Preparation and microwave dielectric properties of Bi2Ti4O11 ceramics

Single phase of Bi₂Ti₄O₁₁ ceramics, which belong to meta-stable phase compounds, were synthesized by controlling the reaction time through conventional solid-state method. The effects of annealing time on phase composition of Bi₂Ti₄O₁₁ ceramic powders and sintered ceramics were studied by XRD analysis. Second phase Bi₂Ti₂O₇ appeared when the annealing time shorter than 4 h. However, pure phase of Bi₂Ti₄O₁₁ powders can be formed by prolonging the annealing time to 6 h at 1,000 °C. The sintering temperatures on microstructure and microwave dielectric properties of Bi₂Ti₄O₁₁ ceramics were investigated. The results show that ceramics sintered at 1,075–1,175 °C are single phase of Bi₂Ti₄O₁₁ and present two different sizes of prismatic shape grains. Smaller size crystals grow into larger ones with increasing sintering temperature. The ceramics sintered at 1,125 °C reach a maximum density and have a microwave dielectric properties of ε_r = 51.2, Q × f = 3,050 GHz and τ_f = ?297 ppm/°C.     

Synthesis and microwave dielectric properties of Ba4Ti3P2O15 ceramics

Present work introduces a new kind of microwave dielectric ceramic, Ba₄Ti₃P₂O₁₅. Ba₄Ti₃P₂O₁₅ ceramic can be prepared by solid state reaction method and be well densified after being sintered at above 1175 °C for 4 h in air. All the XRD patterns can be fully indexed as single-phase structure. The best microwave dielectric properties can be obtained in ceramic sintered at 1200 °C for 4 h with permittivity about 20.7, Q × f about 42,210 GHz and TCF about 37 ppm °C^?1. Measurements of the microwave dielectric properties of Ba₄Ti₃P₂O₁₅ ceramic revealed the existence of a maximum in the temperature dependence of the dielectric loss because of the defect dipoles relaxation.     

Non-Ohmic and dielectric properties of Ba-doped CaCu3Ti4O12 ceramics

The microstructure, dielectric and electrical properties of Ca_1?x Ba _x Cu₃Ti₄O₁₂ (where x = 0, 0.025, and 0.05) ceramics were investigated. Our microstructural analyses revealed that Ba²⁺ doping ions preferentially form in a secondary phase, and are not introduced into the CaCu₃Ti₄O₁₂ lattice. Grain growth rate of CaCu₃Ti₄O₁₂ ceramics was significantly inhibited by the Ba-related secondary phase particles, resulting in a large decrease in their mean grain size. The dielectric permittivity of CaCu₃Ti₄O₁₂ ceramics decreased with increasing Ba content. Their loss tangent decreased after addition of CaCu₃Ti₄O₁₂ with 2.5 mol% of Ba²⁺, and increased with increasing Ba contents to 5.0 mol%. The nonlinear coefficient and breakdown field of the Ca_1?x Ba _x Cu₃Ti₄O₁₂ ceramics were significantly enhanced by adding 2.5 mol% of Ba²⁺, followed by a slight decrease as Ba²⁺ concentration was increased to 5.0 mol%. Using impedance spectroscopy analysis, it was revealed that variations in dielectric and non-Ohmic properties are associated with electrical response of grain boundaries. This supports the internal barrier layer capacitor model.     

Microstructures and microwave dielectric properties of low-temperature sintered Ca2Zn4Ti15O36 ceramics

Low-temperature sintered Ca₂Zn₄Ti₁₅O₃₆ microwave dielectric ceramic was prepared by conventional solid state reaction method. The influences from V₂O₅ addition on the sintering behavior, crystalline phases, microstructures and microwave dielectric properties were investigated. The crystalline phases and microstructures of Ca₂Zn₄Ti₁₅O₃₆ ceramic with V₂O₅ addition were investigated by X-ray diffraction, scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). V₂O₅ addition lowered the sintering temperature of Ca₂Zn₄Ti₁₅O₃₆ ceramics from 1140 °C to 930 °C. Ca₂Zn₄Ti₁₅O₃₆ ceramic with 5wt% V₂O₅ addition could be densified well at 930 °C, and showed good microwave dielectric properties of ε_r ~ 46, Q × f ~ 13400 GHz, and temperature coefficient of resonant frequency (τ_f) ~ 164 ppm/°C.

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Microwave dielectric properties of Sr2Ce2Ti5O16 ceramics

Sr₂Ce₂Ti₅O₁₆ dielectric ceramics were prepared by conventional solid-state ceramic route. The structure and microstructure of the ceramics were investigated by X-ray diffraction and scanning electron microscopic methods. The Sr₂Ce₂Ti₅O₁₆ has a psuedocubic structure. It has ɛ_r of 113, unloaded quality factor (Q_u × f) of 8000 GHz and temperature coefficient of resonant frequency of 306 ppm/°C. The effects of various dopants on the structure, microstructure and microwave dielectric properties of the material have been investigated. It is found that addition of small amount of dopants such as PbO, Al₂O₃, Nd₂O₃, MoO₃, CeO₂, La₂O₃, Fe₂O₃ and NiO improve the microwave dielectric properties of Sr₂Ce₂Ti₅O₁₆.     

Modified giant dielectric properties of samarium doped CaCu3Ti4O12 ceramics

Effects of Sm³⁺ substitution on the microstructure and dielectric properties of CaCu₃Ti₄O₁₂ ceramics were investigated. The grain size of CaCu₃Ti₄O₁₂ ceramics was greatly decreased by doping with Sm³⁺, resulting from the ability of Sm³⁺ to inhibit the grain growth rate. This result can cause a decrease in the dielectric constant (?′) and loss tangent (tan δ) of CaCu₃Ti₄O₁₂ ceramics. Interestingly, high dielectric permittivity (?′ ～ 10,863) and low loss tangent (tan δ ～ 0.043 at 20 °C and 1 kHz) were observed in the Ca_0.925Sm_0.05Cu₃Ti₄O₁₂ ceramic. Nonlinear electrical properties of CaCu₃Ti₄O₁₂ ceramics were modified by doping with Sm³⁺. The dielectric relaxation behavior of Sm-doped CaCu₃Ti₄O₁₂ ceramics can be well ascribed based on the internal barrier layer capacitor model of Schottky barriers at the grain boundaries.     

Low temperature sintering and microwave dielectric properties of Ba4Sm9.33Ti18O54 ceramics

The effect of BaCu(B₂O₅) (BCB) on the sinterability, microstructure and microwave dielectric properties of Ba₄Sm_9.33Ti₁₈O₅₄ (BST) has been investigated. Dilatometric measurements reveal that the sintering temperature of BST can be reduced by the addition of BCB. Microstructural analysis shows abnormal grain growth with large amount of BCB. A ceramic composite with Q × f = 4000 GHz, ?_r = 52 and τ_f = ?29 ppm/°C which can be sintered at 950 °C is obtained when 10 wt% BCB is added to BST. EDS analysis shows that the composite is chemically compatible with silver.     

Influence of sintering temperature on secondary phases formation and microwave dielectric properties of Ca2Ce2Ti5O16 ceramics

Ca₂Ce₂Ti₅O₁₆ dielectric ceramics prepared by conventional solid-state ceramic route was investigated. Phase composition and microwave dielectric properties were measured using XRD and Vector network analyzer, respectively. XRD analysis of the calcined and sintered samples revealed the formation of CeO₂ and another unidentified phase (that vanished at ? 1400 °C) as secondary phases along with the parent Ca₂Ce₂Ti₅O₁₆ phase. The amount of the parent Ca₂Ce₂Ti₅O₁₆ phase increased with increasing sintering temperature from 1350 °C to 1450 °C accompanied by a decrease in the apparent density. The density decreased but ? _r and Q _u f _o increased with sintering temperature. An ? _r ～ 81.5, Q _u f _o ～ 5915 GHz and τ _f ～ 219 GHz were achieved for the sample sintered at 1450 °C.     

Ti4+取代Zn2+、Nb5+对Bi2O3-ZnO-Nb2O5系介质材料结构和性能的影响

研究了Ti4 取代Zn2 ,Nb5 对Bi2O3-ZnO-Nb2O5系介质材料结构和性能的影响,研究表明,少量替代对于材料的结构和性能没有太大的影响;随着替代量的增加,相结构中出现正交Bi4Ti3O12相;微观形貌中出现棒晶,介电常数逐渐增大,温度系数逐渐向负温度系数方向移动,适量Ti4 替代可以获得性能很好的NP0介质材料。     

Effect of different raw materials on the microwave dielectric properties of Ba2Ti9O20 ceramics

Dibarium nona titanate (Ba₂Ti₉O₂₀) dielectric ceramics have been prepared through solid-state route using raw materials of different origin. The dielectric resonator properties are studied in the microwave frequency region. The impurities in the raw materials drastically affect the microwave dielectric properties of Ba₂Ti₉O₂₀. Presence of TiO₂, which deteriorates the temperature coefficient of resonant frequency can be identified clearly by XRD in the range 40–45° of 2.     

Effect of V2O5 and CuO additives on sintering behavior and microwave dielectric properties of BiNbO4 ceramics

The influences of V₂O₅ and CuO additives on the sintering behavior and microwave dielectric properties of BiNbO₄ ceramics were investigated. The V₂O₅ and CuO additives lowered the sintering temperature of BiNbO₄ ceramics to the range 875 °C–935 °C. All BiNbO₄ compounds with additives had the orthorhombic structure. The dielectric constant _r was not significantly changed, while the unloaded Q value was affected with additives. The Qf value was found to be a function of the sintering temperatures and the amount of additives. It varied from 4500 to 15800 (GHz) and 1000 to 8000 (GHz) with additives V₂O₅ and CuO, respectively. The _f values were increased in positive values with V₂O₅ doped, while decreased in negative values with CuO addition. V₂O₅ and CuO additives effectively improved the densification and dielectric properties of BiNbO₄ ceramics. The correlation between the microstructure and the Qf value was observed with different additives.     

Effects of Kaolinite additions on sintering behavior and dielectric properties of CaCu3Ti4O12 ceramics

Commercial Kaolinite was employed as sintering aid to reduce the sintering temperature of CaCu₃Ti₄O₁₂ (CCTO) ceramics. The effects of Kaolinite content and sintering temperature on the densification, microstructure and dielectric properties of CCTO ceramics have been investigated. The density characterization results show that the addition of Kaolinite significantly enhanced the relative density of CCTO ceramics to about 92 %. X-ray diffraction results show CCTO ceramics with a low amount of Kaolinite exhibited perovskite-like structure, but 1.0 wt% Kaolinite additions resulted in the formation of a secondary phase, CaO–TiO₂–Al₂O₃–SiO₂ glass phase was formed and improved the dielectric constant of ceramics, which was supported by scanning electron microscopy–energy dispersive X-ray results. CCTO ceramic with 1.0 wt% Kaolinite addition possessed well temperature and frequency stability of dielectric constant. It was found that Kaolinite lowered the dielectric loss of the samples.     

The microstructure and microwave dielectric properties of zirconium titanate ceramics in the solid solution system ZrTiO4–Zr5Ti7O24

Zirconium titanate (ZT) ceramics having compositions in the range of ZrTiO4-Zr5Ti7O24 were prepared via the mixed oxide route, using ZnO and CuO as sintering aids and Y2O3 as stabilizer. Specimens were sintered at 1450°C for 4 h and then cooled at 6°C h-1, 120°C h-1 or air-quenched. All products exhibited densities exceeding 95% of the theoretical values. The amount of ZnO and CuO in the products decreased as the cooling rate decreased and as the content of TiO2 increased. Energy dispersive analytical spectroscopy studies suggested that a grain boundary phase, rich in ZnO and CuO, existed as a continuous layer. Both composition and cooling rate were found to have significant effects on the microstructure of the zirconium titanate ceramics. Transmission electron microscopy showed that as the TiO2 content increased, a superstructure with a tripled a-axis developed, but there was no obvious change in the lattice parameters. As the cooling rate decreased, extra peaks were observed in X-ray spectra and the lattice parameter in the b direction shortened dramatically; both are associated with cation ordering. A short-range commensurate superstructure with a ZTTZZTTZTTZZTT (or ZTTZZTTZTTZZTT) stacking sequence was observed in the ordered ZrTiO4 specimens. All the samples showed poor dielectric properties at microwave frequency (4 GHz). The low dielectric Q values (400–1000) were due to the presence of the structural stabilizer, Y2O3, within the grains. The Q value increased slightly with increasing TiO2 content. The air-quenched samples had the highest Q values (850–1000); slower cooling led to the formation of microcracks within the samples and the reduction of Q values. The relative permittivity was controlled by bulk composition, the presence of a grain boundary phase, microcracks, oxygen vacancies and cation ordering. The ordering of cations and the presence of microcracks reduced the relative permittivity; rapidly cooled samples with higher TiO2 content had higher relative permittivities (with a maximum of 44.3 for air-quenched Zr5Ti7O24). This revised version was published online in November 2006 with corrections to the Cover Date.     

Microstructural and dielectric properties of donor doped (La3+) CaCu3Ti4O12 ceramics

The effect of La³⁺ doping on Ca²⁺ sites in CaCu₃Ti₄O₁₂ (CCTO) was examined. Polycrystalline samples in the chemical formula Ca_(1-x)La_(2/3)x Cu₃Ti₄O₁₂ with x = 0, 0.5, 1 were synthesized via the conventional solid state reaction route. X-ray powder diffraction analysis confirmed the formation of the monophasic compounds and indicated the structure to be remaining cubic with a small increase in lattice parameter with increase in La³⁺ doping. The dielectric and impedance characteristics of Ca_(1-x)La_(2/3)x Cu₃Ti₄O₁₂ were studied in the 100 Hz–10 MHz frequency range at various temperatures (100–475 K). A remarkable decrease in grain size from 50 μm to 3–5 μm was observed on La³⁺ substitution. The dielectric constant of CaCu₃Ti₄O₁₂ decreased drastically on La³⁺ doping. The frequency and temperature responses of dielectric constant of La³⁺ doped samples were found to be similar to that of CaCu₃Ti₄O₁₂. The effects of La³⁺ doping on the electrical properties of CaCu₃Ti₄O₁₂ were probed using impedance spectroscopy. The conducting properties of grain decreased while that of the grain boundary increased on La³⁺ doping, resulting in a decrease of the internal barrier layer effect. A decrease in grain boundary capacitance and stable grain response in La³⁺ doped CCTO ceramics were unambiguously established by modulus spectra studies.     

Microstructure and dielectric properties of CaCu3Ti4O12 ceramic

CaCu₃Ti₄O₁₂ (CCTO) was prepared by the solid state technique. The sample was calcined at 900 °C/12 h and sintered at 1050 °C/24 h, then subjected to XRD to ensure CCTO formation. The microstructure was observed by SEM. XRD results identified both samples as single phase CCTO, whereas the microstructure shows abnormal grain growth and large pores. Sintering was studied in the temperature range of 950–1050 °C for 3–12 h. Increasing sintering temperature enhances the density and secondary formation of Cu₂O. A clear grain boundary and dense microstructure were observed. The results show that the sample sintered at 1040 °C/10 h yields a clearly uniform grain size with the highest ε_r (33,210).