Y<Subscript>2</Subscript>O<Subscript>3</Subscript> and Nd<Subscript>2</Subscript>O<Subscript>3</Subscript> co-stabilized ZrO<Subscript>2</Subscript>-WC composites

Y₂O₃ + Nd₂O₃ co-stabilized ZrO₂-based composites with 40 vol% WC were fully densified by pulsed electric current sintering (PECS) at 1350 °C and 1450 °C. The influence of the PECS temperature and Nd₂O₃ co-stabilizer content on the densification, hardness, fracture toughness and bending strength of the composites was investigated. The best combination of properties was obtained for a 1 mol% Y₂O₃ and 0.75 mol% Nd₂O₃ co-stabilized composite densified for 2 min at 1450 °C under a pressure of 62 MPa, resulting in a hardness of 15.5 ± 0.2 GPa, an excellent toughness of 9.6 ± 0.4 MPa.m^0.5 and an impressive 3-point bending strength of 2.04 ± 0.08 GPa. The hydrothermal stability of the 1 mol% Y₂O₃ + 1 mol% Nd₂O₃ co-stabilized ZrO₂-WC (60/40) composites was compared with that of the equivalent 2 mol% Y₂O₃ stabilized ceramic. The double stabilized composite did not degrade in 1.5 MPa steam at 200 °C after 4000 min, whereas the yttria stabilized composite degraded after less than 2000 min. Moreover, the (1Y,1Nd) ZrO₂-WC composites have a substantially higher toughness (~9 MPa.m^0.5) than their 2Y stabilized equivalents (~7 MPa.m^0.5).     

Diffusion bonding of Ti<Subscript>3</Subscript>AlC<Subscript>2</Subscript> ceramic via a Si interlayer

Based on the structure characteristic of Ti₃AlC₂ and the easy formation of Ti₃Al_{1 − x} Si _x C₂ solid solution, a Si interlayer was selected to join Ti₃AlC₂ layered ceramic by diffusion bonding method. Joining was performed at 1,300–1,400 °C for 120 min under 5 MPa load in an Ar atmosphere. The phase composition and interface microstructure of the joints were investigated by XRD, SEM and EPMA. The results revealed that Ti₃Al(Si)C₂ solid solution formed at the interface. The mechanism of bonding is attributed to silicon diffusing inward the Ti₃AlC₂. The strength of joints was evaluated by a 3-point bending test. The jointed specimens exhibit a high flexural strength of 285 ± 11 MPa, which is about 80% of that of the Ti₃AlC₂; and retain this strength up to 1,000 °C. The high mechanical performance of the joints indicates that diffusion bonding via a Si interlayer is effective to bond Ti₃AlC₂ ceramic.     

Formation behavior of CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> from CaTiO<Subscript>3</Subscript>, CuO and TiO<Subscript>2</Subscript>

The formation behavior of CaCu₃Ti₄O₁₂ (CCTO) had been investigated via solid state reaction from CaTiO₃, CuO and TiO₂ powders. In the temperature range from 750 to 1,200 °C, the reaction sequence was traced by XRD, and the microstructure evolution of calcined powders was also investigated by SEM. CCTO began to form owing to the reaction between CaTiO₃, CuO and TiO₂ at around 850 °C, and became the major phase at 1,000 °C. Finally, the single phase CCTO was obtained at 1,150 °C. However, CCTO was decomposed at CaTiO₃, CuO and TiO₂ when the temperature increased to 1,200 °C. In addition, no other intermediate phases occurred in the synthesized process. The formation behaviors indicated that CaTiO₃ prevented the formation and growth of CCTO.     

Sintering and electrical properties of Ce<Subscript>0.8</Subscript>Sm<Subscript>0.2</Subscript>O<Subscript>1.9</Subscript> film prepared by spray pyrolysis and tape casting

Ce_0.8Sm_0.2O_1.9 (SDC) powder was synthesized by spray pyrolysis at 650 °C. XRD results showed that phase-pure SDC powder with an average crystallite size of 11 nm was synthesized. SDC electrolyte film was prepared by tape casting and sintered at different temperatures of 1,300, 1,400 and 1,500 °C for 2 h, respectively. The SDC electrolyte film was relatively denser and showed finer microstructure at relatively lower temperature of 1,400 °C, which might be due to the high sintering activity of the spray pyrolysis SDC powder. The ionic conductivity of the SDC electrolyte film sintered at 1,400 °C reached a maximum value of 9.5 × 10⁻³ S cm⁻¹ (tested at 600 °C) with an activation energy for conduction of 0.90 eV.     

Preparation and mechanical properties of ZrB<Subscript>2</Subscript>-based ceramics using MoSi<Subscript>2</Subscript> as sintering aids

ZrB₂ (zirconium diboride)-based ceramics reinforced by 15vol.% SiC whiskers with high density were successfully prepared using MoSi₂ as sintering aids. The effects of sintering condition and MoSi₂ content on densification behavior, phase composition, and mechanical properties of SiC_w/ZrB₂ composites were studied. Nearly, fully dense materials (relative density >99%) were obtained by hot-pressing (HP) at 1700°C–1800°C in flow argon atmosphere. The grain size of ZrB₂ phase in the samples sintered by HP at 1700°C–1800°C were very fine, with mean size below 5 μm. Mechanical properties (such as flexural strength, fracture toughness, and Vickers hardness) of the sintered samples were measured. The sample with 15vol.% MoSi₂ addition sintered by HP at 1750°C displayed the best mechanical properties.     

Mechanical properties of bovine hydroxyapatite (BHA) composites doped with SiO<Subscript>2</Subscript>, MgO,Al<Subscript>2</Subscript>O<Subscript>3</Subscript>, and ZrO<Subscript>2</Subscript>

Biologically derived hydroxyapatite from calcinated (at 850 °C) bovine bones (BHA) was doped with 5 wt% and 10 wt% of SiO₂, MgO, Al₂O₃ and ZrO₂ (stabilized with 8% Y₂O₃). The aim was to improve the sintering ability and the mechanical properties (compression strength and hardness) of the resultant BHA-composites. Cylindrical samples were sintered at several temperatures between 1,000 and 1,300 °C for 4 h in air. The experimental results showed that sintering generally occurs at 1,200 °C. The BHA–MgO composites showed the best sintering performance. In the BHA–SiO₂ composites, extended formation of glassy phase occurred at 1,300 °C, resulting in structural degradation of the resultant samples. No sound reinforcement was achieved in the case of doping with Al₂O₃ and zirconia probably due to the big gap between the optimum sintering temperatures of BHA and these two oxides.     

Microwave dielectric properties of Ba<Subscript>5</Subscript>Nb<Subscript>4</Subscript>O<Subscript>15</Subscript> ceramic by molten salt method

Ba₅Nb₄O₁₅ powders were synthesized by molten-salt method in NaCl–KCl flux at a low temperature of 650–900 °C for 2 h, which is lower than that of the conventional solid-state reaction. This simple process involved mixing of the raw materials and salts in a certain proportion. Subsequent calcination of the mixtures led to Ba₅Nb₄O₁₅ powders at 650–900 °C. XRD and SEM techniques were used to characterize the phase and morphology of the fabricated Ba₅Nb₄O₁₅ powders, respectively. After sintering at 1,300 °C for 2 h, the densified Ba₅Nb₄O₁₅ ceramics with good microwave dielectric properties of ε_r = 39.2, Q × f approximated as 27,200 GHz and τ _f  = 72 ppm/°C have been obtained.     

Structure and properties of Ba(Zr<Subscript>0.2</Subscript>Ti<Subscript>0.8</Subscript>)O<Subscript>3</Subscript> ceramics prepared by spark plasma sintering

Ba(Zr_0.2Ti_0.8)O₃ (BZT) ceramics are prepared from spray-dried powder by spark plasma sintering (SPS) and by normal sintering. By the application of SPS, ceramics with >96% relative densities could be obtained by sintering at 1,100 °C for 5 min in air atmosphere. The pellet as sintered by SPS at 1,100 °C was black and conductive. Although SPS was carried out in air atmosphere, the samples were deoxidized by heating the carbon die. By post-annealing at 1,000 °C for 12 h in air, the pellet was oxidized and became white and insulating. Grain growth was suppressed in the ceramics prepared by SPS, and the average grain size was 0.52 μm. The starting powder contained 1.90% carbon, mainly as binder, and the SPS-prepared ceramics and ordinary prepared ceramics contained 0.15 and 0.024% carbon, respectively. The BZT ceramics obtained by SPS and the subsequent annealing at 1,000 °C for 12 h exhibited a mild temperature dependence of their dielectric constant. The field-induced displacement of the BZT ceramics was less hysteretic and smaller than that of the ceramics sintered by the conventional method.     

Effect of replacement of MgO by CaO on sintering,crystallization and properties of MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript> system glass-ceramics

The effects of replacement of MgO by CaO on the sintering and crystallization behavior of MgO–Al₂O₃–SiO₂ system glass-ceramics were investigated. The results show that with increasing CaO content, the glass transition temperature firstly increased and then decreased, the melting temperature was lowered and the crystallization temperature of the glass-ceramics shifted clearly towards higher temperatures. With the replacement of MgO by less than 3 wt.% CaO, the predominant crystalline phase in the glass-ceramics fired at 900 °C was found to be α-cordierite and the secondary crystalline phase to be μ-cordierite. When the replacement was increased to 10 wt.%, the predominant crystalline phase was found to be anorthite and the secondary phase to be α-cordierite. Both thermal expansion coefficient (TCE) and dielectric constant of samples increases with the replacement of MgO by CaO. The dielectric loss of sample with 5 wt.% CaO fired at 900 °C has the lowest value of 0.08%. Only the sample containing 5 wt.% and10 wt.% CaO (abbreviated as sample C5 and C10) can be fully sintered before 900 °C. Therefore, a dense and low dielectric loss glass-ceramic with predominant crystal phase of α-cordierite and some amount of anorthite was achieved by using fine glass powders (D₅₀ = 3 μm) fired at 875–900 °C. The as-sintered density approaches 98% theoretical density. The flexural strength of sample C5 firstly increases and then decreases with sintering temperature, which closely corresponds to its relative density. The TCE of sample C5 increases with increasing temperature. The dielectric property of sample C5 sintered at different temperatures depends on not only its relative density but also its crystalline phases. The dense and crystallized glass-ceramic C5 exhibits a low sintering temperature (≤900 °C), a fairly low dielectric constant (5.2–5.3), a low dielectric loss (≤10⁻³) at 1 MHz, a low TCE (4.0–4.25 × 10⁻⁶ K⁻¹), very close to that of Si (∼3.5 × 10⁻⁶ K⁻¹), and a higher flexural strength (≥134 MPa), suggesting that it would be a promising material in the electronic packaging field.     

Textured BaTi<Subscript>2</Subscript>O<Subscript>5</Subscript> ceramic synthesized by laser rapid solidification method and its dielectric properties

Textured poly crystalline barium dititanate BaTi₂O₅ (BT2) ceramics with a preferred 〈010〉 orientation were synthesized by laser rapid solidification method, with a CO₂ laser. The 〈010〉 orientation of the BT2 is along the laser incident direction, and the orientation factor (f) and relative density of the unannealed BT2 sample are 0.40 and 96.2%, respectively. The two quantities increase with increasing annealing time, and reach the maximum values of 0.42 (annealed at 1,000 °C for 12 h) and 97.5% (annealed at 1,000 °C for 24 h), respectively. The images of scanning electron microscopy reveal that the BT2 are composed of flake-like microstructures with the maximum thickness of 20 μm and dimension of 0.6 mm, which are parallel to the laser incident direction. The measured Curie temperature (T _c) and the maximum dielectric constant (ε_max) are 443 and 6,000 °C, respectively.     

Some physical properties and Vickers hardness measurements of Fe diffusion-doped Bi<Subscript>1.8</Subscript>Pb<Subscript>0.35</Subscript>Sr<Subscript>1.9</Subscript>Ca<Subscript>2.1</Subscript>Cu<Subscript>3</Subscript>O<Subscript>y</Subscript> superconductors

In this study we have investigated the influence of iron diffusion and diffusion-annealing time on the mechanical and the superconducting properties of bulk Bi_1.8Pb_0.35Sr_1.9Ca_2.1Cu₃O_y superconductors by performing X-ray diffraction (XRD), scanning electron microscopy (SEM), Vickers hardness, dc resistivity (ρ-T) and critical current density (J_c) measurements. The samples are prepared by the conventional solid-state reaction method. Doping of Bi-2223 was carried out by means of iron diffusion during sintering from an evaporated iron film on pellets. Then, the Fe layered superconducting samples were annealed at 830 °C for 10, 30 and 60 h. The mechanical properties of the compounds have been investigated by measuring the Vickers hardness (H_v). The mechanical properties of the samples were found to be load dependent. The load independent Vickers hardness (H₀), Young’s modulus (E), yield strength (Y), and fracture toughness (K_IC) values of the samples are calculated. These all measurements showed that the values of the Vickers hardness, critical current density, and critical transition temperature and lattice parameter c increased with increasing Fe doping and diffusion-annealing time.     

High voltage SnO<Subscript>2</Subscript> varistors prepared from nanocrystalline powders

In this study, SnO₂-based varistors were prepared from mechanically activated nanocrystalline powders. Nanocrystalline powders were derived by subjecting the initial powders to intensive high-energy activation with different times and ball to powder ratio. The effect of activation parameters on the powder properties and sintering temperature, as well as microstructural, micro-electrical and macro-electrical properties of the final specimens was evaluated. Varistors derived from high-energy mechanical activation exhibit a higher density (98.3% relative density) and more refined microstructure upon sintering at 1,300 °C in comparison varistors prepared from conventional powders. Breakdown voltage and nonlinear coefficient were increased up to 24 kV/cm and 45 respectively.     

Low-temperature sintering of SiC reticulated porous ceramics with MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript> additives as sintering aids

SiC reticulated porous ceramics (SiC RPCs) was fabricated with polymer replicas method by using MgO–Al₂O₃–SiO₂ additives as sintering aids at 1,000∼1,450 °C. The MgO–Al₂O₃–SiO₂ additives were from alumina, kaolin and Talc powders. By employing various experimental techniques, zeta potential, viscosity and rheological measurements, the dispersion of mixed powders (SiC, Al₂O₃, talc and kaolin) in aqueous media using silica sol as a binder was studied. The pH value of the optimum dispersion was found to be around pH 10 for the mixtures. The optimum condition of the slurry suitable for impregnating the polymeric sponge was obtained. At the same time, the influence of the sintering temperature and holding time on the properties of SiC RPCs was investigated. According to the properties of SiC RPCs, the optimal sintering temperature was chosen at 1,300 °C, which was lower than that with Al₂O₃–SiO₂ additives as sintering aids.     

Varistor properties and aging behavior of ZnO-V<Subscript>2</Subscript>O<Subscript>5</Subscript>-Mn<Subscript>3</Subscript>O<Subscript>4</Subscript> ceramics with sintering process

The microstructure, electrical properties, and DC-accelerated aging behavior of the ZnO-V₂O₅-Mn₃O₄ ceramics were investigated at different sintering temperatures of 850–925°C. The microstructure of the ZnO-V₂O₅-Mn₃O₄ ceramics consisted of ZnO grain as a primary phase, and Zn₃(VO₄)₂ which acts as a liquid-phase sintering aid, in addition to Mn-rich phase as secondary phases. The maximum value (3,172 V/cm) and minimum value (977 V/cm) of breakdown field were obtained at sintering temperature of 850 and 900°C, respectively. The nonlinear coefficient exhibited the highest value, reaching 30 at 925°C and the lowest value, reaching 4 at 850°C. The optimum sintering temperature was 900°C, which exhibited not only high nonlinearity with 24 in nonlinear coefficient, but also the high stability, with %ΔE_1mA = −0.9% and %∆α = −12.5% for DC-accelerated aging stress of 0.85 E_1mA/85°C/24 h.     

Preparation and characterization of ZrB<Subscript>2</Subscript>-SiC ultra-high temperature ceramics by microwave sintering

ZrB₂-SiC ultra-high temperature ceramic composites reinforced by nano-SiC whiskers and SiC particles were prepared by microwave sintering at 1850°C. XRD and SEM techniques were used to characterize the sintered samples. It was found that microwave sintering can promote the densification of the composites at lower temperatures. The addition of SiC also improved the densification of ZrB₂-SiC composites and almost fully dense ZrB₂-SiC composites were obtained when the amount of SiC increased up to 30vol.%. Flexural strength and fracture toughness of the ZrB₂-SiC composites were also enhanced; the maximum strength and toughness reached 625 MPa and 7.18 MPa·m^1/2, respectively.     

Microstructure and mechanical properties of SiC<Subscript>P</Subscript>/SiC and SiC<Subscript>W</Subscript>/SiC composites by CVI

37.2 vol.% SiC_P/SiC and 25.0 vol.% SiC_W/SiC composites were prepared by chemical vapor infiltration (CVI) process through depositing SiC matrix in the porous particulate and whisker preforms, respectively. The particulate (or whisker) preforms has two types of pores; one is small pores of several micrometers at inter-particulates (or whiskers) and the other one is large pores of hundreds micrometers at inter-agglomerates. The microstructure and mechanical properties of 37.2 vol.% SiC_P/SiC and 25.0 vol.% SiC_W/SiC composites were studied. 37.2 vol.% SiC_P/SiC (or 25.0 vol.% SiC_W/SiC) consisted of the particulate (or whisker) reinforced SiC agglomerates, SiC matrix phase located inter-agglomerates and two types of pores located inter-particulates (or whiskers) and inter-agglomerates. The density, fracture toughness evaluated by SENB method, and flexural strength of 37.2 vol.% SiC_P/SiC and 25.0 vol.% SiC_W/SiC composites were 2.94 and 2.88 g/cm³, 6.18 and 8.34 MPa m^1/2, and 373 and 425 MPa, respectively. The main toughening mechanism was crack deflection and bridging.     

Low-temperature synthesis of Sr<Subscript>0.3</Subscript>Ba<Subscript>0.7</Subscript>Nb<Subscript>2</Subscript>O<Subscript>6</Subscript> ultrafine powder and its characteristics

Ultrafine strontium barium niobate (Sr_0.3Ba_0.7Nb₂O₆, SBN30) powders were prepared by urea method starting from a precursor solution constituting of Sr (NO₃)₂, Ba (NO₃)₂, NbF₅, urea and polyvinyl alcohol (PVA) as surfactant. Their structural behavior and morphology were examined by means of X-ray diffractometry (XRD) and Scanning electron microscopy (SEM). The results showed that the SBN30 powders crystallized to a pure tetragonal phase at annealing temperatures as low as 750 °C. The average particle size of SBN powders subjected to 750 °C was of the order of 150–300 nm. With increasing calcination temperature,however, the average particle size of the calcined powders increased. The SBN30 ceramic prepared from urea method can be sintered at temperature as low as 1,225 °C. The transition temperature from the ferroelectric phase to the paraelectric phase and the relative dielectric permittivity of the SBN30 powder were less than the corresponding values of the bulk ceramic. The permittivity and loss tangent (tan δ) at room temperature (1 kHz) was found to be 930 and below 0.025.     

Compressive deformation behavior of ternary compound Cr<Subscript>2</Subscript>AlC

The compressive properties of ternary compound Cr₂AlC at different temperatures and strain rates were studied. When tested at a strain rate of 5.6 × 10⁻⁴ s⁻¹, the compressive strength decreases continuously from 997 ± 29 MPa at room temperature to 523 ± 7 MPa at 900 °C. The ductile-to-brittle transition temperature is measured to be in the range of 700 to 800 °C. When tested in the strain rate range of 5.6 × 10⁻⁵ to 5.6 × 10⁻³ s⁻¹, Cr₂AlC fails in a brittle mode at room temperature, whereas the deformation mode changes from a brittle to a ductile as the strain rate is lower than 5.6 × 10⁻⁴ s⁻¹ when compressed at 800 °C. The compressive strength increases slightly with increasing strain rate at room temperature and it is less dependent on strain rate when tested at 800 °C. The plastic deformation mechanism of Cr₂AlC was discussed in terms of dislocation-related activities, such as kink band formation, delamination, decohesion of grain boundary, and microcrack formation.     

Microwave dielectric properties and its compatibility with silver electrode of LiNb<Subscript>0.6</Subscript>Ti<Subscript>0.5</Subscript>O<Subscript>3</Subscript> with B<Subscript>2</Subscript>O<Subscript>3</Subscript> and CuO additions

The influences of B₂O₃ and CuO (BCu, B₂O₃: CuO = 1:1) additions on the sintering behavior and microwave dielectric properties of LiNb_0.6Ti_0.5O₃ (LNT) ceramics were investigated. LNT ceramics were prepared with conventional solid-state method and sintered at temperatures about 1,100 °C. The sintering temperature of LNT ceramics with BCu addition could be effectively reduced to 900 °C due to the liquid phase effects resulting from the additives. The addition of BCu does not induce much degradation in the microwave dielectric properties. Typically, the excellent microwave dielectric properties of ε_r = 66, Q × f = 6,210 GHz, and τ _f  = 25 ppm/^oC were obtained for the 2 wt% BCu-doped sample sintered at 900 °C. Chemical compatibility of silver electrodes and low-fired samples has also been investigated.     

The influences of firing temperatures and excess PbO on the crystal structure and microstructure of (Pb<Subscript>0.25</Subscript> Sr<Subscript>0.75</Subscript>)TiO<Subscript>3</Subscript> ceramics

Polycrystalline samples of (Pb_0.25Sr_0.75)TiO₃ (PST75) were prepared by the solid-state reaction method. The effects of firing temperatures and excess PbO on PST75 ceramics were investigated. The PST75 was calcined between 600 and 1000 °C for 3 h and the sintering temperature ranged between 1050 and 1250 °C for 2 h. The optimized calcination and sintering conditions were identified as 950 and 1250 °C, respectively. The lattice parameter c increased, while the lattice parameter a decreased with increased firing temperatures. The average particle size and average grain size increased with increased firing temperatures. After the addition of PbO—excess 0, 1, 3, 5, and 10 wt%—in the PST75 samples, the lattice parameter a decreased. The average particle size and the average grain size increased with the increase of PbO. The porous microstructure slightly decreased with an increasing amount of PbO—up to 3 wt%—then slightly increased with the higher excess PbO. The density was improved by adding 3 wt% of excess PbO. A low dielectric loss was observed from the 3 wt% excess PbO sample.