Preparation of nanostructured TiO2 ceramics by spark plasma sintering

The effect of spark plasma sintering (SPS) on the densification of TiO₂ ceramics was investigated using a nanocrystalline TiO₂ powder. A fully-dense TiO₂ specimen with an average grain size of ∼200 nm was obtained by SPS at 700 °C for 1 h. In contrast, a theoretical density specimen could only be obtained using conventional sintering above 900 °C for 1 h with an average grain size of 1-2 μm.     

Microstructure and mechanical properties of silicon nitride-titanium nitride composites prepared by spark plasma sintering

Si₃N₄-TiN composites were prepared by spark plasma sintering (conventional sintering (SPS1) and in situ reaction sintering (SPS2)). Homogeneous distribution of equiaxed TiN grains in Si₃N₄ matrix results in the highest microhardness (21.7 GPa) and bending strength (621 MPa) of sample SPS1 sintered at 1550 °C. Dispersion of elongated TiN grains in Si₃N₄ matrix results in the highest fracture toughness (8.39 MPa m^1/2) of sample SPS2 sintered at 1300 °C.     

Study on the structure and properties of fine-grained alumina fast sintered with high heating rate

Fine-grained alumina was obtained in 2 min by a new densification method based on Self-propagating High-temperature Synthesis plus Quick Pressing (SHS/QP). The sample was densified to more than 99% of theoretical density under a large mechanical pressure (100 MP) and a fast heating rate (1600 °C/min). Compared with the alumina sample obtained by spark plasma sintering (SPS) at lower heating rates (100 or 500 °C/min), almost no grain growth was found in the sample obtained in this work. The microstructure and mechanical properties were studied. Hardness value of 18.6 ± 0.4 GPa and fracture resistance value of 3.4 ± 0.3 MPa m^1/2 were measured for fine-grained alumina of this work. The densification mechanism was discussed.     

Processing of porous Ti and Ti5Mn foams by spark plasma sintering

Titanium and its alloys are one of the best metallic biomaterials to be used for implant application. In this study, porous Ti and Ti5Mn alloy with different porosities were successfully synthesized by powder metallurgy process with the addition of NH₄HCO₃ as space holder and TiH₂ as foaming agent. The consolidation of powder was achieved by spark plasma sintering process (SPS) at 16 MPa and pressureless conditions. The morphology of porous structure was investigated by using scanning electron microscopy (SEM) and X-ray micro-tomography (μ-CT). Nano-indentation tester was used to evaluate Young’s modulus of the porous Ti and Ti5Mn alloy. Experimental results showed that pure Ti sample, which sintered under pressure of 16 MPa, full relative density was achieved even at a relative low sintering temperature 750 °C; however, in the case of pressureless condition at sintering temperature 1000 °C the porosity was 53% and Young’s modulus was 40 GPa. The Ti5Mn alloy indicated a good pore distribution, and the porosity decreased from 56% to 21% by increasing the sintering temperature from 950 °C to 1100 °C. Young’s modulus was increased from 35 GPa to 51.83 GPa with increasing of the sintering temperatures from 950 °C to 1100 °C.     

Fabrication and mechanical properties of monolithic MoSi2 by spark plasma sintering

Fine MoSi₂ powders containing a small amount of Mo₅Si₃ have been prepared by self-propagating high-temperature synthesis (SHS), followed by spark plasma sintering (SPS) for 10 min at 1200-1500°C and 30 MPa. Dense MoSi₂ materials, in which the grain size is ∼7.5 μm, have been fabricated at 1300°C. They exhibit excellent mechanical properties: Vicker’s hardness H_v (10.6 GPa), fracture toughness K_IC (4.5 MPa m^1/2), and bending strength σ_b (560 MPa). The strength of 325 MPa can be retained up to 1000°C.     

Synthesis and evaluation of Zr0.5Ti0.5B2 solid solution

Boride ceramics are useful materials because of their high strengths, hardness and melting points, which allow them to be used as high-temperature structural materials. In this study, sintered bodies of a solid solution of ZrB₂-TiB₂ system were prepared using hot pressing (HP) and spark plasma sintering (SPS). The sintering behavior was evaluated, and the effect of pulverization on sinterability and reactivity was examined using a Nanomizer. The combination of SPS processing at 2200 °C and pulverization yielded a nearly single-phase Zr_0.5Ti_0.5B₂ solid solution having a relative density of 95%.     

Preparation of W–Sc2O3 targets and scandate cathodes with film prepared by pulsed laser deposition

Sub-micrometer Sc₂O₃–W powder with a narrow particle size distribution has been obtained by a sol–gel method combined with two-step hydrogen reduction process. Based on the obtained powder, the W–Sc₂O₃ targets have been sintered via spark plasma sintering (SPS) at 1300 °C. The W–Sc₂O₃ targets have the average grain size of about 1 μm. Both the sintering temperature and holding time are much lower than those of the targets prepared with micrometer sized powders. The obtained W–Sc₂O₃ targets have a high comparative density of 96.4% and rockwell hardness of 86.4 HRC. Using the target, the scandate cathode deposited with a film containing 5% Sc₂O₃ and 95% W has been obtained by pulsed laser deposition (PLD) method. This cathode has good emission property, i.e., the highest thermionic emission current density reaches 43.09 A/cm² of J_div at 900 °C_b after being activated for 8 h, which is much higher than that of scandate cathode without film. Scandium (Sc) supplied by the film on the surface during the activation forms a Ba–Sc–O active layer, which helps to the emission.     

Effect of phosphorus addition on the sintering and dielectric properties of Pb(Zr0.52Ti0.48)O3

It has been found that the sintering temperature of piezoelectric Pb(Zr_0.52Ti_0.48)O₃ (PZT) can be reduced by phosphorus addition without compromising the dielectric properties. A sintered density of 98.6% of the theoretical density was obtained for 2 wt.% P₂O₅ addition after sintering at 1050 °C for 4 h. The P₂O₅ addition, either above or below 2 wt.%, showed an inferior densification. Coincidentally, the P₂O₅ addition gave rise to a lower lead loss, and the dielectric constant showed a peak at 1 wt.% P₂O₅ addition.     

Spark plasma sintering of Co-WC cubic boron nitride composites

25 vol.% cubic boron nitride (cBN) added tungsten carbide (WC) powders containing 6 wt.% Co (WC-6Co) were densified by spark plasma sintering (SPS) technique under different experimental conditions and the effect of cBN addition on the microstructure, mechanical properties and thermal conductivity were investigated. Over 99.5% theoretical density was achieved for WC-6Co-cBN composites sintered at 1300 °C, under 75 MPa pressure for 7.5 min. Under these conditions, cBN → hBN phase transformation was not observed.     

Synthesis of BaTi4O9 ceramics by reaction-sintering process

Synthesis of BaTi₄O₉ ceramics by a reaction-sintering process was investigated. The mixture of raw materials for stoichiometric BaTi₄O₉ were pressed and sintered into ceramics without any calcination stage involved. Pure BaTi₄O₉ phases were obtained at 1150-1280 °C. High-sintered density, 98.2-99.5% of theoretical value (4.533 g/cm³), can be obtained for pellets sintered at 1200-1280 °C for 2-6 h. Some rod-shaped grains 3-7 μm in the longitudinal axis appear in pellets sintered at 1230 °C. Both the size and the amount of these rod-shaped grains increase at higher sintering temperature.     

Spark plasma sintered tantalum carbide: Effect of pressure and nano-boron carbide addition on microstructure and mechanical properties

TaC and TaC-1 wt.% B₄C powders were consolidated using spark plasma sintering (SPS) at 1850 °C and varying pressure of 100, 255 and 363 MPa. The effect of pressure on the densification and grain size is evaluated. The role of nano-sized B₄C as sintering aid and grain growth inhibitor is studied by means of XRD, SEM and high resolution TEM. Fully dense TaC samples were produced at a pressure of 255 MPa and higher at 1850 °C. The increasing pressure also resulted in an increase in TaC grain size. Addition of B₄C leads to an increase in the density of 100 MPa sample from 89% to 97%. B₄C nano-powder resists grain growth even at high pressure of 363 MPa. The formation of TaB₂/Carbon at TaC grain boundaries helps in pinning the grain boundary and inhibiting grain growth. The effect of B₄C addition on hardness and elastic modulus measured by nanoindentation and the indentation fracture toughness has been studied. Relative fracture toughness increased by up to 93% on B₄C addition.     

Rapid fabrication of in situ TiC particulates reinforced Fe-based composites by spark plasma sintering

TiC particulates reinforced Fe-based composites have been fabricated using ferrotitanium and carbon black powders with the combination of in situ and spark plasma sintering (SPS) technique. The sintering and densification behaviors were investigated. The results show that when the composite was sintered at 1150 °C for 5 min, the maximum relative density and hardness are 99.2% and 83.2 HRA, respectively. The phase evolution during sintering indicates that the in situ reaction occurs evidently between 850 °C and 1050 °C. The microstructure investigation demonstrates that with the rapid in situ SPS technique, fine TiC particulates with a size of ~ 1 μm are homogeneously distributed in the matrix.     

Effect of the sintering temperature on the properties of Ce0.85La0.10Ca0.05O2−δ electrolyte material

Rare earth and alkaline earth co-doped Ce_0.85La_0.10Ca_0.05O_2−δ electrolyte material with the powder obtained by solid-state reaction method was sintered at 1300, 1400, 1500 and 1600 °C respectively. The results showed that the ionic conductivity of the sample sintered at 1400 °C was slightly lower compared to that sintered at 1500 °C in the temperature range of 300-550 °C, while the sample sintered at 1400 °C showed the highest ionic conductivity in all the samples above 550 °C. The ionic conductivity of ∼0.021 S/cm at 600 °C and the relative density of 98.2% were observed for the sample sintered at 1400 °C. In addition, the highest flexural strength with 145 MPa was also obtained for the sample sintered at 1400 °C. It suggested that the sintering temperature for Ce_0.85La_0.10Ca_0.05O_2−δ electrolyte may be reduced to as low as 1400 °C with desired properties.     

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.     

Microwave dielectric properties and microstructures of CuO- and ZnO-doped LaAlO3 ceramics

The microwave dielectric properties and the microstructures of 0.25 wt.% CuO-doped LaAlO₃ ceramics with ZnO additions have been investigated. The sintered LaAlO₃ ceramics are characterized by X-ray diffraction spectra and scanning electron microscopy (SEM). Tremendous reduction in sintering temperature can be achieved with the addition of sintering aids CuO and ZnO. The ceramic samples show that dielectric constants (ε_r) of 22−24 and Q×f values of 33,000−57,000 (at 9.7 GHz) can be obtained at low sintering temperatures 1340−1460°C. The temperature coefficient of resonant frequency varies from −24 to −48 ppm/°C. At the level of 0.25 wt.% CuO and 1 wt.% ZnO additions, LaAlO₃ ceramics possesses a dielectric constant (ε_r) of 23.4, a Q×f value of 57,000 (at 9.7 GHz) and a τ_f value of −38 ppm/°C at 1400°C for 2 h.     

Transparent polycrystalline ruby ceramic by spark plasma sintering

Fine-grained and transparent polycrystalline ruby ceramics (Cr₂O₃-doped Al₂O₃) were successfully prepared by spark plasma sintering (SPS). The effect of Cr₂O₃ concentration on the grain size, hardness, fracture toughness and thermal conductivity of ruby ceramics was investigated systematically. For 0.05 wt.% Cr₂O₃, high in-line transmittance of 85% at 2000 nm can be reached, further increase of Cr₂O₃ concentration leads to the decrease in transmittance. High hardness of 23.95-25.05 GPa can be achieved due to the fine grain size in all ruby ceramics. The fracture toughness of 1.9-2.29 MPa m^1/2 indicates that no improvement in fracture toughness over pure Al₂O₃ can be obtained by Cr₂O₃ doping in these submicron grained ruby ceramics. High thermal conductivity of 28-29.8 W/(m K) at room temperature, close to that of single crystal sapphire, can be achieved. The change in grain size for different Cr₂O₃ concentrations is the major reason for the change in mechanical and thermal properties, but not for the change in optical properties.     

Stoichiometric Pb(Mg1/3Nb2/3)O3 perovskite ceramics produced by reaction-sintering process

Stoichiometric lead magnesium niobate, Pb(Mg_1/3Nb_2/3)O₃ (PMN), perovskite ceramics produced by reaction-sintering process were investigated. Without calcination, a mixture of PbO, Nb₂O₅, and Mg(NO₃)₂ was pressed and sintered directly. Stoichiometric PMN ceramics of 100% perovskite phase were obtained for 1, 2, and 4 h sintering at 1250 and 1270 °C. PMN ceramics with density 8.09 g/cm³ (99.5% of theoretical density 8.13 g/cm³) and K_max 19,900 under 1 kHz were obtained.     

Reactive and dense sintering of reinforced-toughened B4C matrix composites

Reactive hot-press (1800-1880 °C, 30 MPa, vacuum) is used to fabricate relatively dense B₄C matrix light composites with the sintering additive of (Al₂O₃ +Y₂O₃). Phase composition, microstructure and mechanical properties are determined by methods of XRD, SEM and SENB, etc. These results show that reactions among original powders B₄C, Si₃N₄ and TiC occur during sintering and new phases as SiC, TiB₂ and BN are produced. The sandwich SiC and claviform TiB₂ play an important role in improving the properties. The composites are ultimately and compactly sintered owing to higher temperature, fine grains and liquid phase sintering, with the highest relative density of 95.6%. The composite sintered at 1880 °C possesses the best general properties with bending strength of 540 MPa and fracture toughness of 5.6 MPa m^1/2, 29 and 80% higher than that of monolithic B₄C, respectively. The fracture mode is the combination of transgranular fracture and intergranular fracture. The toughening mechanism is certified to consist of crack deflection, crack bridging and pulling-out effects of the grains.     

Sintering and dielectric properties of BaTiO3 prepared by a composite-hydroxide-mediated approach

High purity tetragonal BaTiO₃ powders consisted of uniform particles of ca. 150 nm in diameter were synthesized by a composite-hydroxide-mediated approach at 240 °C using a novel hydrothermal reaction apparatus with a rolling system. The product showed sinterability superior to the commercial powder, i.e., it could be sintered to full theoretical density at 1200 and 1100 °C without an additive and with 0.3 wt% of Li₂CO₃-0.04 wt% of V₂O₅ mixed sintering aid, respectively. The sintered body of the product also showed piezoelectric properties superior to the commercial one.     

Low temperature sintering and properties of piezoelectric PZT-PFW-PMN ceramics with YMnO3 addition

Low temperature sintering of Pb(Zr,Ti)O₃-Pb(Fe_2/3W_1/3)O₃-Pb(Mn_1/3Nb_2/3)O₃ (PZT-PFW-PMN) quaternary piezoelectric ceramics were studied with the use of YMnO₃ as sintering aid. The sintering aid improved the sinterability of PZT-PFW-PMN ceramics due to the effect of YMnO₃ liquid phase. The effects of YMnO₃ contents and sintering temperature on the phase structure, density, dielectric and piezoelectric properties were investigated. The results show that the sintering temperature can be decreased and the electrical properties can be maintained by the YMnO₃ addition. The optimized properties were obtained by doping 0.30 wt.% YMnO₃ and sintering at 1020 °C, which are listed as follows: d₃₃ = 341 pC/N, K_p = 0.57, Q_m = 1393, tan δ = 0.0053, T_c = 304 °C, P_r = 17.13 μC/cm² and E_c = 11.15 kV/cm, which make this system be a promising material for multilayer piezoelectric actuator and transformer applications.