Enhancement of Sinter Densification of SrO-BaO-Nb2O5-SiO2 Tungsten-Bronze Glass-Ceramics by Doping with P2O5

Densification behaviors of SrO—BaO—Nb₂0₅—SiO₂ based glass—ceramics prepared by conventional sintering were investigated with an emphasis on the influence of P₂O₅ content.Although P₂0₅ dopant did not modify the surface crystallization mechanism,it resulted in a decrease of the glass transition temperature,which facilitates the viscous glass flow necessary for sintering.However,premature crystallization of（Sr,Ba）Nb₂O₆ induced by addition of excess amount of P₂0₅ essentially retarded sintering due to the formation of closed pores in the matrix.The SrO-BaO-Nb₂0₅-Si0₂ glass with 1.0 mol%P₂0₅（SBN-1P） showed the best sinter densification,which was accomplished at about 850℃.     

Densification process of TaC/TaB2 composite in spark plasma sintering

A TaC composite with ∼11 wt% in situ TaB₂ was fabricated by spark plasma sintering at 1600–1900 °C. The densification process was studied by analysis of the densifying shrinkage of the powder compacts. Three distinct stages for densification were determined. The starting powder mixture of TaC, B₄C and Ta completed reaction to form the desired TaC and TaB₂ at temperature <1583 °C. At around ∼1750 °C, the TaC/TaB₂ material significantly improved relative density to ∼95% with rapid grain growth. The final densification took place very rapidly at 1900 °C by releasing a high pressure vapor.     

Preparation of polycrystalline BaTi2O5 ferroelectric ceramics

Polycrystalline BaTi₂O₅ (BT₂) was prepared by solid state sintering in air using BaCO₃ and TiO₂ as starting materials. A rod-like BT₂ sintered bodies in a single phase were obtained above 1025 °C by adding 5 wt.% B₂O₃. The densification of BT₂ sintered bodies decreased with increasing sintering temperature. The maximum permittivity of BT₂ sintered body was 640 at the Curie temperature (T_c) of 461 °C and the frequency of 100 kHz. The addition of B₂O₃ was effective to obtain BT₂ in a single phase at low temperatures with elongated microstructure and to improve the permittivity, indicating the formation of preferred orientation at low temperature was related with liquid-phase sintering mechanism.     

Improvements in mechanical properties of TiB2 ceramics tool materials by the dispersion of Al2O3 particles

TiB₂–Al₂O₃ composites with Ni–Mo as sintering aid have been fabricated by a hot-press technique at a lower temperature of 1530 °C for 1 h, and the mechanical properties and microstructure were investigated. The microstructure consists of dispersed Al₂O₃ particles in a fine-grained TiB₂ matrix. The addition of Al₂O₃ increases the fracture toughness up to 6.02 MPa m^1/2 at an amount of 40 vol.% Al₂O₃ and the flexural strength up to 913.86 MPa at an amount of 10 vol.% Al₂O₃. The improved flexural strength of the composites is a result of higher density than that of monolithic TiB₂. The increase of fracture toughness is a result of crack bridging by the metal grains on the boundaries, and crack deflection by weak grain boundaries due to the bad wetting characters between Ni–Mo and Al₂O₃.     

Low temperature sintering and microwave dielectric properties of ZnTiNb2O8 ceramics with BaCu(B2O5) additions

The phases, microstructure and microwave dielectric properties of ZnTiNb₂O₈ ceramics with BaCu(B₂O₅) additions prepared by solid-state reaction method have been investigated using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The pure ZnTiNb₂O₈ ceramic shows a high sintering temperature of about 1250 °C. However, it was found that the addition of BaCu(B₂O₅) lowered the sintering temperature of ZnTiNb₂O₈ ceramics from above 1250 °C to 950 °C due to the BCB liquid-phase. The results showed that the microwave dielectric properties were strongly dependent on densification, crystalline phases and grain size. Addition of 3 wt% BCB in ZnTiNb₂O₈ ceramics sintered at 950 °C afforded excellent dielectric properties of ?_r = 32.56, Q × f = 20,100 GHz (f = 5.128 GHz) and τ_f = −64.87 ppm/°C. These represent very promising candidates for LTCC dielectric materials.     

Microwave dielectric properties and microstructures of the 11Li2O-3Nb2O5-12TiO2 ceramics with B2O3 addition

The effects of B₂O₃ addition, as a sintering agent, on the sintering behavior, microstructure and microwave dielectric properties of the 11Li₂O-3Nb₂O₅-12TiO₂ (LNT) ceramics have been investigated. With the low-level doping of B₂O₃ (≤2 wt.%), the sintering temperature of the LNT ceramic could be effectively reduced to 900 °C. The B₂O₃-doped LNT ceramics are also composed of Li₂TiO₃ss and “M-phase” phases. No other phase could be observed in the 0.5-2 wt.% B₂O₃-doped ceramics sintered at 840-920 °C. The addition of B₂O₃ induced no obvious degradation in the microwave dielectric properties but increased the τ_f values. Typically, the 0.5 wt.% B₂O₃-doped ceramics sintered at 900 °C have better microwave dielectric properties of ?_r = 49.2, Q × f = 8839 GHz, τ_f = 57.6 ppm/°C, which suggest that the ceramics could be applied in multilayer microwave devices requiring low sintering temperatures.     

Microstructure and mechanical properties of pulsed electric current sintered B4C-TiB2 composites

Monolithic B₄C, TiB₂ and B₄C-TiB₂ particulate composites were consolidated without sintering additives by means of pulsed electric current sintering in vacuum. Sintering studies on B₄C-TiB₂ composites were carried out to reveal the influence of the pressure loading cycle during pulsed electrical current sintering (PECS) on the removal of oxide impurities, i.e. boron oxide and titanium oxide, hereby influencing the densification behavior as well as microstructure evolvement. The critical temperature to evaporate the boron oxide impurities was determined to be 2000 °C. Fully dense B₄C-TiB₂ composites were achieved by PECS for 4 min at 2000 °C when applying the maximum external pressure of 60 MPa after volatilization of the oxide impurities, whereas a relative density of 95-97% was obtained when applying the external pressure below 2000 °C. Microstructural analysis showed that B₄C and TiB₂ grain growth was substantially suppressed due to the pinning effect of the secondary phase and the rapid sintering cycle, resulting in micrometer sized and homogeneous microstructures. Excellent properties were obtained for the 60 vol% TiB₂ composite, combining a Vickers hardness of 29 GPa, a fracture toughness of 4.5 MPa m^1/2 and a flexural strength of 867 MPa, as well as electrical conductivity of 3.39E+6 S/m.     

The effect of P2O5 on the structure,sintering and sealing properties of barium calcium aluminum boro-silicate (BCABS) glasses

The effect of P₂O₅ incorporation on the sintering, flow and crystallization characteristics of BCABS glasses of composition (mol%) 35BaO–15CaO–5Al₂O₃–(37 − x)SiO₂–8B₂O₃–xP₂O₅ (0 ≤ x ≤5) is investigated. It is observed that addition of P₂O₅, removes cations (Ba²⁺ and Ca²⁺) from the silicate network, resulting in an increase in polymerization. This is reflected by a reduction in TEC and an increase in sealing temperature. In addition, the removal of cations for charge compensation causes a change in major crystalline phases formed, from BaSiO₃ to Ba(Al₂Si₂O₈). In addition, beyond 3 mol% P₂O₅, crystallization of phosphate phases is evident. Based upon the flow temperature, glasses with 0, 1 and 2 mol% P₂O₅ are selected for sealing. In these glasses, conversion of Cr to Cr₂O₃ is observed_, yielding improved adhesion. However, the 2 mol% P₂O₅ glass showed an increased crystallization tendency, resulting in incomplete sintering. Therefore, 1 mol% P₂O₅ seems a good compromise for sealing with improved adhesion.     

Dielectric properties of Y2O3 donor-doped Ba0.8Sr0.2TiO3 ceramics

Ba_0.8Sr_0.2TiO₃ ceramics doped with Y₂O₃ from 0 to 0.10 mol% exhibit normal ferroelectric phase transition, while the ceramics doped with Y₂O₃ from 0.20 to 0.30 mol% show a giant dielectric constant behavior with loss less than 0.15 at 1 kHz from −40 °C to 140 °C, which is suggested due to semiconductive grain and the Maxwell–Wagner effect by structure disordering in grain boundary. The analyses of unipolar charge for the semiconductive grain indicate three kinds of dielectric processes: thermally stimulated process of unipolar hopping, dispersion process of dielectric constant with frequency, and phase transition process accompanied with disappearance of giant dielectric constant in cubic phase. The XPS results confirm that some of the barium ions are in low energy state to form e-Ba²⁺ and to provide hopping sites for electrons. The ceramics doped with Y₂O₃ from 0.50 to 0.75 mol% recover the normal ferroelectricity. The possible mechanics are relevant to binding effect of cation vacancies on electrons.     

Microwave dielectric properties and microstructures of MgTa2O6 ceramics with CuO addition

The effect of CuO addition on the microstructures and the microwave dielectric properties of MgTa₂O₆ ceramics has been investigated. It is found that low level-doping of CuO (up to 1 wt.%) can significantly improve the density of the specimens and their microwave dielectric properties. Tremendous sintering temperature reduction can be achieved due to the liquid phase effect of CuO addition observed by scanning electronic microscopy (SEM). The sintered samples exhibit excellent microwave dielectric properties, which depend upon the liquid phase and the sintering temperature. With 0.5 wt.% CuO addition, MgTa₂O₆ ceramic can be sintered at 1400 °C and possesses a dielectric constant (_r) of 28, a Q × f value of 58000 GHz and a temperature coefficient of resonant frequency (τ_f) of 18 ppm/°C.     

Effect of Al2O3 particle size on vacuum breakdown behavior of Al2O3/Cu composite

In order to clarify the effect of Al₂O₃ particle size on the arc erosion behavior of the ceramic-reinforced Al₂O₃/Cu composite, Al₂O₃/Cu composites with different sizes of Al₂O₃ particles were prepared by powder metallurgy, the effect of Al₂O₃ particle size on the characteristics of arc motion was studied, and the mechanism of arc erosion of Al₂O₃/Cu composites was discussed as well. The results show that with decrease in the size of Al₂O₃ particles, the erosion area increases significantly and the erosion pits become shallower. The vacuum breakdown is preferred to appear in the area between Al₂O₃ particle and the copper matrix. Based on the experimental results and theoretical analysis, a particle partition arc model is proposed.     

Microstructure and mechanical properties of small amounts of In2O3 reinforced Pb(ZrxTi1−x)O3 ceramics

Piezoelectric Pb(Zr_xTi_1−x)O₃ (PZT) ceramics with small amount (0.5-2.0 wt.%) of In₂O₃ are prepared by conventional sintering method. Based on X-ray diffraction analysis, the tetragonality of PZT matrix decreases with In₂O₃ content, indicating that In₂O₃ diffuses into PZT matrix. The microstructure of PZT matrix is significantly refined by doping small amounts of In₂O₃. The grain size reduction and the matrix grain boundary reinforcement are the probable mechanism responsible for the high strength and hardness in the PZT/In₂O₃ materials. The enhancement in Young’s modulus is attributed to In³⁺ substitution. The decreased tetragonality with In₂O₃ addition results in less crack energy absorption by domain switching and, hence, causes the small reduction in fracture toughness.     

Enhanced piezoelectric and mechanical properties of ZnO whiskers and Sb2O3 co-modified lead zirconate titanate composites

ZnO whiskers and Sb₂O₃ co-modified lead zirconate titanate (denoted as PZT/ZnO_w/Sb₂O₃) piezoelectric composites were fabricated using a solid state sintering technique. The characteristic diffraction peaks of the PZT perovskite and ZnO phases were identified from all the composites, suggesting the retention of these individual phases. The grain size of PZT was found to be reduced with Sb₂O₃ addition. A high relative density of 96.5%-99.1% was achieved in PZT co-doped with ZnO_w and Sb₂O₃. Both the piezoelectric and mechanical properties of the PZT/ZnO_w/Sb₂O₃ composites showed significant improvement over the monolithic PZT. The intrinsic effects of ZnO_w and Sb₂O₃ on the electrical and mechanical properties of the PZT/ZnO_w/Sb₂O₃ composites were discussed.     

Molten salt synthesis and thermoelectric properties of Ca2Co2O5

A molten salt method was applied to synthesize Ca₂Co₂O₅ powder by using Co₃O₄ and CaCO₃ as raw materials and CaCO₃-CaCl₂ as eutectic salt. The formation process and molten salt mechanism of Ca₂Co₂O₅ were investigated by powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that sheet-like particles can be obtained at 963 K. Moreover, the electrical conductivity and the Seebeck coefficient of the specimen were measured from 323 to 963 K. The properties increased with increasing temperature and the highest value of power factor (2.0 × 10^− 4 W m^− 1 K^− 2) was obtained at 963 K, which indicates that molten salt synthesis is a promising method to prepare high thermoelectric performance material.     

Multiferroic properties of Pb2Fe2O5 ceramics

Pb₂Fe₂O₅ (PFO) powders in monoclinic structure have been synthesized using lead acetate in glycerin and ferric acetylacetonate as the precursor. The powders were pressed into pellets, which were sintered into ceramics at 800 °C for 1 h. The morphology and structure have been determined by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). Polarization was observed in Pb₂Fe₂O₅ ceramics at room temperature, exhibiting a clear ferroelectric hysteresis loop. The remanent polarization of Pb₂Fe₂O₅ ceramic is estimated to be Pr ∼ 0.22 μC/cm². The origin of the polarization may be attributed to the off-centers of shifted Pb²⁺ ions as well as the FeO₆ octahedra in the perovskite-based structure of Pb₂Fe₂O₅. Magnetic hysteresis loop was also observed at room temperature. The Pb₂Fe₂O₅ ceramic shows coexistence of ferroelectricity and ferromagnetism. It provides a new field of research for complex oxides with multiferroic properties.     

Microstructures and Dielectric Properties of Ba1-xSrxTiO3 Ceramics Doped with B2O3-Li2O Glasses for LTCC Technology Applications

Ba1-xSrxTiO3 ceramics, doped with B2O3-Li2O glasses have been fabricated via a traditional ceramic process at a low sintering temperature of 900 ℃ using liquid-phase sintering aids. The microstructures and di- electric properties of B2O3-Li2O glasses doped Ba1-xSrxTiO3 ceramics have been investigated systemat- ically. The temperature dependence dielectric constant and loss reveals that B2O3-Li2O glasses doped Ba1-xSrxTiO3 ceramics have di?usion phase transformation characteristics. For 5 wt% B2O3-Li2O glasses doped Ba0.55Sr0.45TiO3 composites, the tunability is 15.4% under a dc-applied electric field of 30 kV/cm at 10 kHz; the dielectric loss can be controlled about 0.0025; and the Q value is 286. These composite ceramics sintered at low temperature with suitable dielectric constant, low dielectric loss, relatively high tunability and high Q value are promising candidates for multilayer low-temperature co-fired ceramics (LTCC) and potential microwave tunable devices applications.     

Photocatalytic properties of TiO2-P2O5 glass ceramics

Binary TiO₂-P₂O₅ glasses with 69 mol% and 76 mol% TiO₂ were prepared and converted into glass ceramics by heat-treatments. XRD measurements show that the main crystalline phases precipitated in the glass ceramics are anatase-type TiO₂ crystals or (TiO)₂P₂O₇ crystals, depending on the concentration of titanium constituent. Photocatalytic activities of the glass ceramics were evaluated by the decomposition of methylene blue (MB) and measuring the water contact angle. It is found that the glass ceramics containing anatase crystals exhibit both photocatalytic oxidation activity and highly photo-induced hydrophilicity under UV irradiation with intensity of 1.0 mW/cm².     

Phase relations and microwave dielectric properties of vanadium modified Ba5Nb4O15 ceramics

Microwave dielectric ceramics of Ba₅Nb_4−xV_xO₁₅ (x = 0-1) were prepared by a solid-state reaction method. Vanadium substitution can markedly lower the sintering temperature of Ba₅Nb₄O₁₅ from 1450 to 1100 °C. The X-ray powder diffraction analysis reveals the multiphase nature of this system. A hexagonal-to-orthorhombic phase transition was also observed for the BaNb₂O₆ secondary phase. The microwave dielectric properties, such as τ_f, ε_r and Q × f value, decreased with increasing vanadium content for samples sintered at 1100 °C. There was an apparent increase in τ_f and Q × f value for samples (x ≥ 0.5) sintered at 1200 °C due to the hexagonal-to-orthorhombic phase transition of the BaNb₂O₆ phase. These results suggested that the microwave dielectric properties of multiphase ceramics strongly depended on the phase compositions and the phase transitions.     

Microstructural and piezoelectric properties of low temperature sintering PMN-PZT ceramics with the amount of Li2CO3 addition

PMN-PZT ceramics doped with Li₂CO₃ and Bi₂O₃ as sintering aids were manufactured in order to develop the low temperature sintering ceramics for multilayer piezoelectric transformer, and their micro structural, dielectric and piezoelectric properties were investigated. The sintering aids were proved to lower the sintering temperature of doped PMN-PZT ceramics due to the effect of LiBiO₂ liquid phase. Optimal values for multilayer piezoelectric transformer application, such as electromechanical coupling factor (k_p) of 0.50, mechanical quality factor (Q_m) of 2264, and dielectric constant (K) of 1216, and curie temperature (T_c) of 317 °C were found at 0.1 wt.% Li₂CO₃ added ceramics sintered at 940 °C.     

Structural and impedance properties of KBa2V5O15 ceramics

The polycrystalline sample of KBa₂V₅O₁₅ ceramics was prepared by a mixed oxide method at low temperature (i.e., at 560 °C). The formation of the compound was confirmed using an X-ray diffraction technique at room temperature. Scanning electron micrograph of the material showed uniform grain distribution on the surface of the sample. Detailed studies of dielectric properties of the compound as a function of temperature at different frequencies suggest that the compound has a dielectric anomaly of ferroelectric to paraelectric type at 323 °C, and exhibits diffuse phase transition. Electrical properties of the material were analyzed using a complex impedance technique. The Nyquists plot showed the presence of both grain (>10³ Hz) and the grain boundary (<10³ Hz) effects in the material. Studies of electrical conductivity over a wide temperature range suggest that the compound exhibits the negative temperature coefficient of resistance behavior. The ac conductivity spectrum was found to obey Jonscher's universal power law.