 1,200 to 850 °C without the formation of additional phases. With the addition of 14.38 wt.% LiBSi and 1 wt.% BaLiF, the ceramics sintered at 850 °C show favorable dielectric properties of ??_r = 55, tan?? = 0.00254.     

X-Ray Pole Figure Analysis and Magnetic Properties of Microwave Sintered Sr-M-type Hexagonal Ferrites

Sr-M-type sintered hexagonal ferrites were prepared by the conventional and microwave sintering method. X-ray diffraction and pole figure analysis, scanning electron microscopy (SEM), and Robograph 2 magnetic properties test instrument were applied to character the structure and magnetic properties of sintered ferrites. The XRD results reveal all the sintered samples are composed of SrFe₁₂O₁₉ single phase with obvious c-axis alignment. The sample with MS treatment at 1050 ^°C exhibits the optimum magnetic alignment, showing the optimum (0?0?8) and (1?0?7) pole figures with almost all circular lines focused on the center and at about 30^° of α, respectively. Few pores and optimal densification characters can be seen from the SEM image of strontium ferrites microwave sintered at 1050 ^°C, resulting in the optical magnetic properties as remanence (B _r) of 410.5 mT, coercivity (H _cj) of 372.2 kA/m, and maximum magnetic energy product ((BH)_max) of 31.53 kJ/m³, respectively.     

Low temperature sintering and properties of lead-free (Ba0.85Ca0.15)(Zr0.1Ti0.9)O3 ceramics with Ba(Cu0.5W0.5)O3 addition

The low-temperature sintering behavior of (Ba_0.85Ca_0.15)(Zr_0.10Ti_0.90)O₃ (BCZT) piezoelectric ceramics with Ba(Cu_0.5W_0.5)O₃ (BCW) addition has been investigated. The addition of 0.1 wt% BCW promotes the sinterability of BCZT ceramics owing to the generation of a liquid phase, resulting in a reduction of sintering temperature from 1,540 to 1,350 °C. The piezoelectric coefficient (d ₃₃), and the electromechanical coupling factor (kp) of the BCZT ? 0.1 wt%BCW specimen sintered at 1,350 °C were 555 pC/N and 55 %, respectively, while Curie temperature (Tc) increases from 85 to 95 °C.     

Effect of spark plasma sintering temperature on the phase equilibria and dielectric properties of BaTi2O5 ceramics

The effect of sintering temperature (ranging from 1055 to 1200 °C) on the phase ingredient and dielectric property of the nominal BaTi₂O₅ ceramics (starting with the Ba/Ti of 1:2) fabricated by a spark plasma sintering method were systematically studied. At the first stage, BaTi₂O₅ component was enhanced in the sintering temperature range of 1055–1120 °C; it turned out to be the dominant phase. For these BaTi₂O₅ phase dominated ceramics, the Curie temperature T _c rised on increasing the sintering temperature and saturated around 440 °C with the maximum dielectric constant of 500. Further increasing the sintering temperature, the decomposition of the obtained BaTi₂O₅ into BaTiO₃ extensively happened; the ceramics turned to be the BaTi₂O₅ and BaTiO₃ coexisting state. These ceramics can be characterized by two dielectric anomalies. One at ~420 °C stood for the phase transition of BaTi₂O₅ while the other at ~150 °C stood for the transition of BaTiO₃, which is exceptionally high as the normal BaTiO₃ ceramics. Further increasing the sintering temperature (until 1200 °C) would dramatically enhance the BaTiO₃ phase; the ceramics showed T _c at 130 °C with the maximum dielectric constant of 1800.     

Effects of Europium Substitution on the Microstructure and Electric Properties of Bismuth Ferrite Ceramics

Bi_1−x Eu _x FeO₃ (x=0.00–0.15) ceramics were synthesized by solid state reaction method with rapid liquid phase sintering process at different europium content and the microstructure and electrical properties of the samples were investigated. X-ray diffraction (XRD) studies show that europium substitution has changed the structure of BiFeO₃ from rhombohedral R3c to orthorhombic Pnma and decreased the impurity phase. Raman spectra results also conform that a structure transition occurs at about x=0.20, and indicate that the Eu substitution at Bi site can obviously affect the Bi–O bond. Impedance analyzer measurements show that both dielectric constant and dielectric loss are strongly dependent on the Eu content. The dielectric constant of the Bi_1−x Eu _x FeO₃ increases with increasing Eu content from 0.00 to 0.20, then decreases with increasing Eu content from 0.20 to 0.30. The dielectric constant measured at 100 Hz is 542.0 for the x=0.20 sample, which is about 8.5 times as big as that for unsubsitituted BiFeO₃. The dielectric loss can be effectively decreased by the substitution of Eu for Bi. In addition, the leakage current measurements show that the substitution of Eu can effectively reduce the leakage current density of BiFeO₃.     

Microstructure,ferroelectric, piezoelectric and ferromagnetic properties of BiFeO3–BaTiO3–Bi(Zn0.5Ti0.5)O3 lead-free multiferroic ceramics

Multiferroic ceramics of (0.70?x)BiFeO₃–0.30BaTiO₃–xBi(Zn_0.5Ti_0.5)O₃ + 1 mol% MnO₂ with perovskite structure were prepared by a conventional ceramic technique and the effects of Bi(Zn_0.5Ti_0.5)O₃ doping and sintering temperature on the microstructure, multiferroic and piezoelectric properties of the ceramics were studied. All the ceramics possess a pure perovskite structure and no second phases can be detected. After the addition of a small amount of Bi(Zn_0.5Ti_0.5)O₃ (x ≤ 0.05), the ferroelectric and piezoelectric properties of the ceramics are improved and the grain growth is promoted. However, excess Bi(Zn_0.5Ti_0.5)O₃ (x ≥ 0.10) retards the grain growth, degrades the ferroelectricity and piezoelectricity, and induces two dielectric anomalies at high temperature. The ceramics can be well sintered at the very wide range of low sintering temperatures (880–980 °C) and exhibit good densification (relative density: 96.2–98.4 %) and strong electric insulation. The increase in the sintering temperature promotes the grain growth and improves the ferroelectricity of the ceramics. The ceramic with x = 0.05 sintered at 880–980 °C possesses improved ferroelectric and piezoelectric properties with remanent polarizations P _r of 21.9–28.1 μm/cm², piezoelectric constants d ₃₃ of 125–139 pC/N and planar electromechanical coupling factors k _p of 30.1–32.4 %, and high Curie temperatures T _C of 523–565 °C. A weak ferromagnetism with remanent magnetizations M _r of 0.0411–0.0422 emu/g and coercive fields H _c of 1.70–1.99 kOe were observed in the ceramics with x = 0–0.025.     

Effects of La-doping on microstructure, dielectric and piezoelectric properties of Ba0.85Ca0.15Ti0.90Zr0.10O3 lead-free ceramics

Lead-free (Ba_0.85Ca_0.15)_1?xLa_2/3xTi_0.90Zr_0.10O₃ + 1 mol% MnO₂ ceramics have been prepared an ordinary sintering technique and the effects of La-doping on the microstructure, dielectric and piezoelectric properties of Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ were studied. All the ceramics possess a pure perovskite structure, indicating that La ions are incorporated into Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ lattices to form a lead-free solid solution. The ceramics are transformed from coexistence of orthorhombic and tetragonal phases to pseudocubic phase with the doping level of La increasing. After the doping of La, grain growth is inhibited, ferroelectric-paraelectric phase transition temperature (T _C) is decreased and the degree of diffuse phase transition is increased. The ferroelectricity of the ceramics is weakened after the addition of La. Unlike donor-doped lead zirconate titanate ceramics, the piezoelectric properties of the ceramics are degraded after the partial substitution of La³⁺ for (Ba_0.85Ca_0.15)²⁺ because of the weakness or disappearance of coexistence of orthorhombic and tetragonal phases near room temperature. The (Ba_0.85Ca_0.15)_1?xLa_2/3xTi_0.90Zr_0.10O₃ + 1 mol% MnO₂ ceramic with x = 0 exhibit the optimum piezoelectric properties: d ₃₃ = 277 pC/N and k _p = 30.3 %, respectively.     

Effect of sintering temperature on the microstructure and electrical properties of zirconium doped barium titanate ceramics

Lead-free Ba(Zr_0.15Ti_0.85)O₃ (BZT15) ceramics were synthesized by adopting the solid-state synthesis method. The effect of increasing sintering temperature (T_s) in the range of 1,350–1,450 °C on the microstructure, dielectric, polarization, and electric field induced strain of the ceramics was studied. Fine grained (~260 nm) BZT15 ceramics displayed single phase perovskite structure with relative densities >94 % of the theoretical density. Both grain size and shape were influenced by the sintering parameters. With increase in T_s, not only the maximum dielectric constant decreased from 11,412 to 8,734 along with an increase in the degree of diffuseness, but also interestingly the Curie temperatures were found to vary within an interval of 61–73 °C. Optimum sintering temperature has been found resulting in high remnant polarisation and strain in these ceramics. The properties observed are attributed to a contribution from all polar vectors present in coexistent phases.     

The effect of glass addition on the dielectric properties of barium strontium titanate

Ba_0.7Sr_0.3TiO₃ (BST) ceramics were prepared by the conventional solid state ceramic route. Different weight percentages of twelve different glasses were added to the calcined BST ceramics and sintered. The structure and microstructure of the sintered materials were investigated by X-ray diffraction and Scanning Electron Microscopic techniques. The low frequency dielectric properties of the glass-ceramic composites were measured using LCR meter. Some of the glasses improved the dielectric properties and considerably lowered the sintering temperature. The glasses were prepared and characterized under identical conditions. Among the different glasses, 1.5 wt% addition of 71ZnO–29B₂O₃ lowered the sintering temperature of BST to 975 °C with a dielectric loss of 9 × 10⁻³ and dielectric constant of 875 at 1 MHz. The curie temperature of BST ceramics was found to shift towards lower temperature with glass addition.     

Synthesis,microstructure, and electrical behavior of (Na<Subscript>0.5</Subscript>Bi<Subscript>0.5</Subscript>)<Subscript>0.94</Subscript>Ba<Subscript>0.06</Subscript>TiO<Subscript>3</Subscript> piezoelectric ceramics via a citric acid sol–gel method

Nanosize (Na_0.5Bi_0.5)_0.94Ba_0.06TiO₃ precursor powders were prepared via the citric acid sol–gel method. The ceramics were sintered at 1100–1150 °C. All ceramics exhibit a single-phase perovskite structure. With increasing sintering temperature, the average size of grains in the samples changes slightly from 0.3 to 0.5 µm. All ceramics show obvious dielectric dispersion. Activation energy values were obtained via impedance, electric modulus, and conductivity, respectively, which are in the range of 0.60–1.06 eV. Compared to ceramics synthesized by solid-state reaction method, the as-synthesized samples are fine-grained and have high depolarization temperature and excellent temperature stability of the piezoelectric constant (d ₃₃). The d ₃₃ value of the sample sintered at 1120 °C remains as high as 119 pC N^?1 with increasing annealing temperature to 115 °C, whereas the reduced amplitude of d ₃₃ is only approximately 3%.     

Processing, dielectric properties and impedance characteristics of Na0.5Bi0.5Cu3Ti4O12 ceramics

Na_0.5Bi_0.5Cu₃Ti₄O₁₂ (NBCTO) ceramics were prepared by conventional solid-state reaction method. The phase structure, microstructure and dielectric properties of NBCTO ceramics sintered at various temperatures with different soaking time were investigated. Pure NBCTO phase could be obtained with increasing the temperature and prolonging the soaking time. High dielectric permittivity (13,495) and low dielectric loss (0.031) could be obtained when the ceramics were sintered at 1000 °C for 7.5 h. The ceramics sintered at 1000 °C for 7.5 h also showed good temperature stability (−4.00 to −0.69%) over a large temperature range from −50 to 150 °C. Complex impedances results revealed that the grain was semiconducting and the grain boundaries was insulating. The grain resistance (R_g) was 12.10 Ω cm and the grain boundary resistance (R_gb) was 2.009 × 10⁵ Ω cm when the ceramics were sintered at 1000 °C for 7.5 h.     

Microwave dielectric properties of Bi(Sc<Subscript>1/3</Subscript>Mo<Subscript>2/3</Subscript>)O<Subscript>4</Subscript> ceramics for LTCC applications

A novel microwave dielectric ceramics Bi(Sc_1/3Mo_2/3)O₄ with low firing temperature were prepared via the solid reaction method. The specimens have been characterized using scanning electron microscopy, X-ray diffraction, Raman spectroscopy and DC conductivity. The Bi(Sc_1/3Mo_2/3)O₄ ceramics showed B-site ordered Scheelite-type structure with space group C2/c. Raman analysis indicated that prominent bands were attributed to the normal modes of vibration of MoO₄ ^2? tetrahedra. The dielectric loss of Bi(Sc_1/3Mo_2/3)O₄ ceramics can be depended strongly the bulk conductivity by DC measurement. The superior microwave dielectric properties are achieved in the Bi(Sc_1/3Mo_2/3)O₄ ceramic sintered at 875 °C/4 h, with dielectric constant?~?25, Q?×?f ~?51,716 GHz at 6.4522 GHz and temperature coefficient of resonance frequency ~???70.4 ppm/°C. It is a promising microwave dielectric material for low-temperature co-fired ceramics technology.     

Multiferroic Properties of (Bi0.9Gd0.1FeO)1−x (BaTiO3) x Ceramics

Conventional solid-state reaction method has been employed for the synthesis of polycrystalline (Bi_0.9Gd_0.1FeO)_1?x (BaTiO₃) _x for x=0.1, 0.2 and 0.3, ceramics samples. The effect of BaTiO₃ content on the multiferroic properties of Gd-doped BiFeO₃ ceramics has been presented. Pure perovskite phase with high density has been obtained by optimizing the synthesis approach, calcination and sintering strategies. Structural analysis carried out using X-ray diffraction confirms the formation of desired morphotropic phase. The dielectric properties have been investigated at different concentration of BaTiO₃ as function of temperature, revealing that by increasing the BaTiO₃ content dielectric constant increases while dielectric losses decrease. Magnetic study shows that initially saturation magnetization increases with increase in BaTiO₃ content up to x=0.1; however, afterwards it decreases for higher concentration of BaTiO₃. According to ferroelectric measurements, PE loops (with low coercive field) are observed at room temperature. The remnant polarization (P _r ) has been found to be 0.169, 0.619 and 0.760 μC/cm², respectively, for samples with x=0.1, 0.2 and 0.3. Magnetoelectric coupling in as-synthesized samples has been indirectly deduced by an anomaly observed at magnetic transition temperature.     

Effects of LiF addition on the sintering behavior and microwave dielectric properties of Li<Subscript>2</Subscript>Mg<Subscript>3</Subscript>SnO<Subscript>6</Subscript> ceramics

Li₂Mg₃SnO₆ (abbreviation for LMS) ceramics doped with 1–4 wt% lithium fluoride (LiF) were prepared by the conventional solid-state reaction method. The effects of LiF addition on the phase compositions, sintering behaviors and microwave dielectric properties of LMS ceramics were investigated. A small amount of LiF addition could effectively decrease the sintering temperatures due to the liquid phase in the sintering process and induced no apparent degradation of the microwave dielectric properties. The optimized quality factor values for each composition firstly increased and then decreased with the increase of the LiF content. Whereas, the optimized dielectric permittivity increased with increasing of the LiF content. Distinguished microwave dielectric properties with a dielectric constant (ε _r) of 11.13, a quality factor (Q·f) of 104,750 GHz, and a temperature coefficient of resonant frequency (τ _f ) of ?10.83 ppm/°C were obtained for LMS ceramics sintered at 950?°C doped with 3 wt% LiF, which showed that the materials were suitable for the low temperature co-fired ceramics applications (LTCC).     

Effects of Bi excess on the structure and electrical properties of high-temperature BiFeO3–BaTiO3 piezoelectric ceramics

BiFeO₃–BTiO₃(BF–BT) ceramics as a promising candidate for lead-free high-temperature piezoelectric ceramics were studied with a special emphasis on the compositional dependence of piezoelectric properties. Excess Bi was added to compensate for the evaporation of Bi³⁺ ions during sintering and this addition was found to be effective in improving the piezoelectric properties of BF–BT ceramics. The microstructure, dielectric and piezoelectric properties of excess Bi doped BF–BT ceramics were investigated. Maximum piezoelectric constant d ₃₃ = 142 pC/N and k _p = 0.302 were obtained with 0.04 Bi doping. At the same time, an enhanced Curie temperature T _c, 452 °C, was obtained. The combination of improved piezoelectric properties and increased T _c makes these ceramics suitable for elevated temperature piezoelectric devices.