Homogeneity Region of Strontium- and Magnesium-Containing LaGaO3 at Temperatures between 1100° and 1500°C in Air

Phase stability studies were performed within the quasi-ternary system LaGaO₃-SrGaO_2.5-"LaMgO_2.5". Emphasis was cast on the temperature dependence of the homogeneity region of La_{1− x} Sr _x Ga_{1− y} Mg _y O_3−δ perovskite solid solutions. Isothermal sections were determined at 1100°, 1250°, 1400°, and 1500°C in a static air atmosphere. The single-phase homogeneity region was found to considerably diminish with decreasing temperature, indicating a reduction of the solid solubility of Sr and Mg, and below 1100°C the doped perovskite becomes unstable. Consequently, the cubic perovskite phase was found to exist only at elevated temperatures and for high Sr and Mg amounts. Sample preparation was performed by the mixed-oxide process as well as by a modified combustion synthesis.     

Effect of V2O5 Doping on the Sintering and Dielectric Properties of M-Phase Li1+x−yNb1−x−3yTix+4yO3 Ceramics

The effect of the addition of V₂O₅ on the structure, sintering and dielectric properties of M -phase (Li_{1+ x − y} Nb_{1− x −3 y} Ti _x +4 _y )O₃ ceramics has been investigated. Homogeneous substitution of V⁵⁺ for Nb⁵⁺ was obtained in LiNb_{0.6(1− x )}V_{0.6 x} Ti_0.5O₃ for x ≤ 0.02. The addition of V₂O₅ led to a large reduction in the sintering temperature and samples with x = 0.02 could be fully densified at 900°C. The substitution of vanadia had a relatively minor adverse effect on the microwave dielectric properties of the M -phase system and the x = 0.02 ceramics had [alt epsilon]_r= 66, Q × f = 3800 at 5.6 GHz, and τ_f= 11 ppm/°C. Preliminary investigations suggest that silver metallization does not diffuse into the V₂O₅-doped M -phase ceramics at 900°C, making these materials potential candidates for low-temperature cofired ceramic (LTCC) applications.     

Microwave Dielectric Properties of CaTiO3-CaAl1/2Nb1/2O3 Ceramics Doped with Li3NbO4

The microwave dielectric properties of CaTi_{1− x} (Al_1/2Nb_1/2) _x O₃ solid solutions (0.3 ≤ x ≤ 0.7) have been investigated. The sintered samples had perovskite structures similar to CaTiO₃. The substitution of Ti⁴⁺ by Al³⁺/Nb⁵⁺ improved the quality factor Q of the sintered specimens. A small addition of Li₃NbO₄ (about 1 wt%) was found to be very effective for lowering sintering temperature of ceramics from 1450–1500° to 1300°C. The composition with x = 0.5 sintered at 1300°C for 5 h revealed excellent dielectric properties, namely, a dielectric constant (ɛ_r) of 48, a Q × f value of 32 100 GHz, and a temperature coefficient of the resonant frequency (τ_f) of −2 ppm/K. Li₃NbO₄ as a sintering additive had no harmful influence on τ_f of ceramics.     

Doped Lanthanum Gallate Film Solid Oxide Fuel Cells Fabricated On a Ni/YSZ Anode Support

A colloidal deposition without any binder was developed to prepare a dense La_0.8Sr_0.2Ga_0.85Mg_0.15O_3−δ (LSGM) film on porous NiO/YSZ substrates, using an incompletely crystallized LSGM powder as starting material. Both the dense LSGM film with a thickness of 15 μm and the required phase composition of the LSGM were achieved simultaneously by sintering at 1400°C for 6 h. The conductivity of the supported LSGM film attained 0.102 S/cm at 800°C, which was comparable with those of the self-supported LSGM films. The maximum power density of the LSGM film cell was 480 at 800°C and 614 mW/cm² at 850°C, respectively.     

Low-Temperature Sintering and Dielectric Properties of Ag(Nb,Ta)O3 Composite Ceramics

The sintering behavior and dielectric properties of perovskite Ag(Nb_{1− x} Ta _x )O₃ (0 < x < 1) solid solutions and two-phase composite assemblages were explored. A small amount of CuO (1 wt%) was used for liquid-phase sintering and led to high densification at temperatures <950°C. The temperature coefficient of capacitance, TCC, was adjusted by varying the Nb:Ta ratio within the solid-solution series and by creating composite microstructures. Two-phase assemblages consisting of Ag(Nb_3/4Ta_1/4)O₃ and Ag(Nb_1/4Ta_3/4)O₃ were synthesized to achieve a temperature-stable dielectric material for high-frequency applications. The composite dielectric with CuO addition had an average dielectric constant of 390 and a Q × f factor of 410 GHz at 2 GHz, with a stable TCC (0 to −180 ppm/°C) in the temperature range from −20° to +60°C. In addition, process compatibility with a silver conductor was confirmed by high-frequency ring-resonator measurements and microstructural characterization. The Ag(Nb_{1− x} Ta _x )O₃ solid solutions and composites are promising candidates as embedded capacitors for radio-frequency/microwave applications.     

Microstructure and Piezoelectric Properties of (1−x)(Na0.5K0.5)NbO3–xLiNbO3 Ceramics

(1− x )(Na_0.5K_0.5)NbO₃– x LiNbO₃ [(1− x )NKN– x LN] ceramics were produced by the conventional solid-state sintering method, and their microstructure and piezoelectric properties were investigated. The formation of the liquid phase and K₆Li₄Nb₁₀O₃₀ second phase that were observed in the (1− x )NKN– x LN ceramics was explained by the evaporation of Na₂O during the sintering. A morphotropic phase boundary (MPB) was observed in the specimens with 0.05< x <0.08. Promising piezoelectric properties were obtained for the specimens with x =0.07. Therefore, the piezoelectric properties of this 0.93NKN–0.07LN ceramic were further investigated and were found to be influenced by their relative density and grain size. In particular, grain size considerably affected the d ₃₃ value. Two-step sintering was conducted at different temperatures to increase the grain size. Piezoelectric properties of d ₃₃=240 (pC/N) and k _p=0.35 were obtained for the 0.93NKN–0.07LN ceramics sintered at 1030°C and subsequently annealed at 1050°C.     

Low-Dielectric Loss Characteristics of Nd(Co1/2Ti1/2)O3 Ceramics at Microwave Frequencies

The microwave dielectric properties and the microstructures of Nd(Co_1/2Ti_1/2)O₃ (NCT) ceramics using starting powders of Nd₂O₃, CoO, and TiO₂ prepared by the conventional solid-state route have been researched. The dielectric constant values (ɛ_r) saturated at 24.8–27. Quality factor ( Q × f ) values of 37 900–140 000 (at 9 GHz) and the measured τ_f values ranging from −45 to −48 ppm/°C can be obtained when the sintering temperatures are in the range of 1410°–1500°C. The ɛ_r value of 27, the Q × f value of 140 000 (at 9 GHz) and the τ_f value of −46 ppm/°C were obtained for NCT ceramics sintered at 1440°C for 4 h. For applications of high selective microwave ceramic resonator, filter, and antenna, NCT is proposed as a suitable material candidate.     

Fabrication of Low-Porosity Indium Tin Oxide Ceramics in Air from Hydrothermally Prepared Powder

Compositionally homogeneous indium tin oxide (ITO) ceramics with low porosity were obtained successfully by sintering hydrothermally prepared powders. The fabrication technique began with the preparation of microcrystalline, homogeneously tin-doped (5 wt%) indium oxyhydroxide powder, under hydrothermal conditions. Low-temperature (∼500°C) calcination of the hydrothermally derived powder led to the formation of a substitutional-vacancy-type solid solution of In₂Sn_{1− x} O_{5− y} , and further heating of this phase at temperatures of >1000°C resulted in the formation of the tin-doped indium oxide phase, which had the C -type rare-earth-oxide structure. The sintering of uniformly packed, calcined powder compacts at 1450°C for 3 h in air resulted in low-porosity (∼0.7%) ITO ceramics.     

1000°C Phase Relations and Superconductivity in the (Nd-Ce-Cu)-O Ternary System

The phase relations involving the 24 K n -type Nd_{2- x} Ce _x CuO₄ superconductor were investigated at 1000°C in air. The terminal solid solubility was confirmed to be x = 0.2. This solid solution is the only ternary phase in the Nd₂O₃–CeO₂–CuO diagram. A binary (1 − y )CeO₂– y NdO_1.5 solid solution exists out to y = 0.4. Phase diagrams for NdO_1.5–CeO₂–CuO (1000°C) and NdO_1.5–CeO₂ (900° to 1500°C) are presented.     

Microwave Characteristics of (Pb,Ca)(Fe,Nb,Sn)O3 Dielectric Materials

The dielectric properties of (Pb_{1− x} Ca _x ){(Fe_1/2Nb_1/2)_{1– y} Sn _y }O₃ solid solutions, where 0.4 lessthan equal tox ≤ 0.6, y = 0.05, 0.1, have been investigated at microwave frequencies. The replacement of Fe³⁺/Nb⁵⁺ by Sn⁴⁺ at the B–site of the perov-skite structure considerably improves the loss quality factor Q and does not remarkably affect the dielectric constant epsilon_r and the temperature coefficient of resonant frequency tau_f. The tau_f value of nearly 0 ppm/°C can be realized for x= 0.55. New high-quality dielectric ceramics having epsilon_r of 85.3-89.9,Qf values of 7510-8600 GHz, and τ_f of 0-9 ppm/°C were obtained at 1150°C for 3 h sintering in air. The influence of the sintering atmosphere on dielectric properties was also investigated.     

Improvement of Mechanical Properties and Corrosion Resistance of Porous β-SiAlON Ceramics by Low Y2O3 Additions

Addition of Y₂O₃ as a sintering additive to porous β-SiAlON (Si_{6− z} Al _z O _z N_{8− z} , z = 0.5) ceramics has been investigated for improved mechanical properties. Porous SiAlON ceramics with 0.05–0.15 wt% (500–1500 wppm) Y₂O₃ were fabricated by pressureless sintering at temperatures of 1700°, 1800°, and 1850°C. The densification, microstructure, and mechanical properties were compared with those of Y₂O₃-free ceramics of the same chemical composition. Although this level of Y₂O₃ addition did not change the phase formation and grain size, the grain bonding appeared to be promoted, and the densification to be enhanced. There was a significant increase in the flexural strength of the SiAlON ceramics relative to the Y₂O₃-free counterpart. After exposure in 1 M hydrochloric acid solution at 70°C for 120 h, no remarkable weight loss and degradation of the mechanical properties (flexural and compression strength) was observed, which was attributed to the limited grain boundary phase, and with the minor Y₂O₃ addition the supposed formation of Y-α-SiAlON.     

Phase Transformation and Tunable Piezoelectric Properties of Lead-Free (Na0.52K0.48−xLix)(Nb1−x−ySbyTax)O3 System

Lead-free (Na_0.52K_{0.48− x} )(Nb_{1− x − y} Sb _y )O₃- x LiTaO₃ (NKNS–LT) piezoelectric ceramics have been fabricated by ordinary sintering. A special attention was paid to the composition design through which the dielectric and piezoelectric properties of the (Li, Ta, Sb) modified NKN systems were significantly promoted. A property spectrum was generated with a particular discussion on the relationship between the Sb content, the LT content, the polymorphic phase transition, and the electrical properties and their temperature stability. Excellent and tunable electrical properties of d ₃₃=242–400 pC/N, k _p=36%–54%,     , and T _c=230°–430°C demonstrate a tremendous potential of the compositions studied for device applications.     

Preparation of PbZrO3–PbTiO3 Ferroelectric Thin Films by the Sol–Gel Process

Ferroelectric films, PbZr _x Ti_{1− x} O₃ ( x = 0 to 0.6), have been prepared from corresponding metal alkoxides partially stabilized with acetylacetone through the sol-gel process. The films dip-coated in an ambient atmosphere were heat-treated at 400°C for decomposition of residual organics and then at temperatures between 500° and 700°C for crystallization of the films. The perovskite phase precipitated at temperatures above 560°C, accompanied by an increase in dielectric constant. The dielectric constant of the films, which was comparable with that of sintered bodies, showed a maximum (∼620) at around x = 0.52 in PbZr _x Ti_{1− x} O₃. These films showed D – E hysteresis, with slightly higher values of coercive field, compared with those of sintered bodies.     

Sintering Behavior, Phase Evolution, and Microwave Dielectric Properties of Bi(Sb1−xTax)O4 Ceramics

Sintering behavior, phase evolution, and microwave dielectric properties of Bi(Sb_{1− x} Ta _x )O₄ ceramics (0.05≤ x ≤0.60) were studied and their relationships were discussed in detail. Phase studies revealed that a pure monoclinic phase could be formed when x ≤0.20 and a pure orthorhombic phase could be obtained when x ≥0.50. As the x value increased from 0.05 to 0.60, the densified temperature of Bi(Sb_{1− x} Ta _x )O₄ ceramics decreased from 1050° to about 960°C whereas the density increased from 8.07 to 8.41 g/cm³. The microwave dielectric constant increased from 20.5 to 34 whereas the Q × f value decreased from 60 000 to 29 000 GHz. In the monoclinic phase region, the temperature coefficients of resonant frequency shifted linearly from −58 to −45 ppm/°C as the x value increased from 0.05 to 0.2 and then remained constant at about −12 ppm/°C when x ≥0.40. The Bi(Sb_{1− x} Ta _x )O₄ ceramics are promising for application of low-temperature cofired ceramics technology.     

Modification of MgAl2O4 Microwave Dielectric Ceramics by Zn Substitution

MgAl₂O₄ microwave dielectric ceramics were modified by Zn substitution for Mg, and their dielectric characteristics were evaluated, along with their structures. Dense (Mg_{1− x} Zn _x )Al₂O₄ ceramics were obtained by sintering at 1550°–1650°C in air for 3 h, and the (Mg_{1− x} Zn _x )Al₂O₄ solid solution was determined in the entire composition range. With Zn substitution for Mg, the dielectric constant ɛ of MgAl₂O₄ just varied from 7.90 to 8.56, while the Q × f value had significantly improved up to a maximal value of 106 000 GHz at x =1.0. Moreover, the τ_f of MgAl₂O₄ ceramics had declined from −73 to −63 ppm/°C.     

Glass-Free KxBa1−xGa2−xGe2+xO8 Ceramics for Low-Temperature Cofired Ceramics Technology: Synthesis, Phase Transitions, Sintering, and Microwave Dielectric Properties

K _x Ba_{1− x} Ga_{2− x} Ge_{2+ x} O₈ (0.6≤ x ≤1) polycrystalline ceramics are potential materials for glass-free low-temperature cofired ceramics (LTCC) substrates. We have made a comprehensive study of the kinetics of the monoclinic-to-monoclinic P 2₁/ a ⇔ C 2/ m phase transition. The low-temperature-stable P 2₁/ a phase with a high Q × f value was synthesized using a subsolidus method and was well sintered at the LTCC temperature with a H₃BO₃ additive. A good combination of low sintering temperature (910°–920°C), high Q × f values (96 700–104 500 GHz), low permittivities (5.6–6.0), and a small temperature coefficient of resonant frequency (∼−20 ppm/°C) was obtained for ceramics with x =0.67 and 0.9 and with 0.1 wt% of H₃BO₃.     

Optimization of Praseodymium-Doped Cerium Pigment Synthesis Temperature

The development of red pigments is of great interest to the ceramic industry. Pr(IV) stabilization in a CeO₂ matrix yields materials with a red color. In this study, the traditional ceramic method involving solid-state reaction was used to prepare pigments in the system Ce_{1− x} Pr _x O_2−δ (0.005 ≤ x ≤ 0.1) from mixtures of rare-earth oxides. The chemical stability of these pigments was then determined in some industrial glazes. The glazing tests indicate that the powder samples calcined at 1200° and1300°C are unstable, whereas those calcined at 1400° and 1500°C are stable. These findings are related to the nonformation of a solid solution, to which the pigmenting power is attributed, in calcinations at temperatures below 1400°C.     

The Li2O–Nb2O5–TiO2 Composite Microwave Dielectric Ceramics with Adjustable Permittivities

A group of new y M-phase/(1− y ) Li_{2+ x} Ti_{1−4 x} Nb_{3 x} O₃ composite ceramics with adjustable permittivities for low-temperature co-fired ceramic applications was initially investigated in the study. The 0.5 M-phase/0.5 Li_{2+ x} Ti_{1−4 x} Nb_{3 x} O₃ ( x =0.01, 0.02, 0.04, 0.06, 0.081) composite ceramics were first investigated to find the appropriate "Li₂TiO₃ss" composition ( x value). The best dielectric properties of ɛ_r=40.1, Q × f values up to 9318 GHz, τ_f=25 ppm/°C, were obtained for the ceramics composites at x =0.02. Based on the good dielectric properties, the suitable "Li₂TiO₃ss" composition with x =0.02 was mixed with the Li_1.0Nb_0.6Ti_0.5O₃ powder as the ratio of y "M-phase"/(1− y ) "Li₂TiO₃ss" ( y =0.2, 0.4, 0.5, 0.6, 0.8). By adjusting the y values, the group of composite ceramics could exhibit largely are adjustable permittivities varying from ∼20 to ∼60, while Q × f and τ_f values relatively good. Nevertheless, in this study, because there are interactions between the M-phase and Li₂TiO₃ss during sintering process, their microwave dielectric properties could not be predicted precisely by the empirical model.     

Spark Plasma Sintered Silicon Nitride Ceramics with High Thermal Conductivity Using MgSiN2 as Additives

Silicon nitride ceramics were prepared by spark plasma sintering (SPS) at temperatures of 1450°–1600°C for 3–12 min, using α-Si₃N₄ powders as raw materials and MgSiN₂ as sintering additives. Almost full density of the sample was achieved after sintering at 1450°C for 6 min, while there was about 80 wt%α-Si₃N₄ phase left in the sintered material. α-Si₃N₄ was completely transformed to β-Si₃N₄ after sintering at 1500°C for 12 min. The thermal conductivity of sintered materials increased with increasing sintering temperature or holding time. Thermal conductivity of 100 W·(m·K)⁻¹ was achieved after sintering at 1600°C for 12 min. The results imply that SPS is an effective and fast method to fabricate β-Si₃N₄ ceramics with high thermal conductivity when appropriate additives are used.     

Phase Structure and Electrical Properties of (K0.48Na0.52)(Nb0.95Ta0.05)O3-LiSbO3 Lead-Free Piezoelectric Ceramics

(1− x )(K_0.48Na_0.52)(Nb_0.95Ta_0.05)O₃– x LiSbO₃ [(1− x )KNNT− x LS] lead-free piezoelectric ceramics were prepared by the conventional solid-state sintering method. A morphotropic phase boundary (MPB) between orthorhombic and tetragonal phases was identified in the composition range of 0.03< x <0.05. The ceramics near the MPB exhibit a strong compositional dependence and enhanced electrical properties. The (1− x )KNNT– x LS ( x =0.04) ceramics exhibit good electrical properties ( d ₃₃=250 pC/N, k _p=45.1%, k _t =46.3%, T _c=348°C, T _{o − t} =74°C, P _r=25.9 μC/cm², E _c=10.7 kV/cm, ɛ_r∼1352, tan δ∼3%). These results show that (1− x )KNNT– x LS ceramic is a promising lead-free piezoelectric material.