Experimental analysis and numerical simulations of the mechanical properties of a (Ce,Y)-TZP/Al2O3/H6A ceramic composite containing coupled toughening mechanisms.

OBJECTIVES: This study investigates the simulation of the mechanical behavior of a bioceramic composite based on (Ce,Y)-TZP reinforced with equiaxed Al2O3 and platelet-shaped hexaaluminate (H6A) grains using Finit Element Method (FEM). METHODS: A commercial (Ce, Y)-TZP/Al2O3 ceramic powder was compacted into disc-shaped specimens that were sintered at 1500 °C for 2 h. The sintered samples were further subjected to hydrothermal degradation in an autoclave at 134 °C, 0.2 MPa, for 10 h and characterized according to their phase composition, microstructure, and relative density. Their flexural strength values were determined by the piston-on-three-ball test, and Weibull statistics was used to evaluate the results. Their hardness, fracture toughness and elastic parameters were also measured. Numerical simulations of the biaxial strength test were performed using the ABAQUS finite element code. RESULTS: The sintered ceramic composite material presented relative density >99%, high resistance to hydrothermal degradation, average hardness of 1435 ± 35 HV, fracture toughness KIC of 9.7 ± 0.5 MPa m1/2, and average biaxial flexural strength of 952.6 ± 88 MPa. The numerical predictions of the biaxial flexural strength showed a consistently lower average biaxial flexural strength value of 880.9 MPa, ∼10% lower than the average experimental results. CONCLUSIONS: The differences observed are attributed to the complex coupled toughness mechanisms of this material, not included in the finite element simulations.

Preparation of TiC/Ti3SiC2 Composite by Sintering Mechanical Alloyed Ti-Si-C Powder Mixtures.

The present work aims to evaluate the crystalline phases and microstructure of a TiC-Ti3SiC2 ceramic composite, obtained by mechanical alloying of Ti, C and Si powders and subsequent sintering. A mechanical alloying technique in a planetary ball mill for 1, 10, 50, 100 and 200 h using Ti, Si and C powders with molar ratios of 3:1:2 as feedstock in argon (Ar) gas was employed to prepare nano-sized Ti-Si-C powders. TiC crystallite size and lattice strain were evaluated by X-ray diffraction analysis (XRD) and the morphological characteristics and particle size distribution were examined using scanning electron microscope (SEM). After milling, a reduction of the average particle size and crystallinity is observed. Furthermore, after 10 h of milling time, TiC starts to crystallize. The powder mixture obtained after 200 h of milling was compacted and sintered at 1200 °C under controlled atmosphere, for 15 min, 2 h or 4 h with a heating rate of 5 °C/min. Almost full densification of samples sintered for 2 h and 4 h has been achieved, with relative densities close to 98.8±0.2% and TiC and Ti3SiC2 as crystalline phases with an average crystallite size of TiC near 0.7 µm. Rietveld refinement indicates that the majority TiC-cubic phase (>85 vol%) presents a unit cell volume of 8.03 nm³ after sintering at 1200 °C. Despite the maintenance of the volume of the hexagonal unit cell of Ti3SiC2, (15.05 nm³), the increase of the isothermal sintering time resulted in an increase of the lattice parameter "a", from 0.315 nm to 0.320 nm, and a reduction of the lattice parameter "c" from 1.750 nm to 1.705 nm. The control of the changes in the residual stresses within the TiC matrix and the Ti3SiC2 precipitates, which is associated with the deformation in the lattice parameters, must be controlled to achieve high fracture toughness in the composite.

Mechanical properties of lithium metasilicate after short-term thermal treatments.

OBJECTIVES: The properties of lithium-silicate dental glass-ceramics are very sensitive to heat treatments which are conducted after CAD/CAM (Computer Aided Design/Computer Aided Machining) processing. In particular, temperature variations inside the furnace chamber which may occur between different models of furnaces may result in altered mechanical properties of these materials. In this work, the effect of thermal treatment parameters on the transformation of lithium metasilicate (Li2SiO3) into lithium disilicate (Li2Si2O5) and on the resulting mechanical properties has been investigated. METHODS: Lithium metasilicate samples. containing 59 vol% of amorphous phase, were thermal treated under vacuum at 820 °C for up to 9 min or at 840 °C for 7min (as control group). The samples were characterized by X-ray diffraction analysis using the Rietveld refinement and scanning electron microscopy. Hardness and fracture toughness (n = 30 indentations/group) were evaluated by the Vickers indentation technique. The elastic properties were measured by the Impulse Excitation Technique and the flexural strength (n = 15/group) was measured using the piston-on-three-ball (P-3B) testing assembly. Complementary Weibull statistic were conducted as statistical analysis. RESULTS: The results indicate a progressive reduction of the Li2SiO3 phase with increasing isothermal holding time at 820 °C until the conversion into Li2Si2O5, is completed for treatments longer than 7 min. A complete transformation of Li2SiO3 into Li2Si2O5 has also been observed for the control group of samples treated at 840 °C for 7min. Samples of the control group exhibited hardness, fracture toughness, Young's modulus and Poisson ratio 5.76 ±â€¯0.17 GPa, 1.60 ±â€¯0.03 MPa m1/2, 100.3 GPa e 0.21, respectively. The reduction of the thermal treatment temperature to 820 °C reduced the fracture toughness and the Young's modulus between 5-10%. Furthermore, the fracture strength was significantly reduced by approximately 71%, because of the lower amount of elongated Li2Si2O5 grains and higher amount of residual amorphous phase. CONCLUSION: In general, the glass-ceramic material containing residual amorphous phase associated with various crystalline phases, presented a reduction of its mechanical properties in relation to the lithium disilicate glass-ceramic. The reasons for these differences in the mechanical behavior are discussed by analyzing the influences of different phenomena such as thermal expansion anisotropy, residual stresses, amorphous phase content and microstructure on the properties.

Bioactivity and cytotoxicity of glass and glass-ceramics based on the 3CaO·P2O5--SiO2--MgO system.

The mechanical strength of bioactive glasses can be improved by controlled crystallization, turning its use as bulk bone implants viable. However, crystallization may affect the bioactivity of the material. The aim of this study was to develop glass-ceramics of the nominal composition (wt%) 52.75(3CaO·P2O5)-30SiO2-17.25MgO, with different crystallized fractions and to evaluate their in vitro cytotoxicity and bioactivity. Specimens were heat-treated at 700, 775 and 975 °C, for 4 h. The major crystalline phase identified was whitlockite, an Mg-substituted tricalcium phosphate. The evaluation of the cytotoxicity was carried out by the neutral red uptake methodology. Ionic exchanges with the simulated body fluid SBF-K9 acellular solution during the in vitro bioactivity tests highlight the differences in terms of chemical reactivity between the glass and the glass-ceramics. The effect of crystallinity on the rates of hydroxycarbonate apatite (HCA) formation was followed by Fourier transformed infrared spectroscopy. Although all glass-ceramics can be considered bioactive, the glass-ceramic heat-treated at 775 °C (V775-4) presented the most interesting result, because the onset for HCA formation is at about 24 h and after 7 days the HCA layer dominates completely the spectrum. This occurs probably due to the presence of the whitlockite phase (3(Ca,Mg)O·P2O5). All samples were considered not cytotoxic.