Low temperature processing of (Zr0.8Sn0.2)TiO4 ceramics with improved Q factor

Polycrystalline (Zr_0.8Sn_0.2)TiO₄ (ZST) ceramics have been synthesized by solid-sate reaction method. The effect of B₂O₃, ZnO-B₂O₃ or 5ZnO-2B₂O₃ glass addition (0.2-1.0 wt.%) on microwave dielectric properties of ZST ceramics are investigated. The increase in average grain size via growth of large grains and dissolution of small grains is explained by Ostwald ripening phenomena. The highest Q × f_o values are found to be 61,500, 48,500 and 51,900 GHz for the ZST dielectric resonators added with B₂O₃, ZnO-B₂O₃ and 5ZnO-2B₂O₃ respectively. The effect of liquid phase sintering on microstructure and microwave dielectric properties of ZST ceramics is discussed.     

The influence of sintering conditions on the dielectric and piezoelectric properties of PbZrTiO–PbMgNbO ceramic tubes

Piezoelectric tube actuators with a composition of 0.9Pb(Zr_0.52Ti_0.48)O₃–0.1Pb(Mg_1/3Nb_2/3)O₃ (0.9PZT–0.1PMN) have been prepared using electrophoretic deposition (EPD) method. The effect of sintering temperature on the phase formation, densification, microstructure, dielectric and piezoelectric properties of the 0.9PZT–0.1PMN system was investigated. The results show that when the sintering temperature varies from 1150 to 1300 °C, the tubes exhibit single perovskite structure with coexistence of rhombohedral and tetragonal phase. The P–E hysteresis loops reveal the ferroelectric nature of 0.9PZT–0.1PMN system. The tip deflection of the tube upon the applied voltage shows typical butterfly loop, which is a feature of piezoelectric systems. It was found that both dielectric and piezoelectric constants increase with increasing sintering temperature up to 1250 °C. When exceeding 1250 °C, the evaporation of PbO degrades the dielectric and piezoelectric properties of the PZT–PMN. The sample packing technique during sintering is also critically important for obtaining good properties.     

Effects of Kaolinite addition on the densification and dielectric properties of BaTiO3 ceramics

Commercial Kaolinite was employed as sintering aid to reduce the sintering temperature of BaTiO₃ ceramics. The effects of Kaolinite content and sintering temperature on the densification, microstructure and dielectric properties of BaTiO₃ ceramics have been investigated. The density characterization results show that the addition of Kaolinite significantly lowered the sintering temperature of BaTiO₃ ceramics to about 1200 °C. XRD results show BaTiO₃ ceramics with a low amount of Kaolinite exhibited perovskite structure, but 10.0 wt% Kaolinite additions resulted in the formation of a secondary phase, BaAl₂Si₂O₈. BaO-TiO₂-Al₂O₃-SiO₂ glass phase was formed and improved the average breakdown strength of ceramics, which was supported by SEM-EDX results. The Kaolinite content had shown a strong influence on the dielectric constant and the diffuse transition. BaTiO₃ ceramic with 4.0 wt% Kaolinite addition possessed well temperature stability of dielectric constant.     

Low temperature sintering and properties of CaO–B2O3–SiO2 system glass ceramics for LTCC applications

The P₂O₅ + ZnO, ZrO₂ + TiO₂, B₂O₃ and a low-melting-point CaO–B₂O₃–SiO₂ glass (LG) are selected as the sintering additives, and the effect of their additions on the microwave dielectric properties, mechanical properties and microstructures of CaO–B₂O₃–SiO₂ system glass ceramics is investigated. It is found that the sintering temperature of pure CBS glass is higher than 950 °C and the sintering range is about 10 °C. With the above additions, the glass ceramics can be sintered between 820 °C and 900 °C. The dielectric properties of the samples are dependent on the additions, densification and microstructures of sintered bodies. The major phases of this material are CaSiO₃, CaB₂O₄ and SiO₂. With 10 wt% B₂O₃ and LG glass additions, the CBS glass ceramics have better mechanical properties, but worse dielectric properties. The _r values of 6.51 and 7.07, the tan δ values of 0.0029 and 0.0019 at 10 GHz, are obtained for the CBS glass ceramics sintered at 860 °C with 2 wt% P₂O₅ + 2 wt% ZnO and 2 wt% ZrO₂ + 2 wt% TiO₂ additions, respectively. This material is suitable to be used as the LTCC material for the application in wireless communications.     

CaCu3Ti4O12 ceramics from basic co-precipitation (BCP) method: Fabrication and properties

High dielectric CaCu₃Ti₄O₁₂ (CCTO) ceramics have been successfully prepared by a novel basic co-precipitation (BCP) method. Compared with the conventional solid-state and/or soft chemistry methods, the BCP method has many advantages such as relatively lower sintering temperature, shorter sintering time and lower costs. The XRD patterns confirm the formation of CCTO crystal phase in the as-prepared samples. Influences of initial ingredients and sintering condition on phase composition, microstructure and dielectric property have been investigated through series of trials. The correlation between the process of the grain growth and dielectric properties of final products has been explored. The final products exhibit the dielectric constants higher than 10,000 and the dielectric losses lower than 0.15 at 1 KHz.     

New dielectric material system of Nd(Mg1/2Ti1/2)O3–CaTiO3 with V2O5 addition for microwave applications

The effects of sintering aids additives on the microstructures and microwave dielectric properties of (1 ? x)CaTiO₃–xNd(Mg_1/2Ti_1/2)O₃ ceramics were investigated. The effects of V₂O₅ additions on the microwave dielectric properties and the microstructures of (1 ? x)CaTiO₃–xNd(Mg_1/2Ti_1/2)O₃ ceramics have been investigated. Doping with 0.5 wt% V₂O₅ can effectively promote the densification and the microwave dielectric properties of (1 ? x)CaTiO₃–xNd(Mg_1/2Ti_1/2)O₃. It is found that CaTiO₃–Nd(Mg_1/2Ti_1/2)O₃ ceramics can be sintered at 1325 °C due to the liquid phase effect of a V₂O₅ additions. The dielectric constant decreases from 140 to 28 as x varies from 0.1 to 1.0. The microwave dielectric properties indicate the possibility of a phase transformation for x between 0.3 and 0.5. A low-pass filter is designed and simulated using the proposed dielectric to study its performance.     

Microwave dielectric properties and its compatibility with silver electrode of Li2MgTi3O8 ceramics

The effects of BaCu(B₂O₅) (BCB) additions on the sintering temperature and microwave dielectric properties of Li₂MgTi₃O₈ ceramic have been investigated. The pure Li₂MgTi₃O₈ ceramic shows a relative high sintering temperature (∼1000 °C) and good microwave dielectric properties as Q × f of 40,000 GHz, ?_r of 27.2, τ_f of 2.6 ppm/°C. It was found that the addition of a small amount of BCB can effectively lower the sintering temperature of Li₂MgTi₃O₈ ceramics from 1025 to 900 °C and induce no obvious degradation of the microwave dielectric properties. Typically, the 0.5 wt% BCB added Li₂MgTi₃O₈ ceramic sintered at 900 °C for 2 h exhibited good microwave dielectric properties of Q × f = 36,200 GHz (f = 7.31 GHz), ?_r = 26 and τ_f = −2 ppm/°C. Compatibility with Ag electrode indicates this material can be applied to low temperature-cofired ceramics (LTCC) devices.     

Effect of addition of Ba(W0.5Cu0.5)O3 in Pb(Mg1/3Nb2/3)O3-Pb(Zn1/3Nb2/3)O3-Pb(Zr0.52Ti0.48)O3 ceramics on the sintering temperature, electrical properties and phase transition

In this work, we report on the Pb(Mg_1/3Nb_2/3)O₃-Pb(Zn_1/3Nb_2/3)O₃-Pb(Zr_0.52Ti_0.48)O₃ (PMN-PZN-PZT) ceramics with Ba(W_0.5Cu_0.5)O₃ as the sintering aid that was manufactured in order to develop the low-temperature sintering materials for piezoelectric device applications. The phase transition, microstructure, dielectric, piezoelectric properties, and the temperature stability of the ceramics were investigated. The results showed that the addition of Ba(W_0.5Cu_0.5)O₃ significantly improved the sintering temperature of PMN-PZN-PZT ceramics and could lower the sintering temperature from 1005 to 920 °C. Besides, the obtained Ba(W_0.5Cu_0.5)O₃-doped ceramics sintered at 920 °C have optimized electrical properties, which are listed as follows: (K_p = 0.63, Q_m = 1415 and d₃₃ = 351 pC/N), and high depolarization temperature above 320 °C. These results indicated that this material was a promising candidate for high-power multilayer piezoelectric device applications.     

Effect of sintering temperature and composition on microstructure and properties of PMS-PZT ceramics

The piezoelectric ceramics xPb（Mn1/3Sb2/3）O3-（1-x）Pb（Zr1/2Ti1/2）O3 （abbreviated as PMS-PZT） were synthesized by traditional ceramics process. The effect of sintering temperature and the amount of Pb（Mn1/3Sb2/3）O3 （abbreviated as PMS） on phase structure, microstructure, piezoelectric and dielectric properties of PMS-PZT ceramics was investigated. The results show that the pure perovskite phase is in all ceramics specimens, the phase structure of PMS-PZT ceramics changes from tetragonal phase to single rhombohedral phase with the increasing amount of PMS. The dielectric constant εr, Curie temperature Tc, electromechanical coupling factor kp and piezoelectric constant d33 decrease, whereas the mechanical quality factor Qm and dielectric loss tanδ increase with the increasing amount of PMS in system. The optimum sintering temperature is 1 200-1 250 ℃. It is concluded that the PMS-PZT （x=0.07） ceramics sintered at 1 250 ℃ is suitable for high-power piezoelectric transformer. These properties include εr=674.8, tanδ =0.005 25, kp=0.658, Qm= 1 520, d33=230 pC/N, Tc=275 ℃.     

Microwave Dielectric Properties of Nd(Zn1/2Ti1/2)O3 Ceramics with V2O5 Additives

The microwave dielectric properties and the microstructures of V₂O₅-doped Nd(Zn_1/2Ti_1/2)O₃ ceramics prepared by conventional solid-state route have been studied. Doping with V₂O₅ (up to 6 wt.%) can effectively promote the densification of Nd(Zn_1/2Ti_1/2)O₃ ceramics with low sintering temperature. At 1300 °C, Nd(Zn_1/2Ti_1/2)O₃ ceramic when added with 6 wt.% V₂O₅ possesses a dielectric constant of 29.9, a quality factor (Q × f) value of 105000 GHz (at 8 GHz), and a temperature coefficient of resonant frequency of ?45 ppm/°C. These V₂O₅-doped Nd(Zn_1/2Ti_1/2)O₃ ceramics can be used in microwave devices.     

Microstructure, dielectric and ferroelectric properties of 0.94Bi0.5Na0.5TiO3-0.06BaTiO3 (NBTB) and 0.05BiFeO3-0.95NBTB ceramics: Effect of sintering atmosphere

0.94Bi_0.5Na_0.5TiO₃-0.06BaTiO₃ (NBTB) and 0.05BiFeO₃-0.95NBTB (BF-doped NBTB) lead-free ceramics were prepared by solid state reaction method. The ceramics were sintered at 1180 °C for 2 h in O₂ and N₂. All ceramics exhibited a single phase of perovskite structure. Relative amount of tetragonal phase was related to the sintering atmospheres. Both grain size and shape were influenced by the sintering atmospheres. Sintering the ceramics in N₂ weakened their dielectric anomalies corresponding to the transition from ferroelectric phase to the so-called “intermediate phase”. When the NBTB and BF-doped NBTB ceramics were sintered in N₂, their maximum dielectric constant and the degree of diffuseness of the transition from the “intermediate phase” to paraelectric phase increased, but their Curie temperatures decreased. The difference in dielectric properties of the ceramics sintered in different atmospheres was closely related to the difference in oxygen vacancy concentration. The correlation between ferroelectric properties and sintering atmospheres is associated with a competing effect among oxygen vacancy concentration, A-site vacancy concentration and percentage of tetragonal phase.     

Fabrication of dense Al2O3-FeAl composites by using solid-state sintering

Highly densified alumina-iron aluminide (Al₂O₃-FeAl) composites consisting of ubiquitous elements were fabricated by using pulse current sintering technique under a certain uni-axial pressure. The solid-state sintering without melting FeAl was the highlight in this study. The mechanical properties of the Al₂O₃-FeAl composites were much greater than previously reported ones fabricated by reaction sintering technique. The poor wettability of FeAl against Al₂O₃ strongly influenced the mechanical properties and made it difficult to be highly densified Al₂O₃-FeAl composites by liquid phase sintering especially when volume fraction of FeAl to Al₂O₃-FeAl was high (>30.5 vol%). However, highly densified Al₂O₃-FeAl composites were obtained by solid-state sintering with control of Al₂O₃ grain size and sintering temperatures. It was concluded that highly controlled powder metallurgy made it possible to fabricate dense ceramic-metal (intermetallic) composites from the combination of materials having poor wettability.     

Spark Plasma Sintering of α/β Si<Subscript>3</Subscript>N<Subscript>4</Subscript> Ceramics with MgO-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> and MgO-Y<Subscript>2</Subscript>O<Subscript>3</Subscript> as Sintering Additives

In the present work, the α/β Si₃N₄ ceramics were fabricated by spark plasma sintering (SPS) at 1400-1500 °C for 6 min with 3wt.%MgO + 5wt.%Al₂O₃ and 3wt.%MgO + 5wt.%Y₂O₃ as sintering additives. The results showed that the phase composition, microstructure and mechanical properties of α/β Si₃N₄ ceramics were highly dependent on the type of sintering additive. The incomplete phase transformation from α to β occurred in the presence of an oxynitride (Mg-Al(Y)-Si-O-N) liquid phase. Compared with MgO-Al₂O₃, MgO-Y₂O₃ can significantly improve the β conversion rate of as-sintered α/β Si₃N₄ ceramics. And the as-sintered ceramics using MgO + Al₂O₃ as sintering additives had higher mechanical properties.     

Electrical and magnetic properties of magnesium ferrite ceramics doped with Bi2O3

The effects of concentration of Bi₂O₃ and sintering temperature on DC resistivity, complex relative permittivity and permeability of MgFe_1.98O₄ ferrite ceramics were studied. The objective of the study was to develop magneto-dielectric materials, with almost equal values of permeability and permittivity, as well as low magnetic and dielectric loss tangent, for the design of antennas with reduced physical dimensions. It was found that the poor densification and slow grain growth rate of MgFe_1.98O₄ can be greatly improved by the addition of Bi₂O₃, because liquid phase sintering was facilitated by the formation of a liquid phase layer due to the low melting point of Bi₂O₃. It was found that 3% Bi₂O₃ can result in fully sintered MgFe_1.98O₄ ceramics. The DC resistivities of the MgFe_1.98O₄ ceramics were increased as a result of the addition of Bi₂O₃, except for 0.5%. The exceptionally low resistivities of the 0.5% samples were explained by a ‘cleaning’ effect of the small amount of liquid phase at the samples’ grain boundaries. The electrical and magnetic properties of the MgFe_1.98O₄ ceramics exhibited a strong dependence on the concentration of Bi₂O₃. The 0.5% samples were found to have the highest dielectric loss tangents, which can be understood similarly to the DC resistivity results. The 2–3% Bi₂O₃ is required to attain low dielectric loss MgFe_1.98O₄ ceramics for antenna application. Low concentration of Bi₂O₃ increased the static permeability of the MgFe_1.98O₄ ceramics owing to the improved densification and grain growth, while too high a concentration led to decreased permeability owing to the incorporation of the non-magnetic component (Bi₂O₃) and retarded grain growth. However, the addition of Bi₂O₃ alone is not able to produce magneto-dielectric materials based on MgFe_1.98O₄ ceramics, and further work is necessary to modify the permeability using cobalt (Co).     

Control of microwave dielectric properties in 0.42ZnNb<Subscript>2</Subscript>O<Subscript>6</Subscript>−0.58TiO<Subscript>2</Subscript> ceramics by the quantitative analysis of phase transition

Phase constitutions of ZnNb₂O₆−TiO₂ mixture ceramics were significantly changed according to the sintering temperature. Phase transition procedures and their effect on the microwave dielectric properties of 0.42ZnNb₂O₆−0.58TiO₂ were investigated using X-ray powder diffraction and a network analyzer. The fractions of the phases composing the mixture were calculated by measuring integral intensities of each reflection. The structural transitions in 0.42ZnNb₂O₆−0.58TiO₂ were interpreted as the association of two distinct steps: the columbite and rutile to ixiolite transition present at lower temperatures (900–950°C) and the ixiolite to rutile transition at higher temperatures (1150–1300°C). These transitions caused considerable variation of microwave dielectric properties. Importantly, τ_f was modified to around 0 ppm/°C in two sintering conditions (at 925°C for 2 hr and at 1300°C for 2 hr), by the control of phase constitution.     

New dielectric material system of La(Mg1/2Ti1/2)O3–Ca0.6La0.8/3TiO3 for microwave applications

The microstructure and microwave dielectric properties of xLa(Mg_1/2Ti_1/2)O₃–(1 − x)Ca_0.6La_0.8/3TiO₃ ceramics system with ZnO additions (0.5 wt.%) investigated by the conventional solid-state route have been studied. Doping with ZnO (0.5 wt.%) can effectively promote the densification and the dielectric properties of xLa(Mg_1/2Ti_1/2)O₃–(1 − x)Ca_0.6La_0.8/3TiO₃ ceramics. 0.6La(Mg_1/2Ti_1/2)O₃–0.4Ca_0.6La_0.8/3TiO₃ ceramics with 0.5 wt.% ZnO addition possess a dielectric constant (_r) of 43.6, a Q × f value of 48,000 (at 8 GHz) and a temperature coefficient of resonant frequency (τ_f) of −1 ppm/°C sintering at 1475 °C. As the content of La(Mg_1/2Ti_1/2)O₃ increases, the highest Q × f value of 62,900 (GHz) for x = 0.8 is achieved at the sintering temperature 1475 °C. A parallel-coupled line band-pass filter is designed and simulated using the proposed dielectric to study its performance.     

Low temperature sintering and microwave dielectric properties of (Mg0.7Zn0.3)0.95Co0.05TiO3 ceramics with BaCu(B2O5) additions

The effects of BaCu(B₂O₅) additives on the sintering temperature and microwave dielectric properties of (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics were investigated. The (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics were not able to be sintered below 1000 °C. However, when BaCu(B₂O₅) were added, they were sintered below 1000 °C and had the good microwave dielectric properties. It was suggested that a liquid phase with the composition of BaCu(B₂O₅) was formed during the sintering and assisted the densification of the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics at low temperature. BaCu(B₂O₅) powders were produced and used to reduce the sintering temperature of the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics. Good microwave dielectric properties of Q × f = 35,000 GHz, ?_r = 18.5.0 and τ_f = −51 ppm/°C were obtained for the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics containing 7 wt.% mol% BaCu(B₂O₅) sintered at 950 °C for 4 h.     

Improved high-Q microwave dielectric resonator using ZnO-doped La(Co1/2Ti1/2)O3 ceramics

The microwave dielectric properties and the microstructures of ZnO-doped La(Co_1/2Ti_1/2)O₃ ceramics prepared by conventional solid-state route have been studied. Doped with ZnO (up to 0.75 wt%) can effectively promote the densification of La(Co_1/2Ti_1/2)O₃ ceramics with low sintering temperature. At 1320 °C, La(Co_1/2Ti_1/2)O₃ ceramics with 0.75 wt% ZnO addition possesses a dielectric constant (_r) of 30.2, a Q × f value of 73,000 GHz (at 8 GHz) and a temperature coefficient of resonant frequency (τ_f) of −35 ppm/°C.     

Effect of Sm2O3 content on microstructure and thermal conductivity of Spark Plasma Sintered AlN ceramics

Dense aluminum nitride ceramics were prepared by Spark Plasma Sintering at a lower sintering temperature of 1700 °C with Sm₂O₃ as sintering additives. The effect of Sm₂O₃ content on the density, phase composition, microstructure and thermal conductivity of AlN ceramics was investigated. The results showed that Spark Plasma Sintering could fabricate dense AlN ceramics with superior thermal properties in a very short time. Sm₂O₃ not only facilitated the densification via the liquid-phase sintering mechanism but also improved thermal conductivity by decreasing oxygen impurity. Thermal conductivity decreased with increasing amount of Sm₂O₃ and the highest thermal conductivity was obtained for the AlN ceramics with 2 wt.% Sm₂O₃ content. During Spark Plasma Sintering process, only 2–3 wt.% sintering additives was enough to fabricate dense AlN ceramics, and the microstructures played a key role in controlling the thermal conductivity of AlN ceramics.     

Reaction-sintering method for ultra-low loss (Mg0.95Co0.05)TiO3 ceramics

Microwave dielectric properties and microstructures of (Mg_0.95Co_0.05)TiO₃ ceramics prepared by a new sintering method (reaction-sintering method) were investigated. A pure phase of (Mg_0.95Co_0.05)TiO₃ was obtained by the new method and excellent dielectric properties were observed due to uniformities of the microstructure and the phase. In contrast, the secondary phase (Mg_0.95Co_0.05)Ti₂O₅ was observed in samples prepared by conventional sintering method. In order to study the influence of secondary phase on the microwave dielectric properties quantitatively, the weight fraction of (Mg_0.95Co_0.05)Ti₂O₅ was calculated on the basis of Rietveld refinement. The pore-free?_r values of specimens prepared by two different methods indicated that porosity plays an important role in the ?_r values of (Mg_0.95Co_0.05)TiO₃ ceramics. Specimens sintered by reaction-sintering method at 1350 °C for 4 h possess excellent dielectric properties with an ?_r of 16.3, a Q × f value of 244,500 GHz, and a τ_f value of −53.5 ppm/°C.