Abstract This study is based on the numerical simulation of the mechanical response of yttrium-stabilized zirconia ceramic (3Y-TZP) dental implants as a function of their intrinsic geometry and masticatory loads. Samples (n=20) of 3Y-TZP ceramics were compacted, sintered at 1500 °C - 2h, and characterized by relative density, X-Ray diffraction (XRD), and scanning electron microscopy (SEM). The elastic parameters (modulus of elasticity and Poisson ratio), used in the numerical simulations, were measured by the Impulse Excitation Technique, and the bending strength was obtained using piston-on-three-balls testing. An authorial implant design and, comparatively, commercial implant CAD models were used in this study as an initial geometry of dental implant in a typical adult mandible anatomy. From CAD and CAE techniques, finite element models were generated for all implant geometries. Loading cases were considered based on different intensities (100N to 500N) and orientation angles (45° or 90°) to reproduce the human masticatory efforts. The numerical predictions were compared with finite element simulations of gold-standard titanium-based implants. The investigated 3Y-TZP sintered ceramics presented high densification (> 99%), with a microstructure formed by submicron equiaxed tetragonal zirconia grains. The 3Y-TZP average bending strength obtained from piston-on-three-balls testing is 1192 ± 99 MPa. For both dental implant geometries, the zirconia implants showed average strength of less than 550 MPa, which, in turn, is independent of the masticatory load value or orientation angle. All finite element predictions are 50% inferior to the corresponding measured flexural strength values and preliminarily enable the 3Y-TZP ceramics for dental implant applications without fracture risk.

In this work, mixtures of ceramic powders containing Al2O3 with different amounts of Y2O3 (1%, 3%, 5% and 10wt.%) along their cross-section were fabricated to obtain multilayer composites based on Al2O3 with different levels of Y3Al5O12 (YAG) as reinforcement. Monolithic cylindrical multilayer Al2O3 blocks were compacted and subsequentially, sintered at 1610°C for 4h. Phase stability, microstructural aspects, and physical and mechanical properties of the specimens were acquired by relative density, X-ray diffraction, scanning electron microscopy, Vickers hardness, fracture toughness, Young’s modulus and biaxial flexural strength measurements. The results indicated that monolithic alumina specimens exhibited relative density of 98%, with average hardness of 1203 ±83 HV, fracture toughness of 2.1 ±0.8 MPa.m1/2 and flexural strength of 187 ±64 MPa. Progressive incorporation of Y2O3 into the chemical composition of the specimens led to formation of the YAG phase by solid state reaction during sintering, which reduced hardness and increased densification, fracture toughness and flexural strength, with average values of HV=1023 ±28 HV, KIC=3.5 ±0.3 MPa.m1/2, σf=273 ±58 MPa and 14% Y3Al5O12 for the specimens with 10wt.% Y2O3. This improvement is probably associated with toughness mechanisms, such as crack deflection and residual thermal stresses between the phases present in the composites.

This work investigated the effect of a composite of tetragonal zirconia with alumina-reinforced Ceria (ATZ) previously synthesized, on the properties of alumina-based ceramics (Al2O3). Monolithic alumina powder and Al2O3 powder mixtures containing 5, 10, 15 and 20 wt.% of Ce-TZP/Al2O3 were processed by high energy milling, compacted and then sintered at 1600 °C - 2 h. Sintered pure alumina and composites were characterized by relative density, scanning electron microscopy, X-ray diffraction and surface roughness. Then, the elastic modulus, the Vickers hardness, the fracture toughness and the 4-point flexural strength were evaluated. The results indicated an increase in relative density as a function of the addition of ATZ, with values between 94.3 ± 0.8% and 98.9 ± 0.7%. The observed microstructure after sintering showed tetragonal ZrO2 grains with average sizes of 0.6 μm well dispersed in the Al2O3 matrix, which presents average grain sizes of around 1.5 μm. The crystalline phases identified in the composites were ZrO2-tetragonal and Al2O3 hexagonal. The addition of the composite (ATZ) in the alumina matrix generates a gradual reduction in the elastic modulus (398 ± 15 GPa ~366 ± 34 GPa) and in the hardness (20.5 ± 1 GPa ~17.3 ± 0.7 GPa) of the sintered ceramics. On the other hand, the addition of this same composite (ATZ) in the alumina matrix considerably increases the materials fracture toughness, reaching values of approximately 6.7 ± 0.9 MPa.m1/2. The same trend was observed in the flexural strength results which ranged from 258 MPa (5wt.% Ce-TZP/Al2O3) to 316 MPa (20wt.% Ce,Y-TZP/Al2O3). The Ce-TZP reinforcement acts as a toughening agent of the Al2O3 matrix due to the coupled mechanisms of toughening by zirconia phase transformation, residual stresses due to the difference in thermal expansion of the crystalline phases and differences in microstructural morphologies.

This work investigated the effect of adding ceria-stabilized tetragonal zirconia (Ce-TZP) on the fatigue behavior of alumina-based ceramic composites. Alumina powder (control group) and mixtures containing 5 wt.% (group A) and 20 wt.% (group B) of a commercial m-ZrO2/Al2O3/CeO2 powder mixture were milled/homogenized, compacted, sintered at 1600°C-2h, and submitted to hydrothermal degradation. The samples were characterized by relative density, microstructure, crystalline phases, and static mechanical properties. The cyclic fatigue strength was determined using the modified staircase method in 4-point bending tests. The results indicate that adding the m-ZrO2/Al2O3/CeO2 powder mixture to the Al2O3-matrix increases the tetragonal-ZrO2 grains (Ce-TZP) content, presenting 2.9 wt.% of Ce-TZP and 11.9 wt.% of Ce-TZP for group A and group B, respectively. Furthermore, the addition of Ce-TZP improves densification (98.5% → 99.1%) with a slight reduction in hardness and modulus of elasticity and a significant KIC increase of the composite (KIC = 6.7 MPa.m1/2, group B) when compared to monolithic alumina (KIC=2.4 MPa.m1/2). The fatigue strength limit of the control group was around 100 MPa, while the composites (groups A and B) presented the values of 279 MPa and 239 MPa, respectively. The results indicated that the incorporation of Ce-TZP significantly improves the fracture toughness of alumina-based ceramics. On the other hand, regarding the fatigue behavior, there was an increase in fatigue resistance in group A, resulting from the benefits of the t→m Ce-TZP grains transformation, which occurs during cyclic loading, producing a zone shielding that involves the tip of the crack, slowing its growth. The increase in the amount of Ce-TZP (group B) leads to an increase in the internal residual stresses between the phases due to anisotropy and difference in the thermal expansion coefficients, which accelerates the phase transformation and formation of microcracks at grain boundaries, reducing the fatigue strength of composites of group B.

The influence of Fe2O3 additions on the microstructure, mechanical properties and translucence of zirconia with 3 mol-% or 5 mol-% Y2O3 was evaluated. Samples were pressed with different thickness and sintered at 1475, 1500, 1550 and 1600°C for 2 h. Density, phases, microstructure, roughness, strength and translucency were analyzed. All samples showed densification greater than 99%. After sintering at 1600°C, the phase analysis revealed only tetragonal ZrO2 in samples with 3% Y2O3, while in samples with 5% Y2O3 the cubic ZrO2 phase was identified. Significant increase in the grain size was noted, when increasing the Y2O3 content from 3% to 5% from 0.8 µm to 2.3 µm for sintered samples at 1600°C. The strength was affected with Y2O3 content and no relevant influence of the Fe2O3 on density, microstructure or mechanical properties. Visible reflectance spectroscopy analyses, related to the CIELab scale, indicate variation in the contrast ratio as function of thickness of samples and coloring agent Fe2O3 content.

The planning and execution of the adequate welding procedure for the superduplex stainless steel (SAF 2507 SDSS) in multiple passes is a complex technological task since thermal cycling may cause the precipitation of harmful phases, such as the sigma (σ) and chi (χ) phases. For this reason, technical standards limit the maximum interpass temperature (T.I.) in an extremely conservative manner at 100 °C. In order to investigate a possibly wider temperature range for this procedure, SAF 2507-SDSS tubes were subjected to autogenous Tungsten Inert Gas (TIG) welding with interpass temperatures ranging from 150°C to 400°C. The different welding zones were characterized by microscopy, Vickers microhardness, and polarization corrosion tests. The results indicated that in the Fusion Zone (FZ), columnar grains of ferrite were formed surrounded by allotriomorphic austenite (AA), besides intragranular austenite (AI) and Widmanstätten austenite (AW). The heat-affected zone (HAZ) had a lower ferrite content and was composed of equiaxed grains of ferrite, also surrounded by AA, besides AI and AW. Hardnesses varied between HV272 and HV293, regardless of the region or the interpass temperature used. Furthermore, the corrosion resistance has not been significantly affected by the interpass temperatures between 150 °C and 400°C.

Abstract The aim of this work was to analyze the properties and shear bond strength (SBS) of lithium disilicate to resin cement before and after etching the glass-ceramic surfaces. Lithium-metasilicate samples were heat treated and characterized by Scanning Electron Microscopy, X-ray diffraction and roughness measurement. For the analysis of the shear bonding strength (SBS) of lithium disilicate to dental resin cement, three groups (n = 12) of Li2Si2O5 were prepared: 1°)without treatment (NT); 2°)surface etching with hydrofluoric acid(HF), followed by silane agent and adhesive treatment; 3°) surface treatment with a self-etching ceramic primer (SECP). After the heat-treatment, the samples had Li2Si2O5 crystalline phase dispersed in a residual amorphous phase. Roughness of the NT and SECP samples was smaller that of the HF samples. Samples without surface treatment (NT) had the lowest SBS (5.5MPa). HF(24.2MPa) and SECP(24.8MPa) samples has similar SBS. Weibull statistics showed that HF-samples are more reliable than NT and SECP. The SBS was significantly increased by either HF etching and SECP surface treatment. While the chemical characteristics of the surface submitted to SECP treatment are considered to be responsible for the SBS increase, the main adhesion mechanism after HF etching is the increase in surface roughness.

Abstract Ti-6Al-4V and TiAl-based alloys are widely used for fabricating the implantable orthopedic devices and automotive components, respectively. Ti6Si2B-based alloys are attractive for use in orthopedic components because their higher hardness, superior biocompatibility and corrosion resistance in simulated body fluid than Ti and Ti-6Al-4V alloy. Limited information on Ti6Si2B stability in Co-dopped 67Ti-22Si-11B alloys are available in literature. This work presents the effect of cobalt doping and milling time on microstructure and Vickers microhardness of 65Ti-2Co-22Si-11B and 61Ti-6Co-22Si-11B (at-%) alloys produced by spark plasma sintering at 1100 oC for 12min using 20MPa. Samples were characterized by X ray diffraction, scanning electron microscopy, energy dispersive spectrometry, laser particle size analysis, and Vickers microhardness. Sintered alloys with 2 and 6at-%Co indicated the major presence of Ti6Si2B and Ti5Si3 dissolving up to 2.7 and 4.2 at-%Co, respectively, besides the minor precipitates of CoTi2 (4.4-16.7at-%Si) and CoTi (4.6-4.7at-%Si). Vickers microhardness of the sintered 65Ti-2Co-22Si-11B and 61Ti-6Co-22Si-11B alloys were in the range of 950-1050 and 1050-1150HV, respectively. Although the increase from 2 to 6at-%Co has reduced the Ti6Si2B stability, the Co-rich phases increased their hardness values up to 1150HV (11.3GPa), which are superior than those of commercial Ti alloys used for joint orthopedic components and automotive rotating parts.

ABSTRACT New techniques for manufacturing of biomaterials using additive/substrate manufacturing such as melting laser sintering (SLM) or CAD/CAM milling use micrometric metal powders to build custom parts. CoCrMo alloys are commonly used as biomaterials due to biocompatibility, high corrosion resistance and good mechanical properties. In this work, Cr-Co-based powder was obtained by mechanical alloying of Cr-Co-Mo-W alloy, using different Ball/Powder-Ratios (BPR) and thermal treatments. The powders were deagglomerated and characterized by X-ray diffraction (XRD) and Scanning electron microscopy (SEM). Based on SEM micrographs, the particle size analysis was used to compare the particles spheroidizing degree, using Feret’s diameter. The XRD patterns shown Co(solid-solution) as crystalline phase. The results of particles size indicates a decrease of Feret’s diameter in BPR (Ball/Powder-Ratio) from 4:1 to 6:1 understanding that from this ratio there is no significant decrease of this relation but there is an average size increase with losses in morphological aspect. The comparison between atomized powders and powder developed in this work indicates that atomized products present relation close to one which indicates there is uniformity in the particles spherical shape. Comparing ground powders from 6:1 ratio (before and after thermal treatment) there is a considerable decrease of Feret’s diameter being it decreased from 1.75 to 1.4, an increase of about 46% in particles spheroidizing.

Abstract In this work, CoCrMo-base alloys specimens were produced by additive manufacturing using selective laser melting (SLM) as well as CAD/CAM milling. For SLM specimens, spherical particles were laser processed at 1320°C under argon atmosphere and submitted to thermal stress relieving at 750°C–45min. Specimens from CoCrMo blocks were milled by CAD/CAM machining and sintered at 1300°C–60min. The materials from both techniques were characterized by relative density, dilatometry, SEM/BSE, OM and XRD analysis. The mechanical properties were determined by Vickers hardness and tensile tests. The specimens from both techniques exhibited single phase γCo (FCC) and CTE of 14 x10-6 °C-1. Relative density of 95.4%/ 85.6%, hardness values near 400HV/ 350HV and UTS of 905MPa/ 780MPa were measured for SLM and CAD/CAM specimens, respectively. Higher relative density is the main factor for increased mechanical properties of SLM specimens. On the other hand, both SLM and CAD/CAM specimens present properties in accordance with ISO-22674 recommendations, compatible with dental applications such as bridges containing four or more elements as well as fully dense pontics.

ZrO2(Y2O3)-based ceramics are widely used as biomaterials due to high fracture toughness, resulting from the tetragonal-monoclinic phase transformation in which the ceramic is submitted during crack propagation. In this context, studies involving the possibility of optimization of the tetragonal phase are important for the properties improvement of this ceramic. This study investigated the recovery of tetragonal phase from a previously transformed ZrO2(3 mol% Y2O3) ceramic. Zirconia samples were sintered at 1450 °C, at 1530 °C - 2 h and at 1600 °C - 4 h, in order to obtain materials with distinct microstructural features. The sintered samples were characterized by relative density, X-ray diffraction and scanning electron microscopy. Samples sintered at 1450 °C, 1530 °C - 2 h and 1600 °C - 4 h, presented relative densities of 94.2, 99.6 and 99.7% with grains size averages of 0.28, 0.49 and 1.31 µm, respectively. All samples were submitted to milling to induce the tetragonal→monoclinic phase transformation presenting 5, 50 and 65 vol% of monoclinic phase. Subsequently, heat treatments between 400 °C and 1200 °C were conducted to retransform monoclinic in tetragonal phase. It has been found that the smaller the grain size after sintering, the lower the necessary annealing temperatures for fully recovering of tetragonal phase. Annealing temperatures of 950, 1100 and 1200 °C were sufficient to recover almost fully the tetragonal phase.

RESUMO O objetivo deste trabalho foi a recuperação de descartes de ZrO2(Y2O3) oriundos de laboratórios de próteses dentárias, a partir do seu reprocessamento. Os descartes de ZrO2(Y2O3) foram fragmentados, peneirados e calcinados a 900ºC. Pós com tamanho menor que 32μm foram prensados uniaxialmente a 100MPa e sinterizados em temperaturas entre 1400 e 1600ºC-120min. Análise de difração de raios X realizadas nos materiais calcinados indicaram a presença majoritária da fase ZrO2 tetragonal. Os compactos apresentaram densidade a verde próximo a 47% e as amostras sinterizadas tiveram sua densidade relativa variando entre 83,5% e 95%, para temperaturas de sinterização de 1400 e 1600ºC, respectivamente. Os resultados da análise de difração de raios X indicaram a presença da fase ZrO2 tetragonal, com dureza Vickers e tenacidade máxima obtidos para as amostras sinterizadas a 1600ºC, da ordem de 1100 HV e 5,7 MPa.m1/2 respectivamente.

ABSTRACT The objective was the recovery of ZrO2(Y2O3) discarded arising from dentistry prosthetic laboratories. ZrO2(Y2O3) were fragmented, sieved and calcined at 900°C. Powders with size less than 32μm were uniaxially pressed to 100MPa and sintered at temperatures between 1400 and 1600ºC-120min. X-ray diffraction analysis performed on the calcined material showed the predominant presence of tetragonal ZrO2 phase. The green compact had the density close to 47% and sintered samples had a relative density ranging between 83.5% and 95% for sintering temperatures of 1400 and 1600ºC, respectively. The analysis results of X-ray diffraction indicated the presence of the tetragonal ZrO2 phase, with maximum Vickers hardness and toughness obtained for the samples sintered at 1600ºC, of the order of 1100 HV and 5.7 MPa.m1/2 respectively.

The focus of this work was to determine microstructural features in commercial Ni-Cr alloys which could be used to identify indirectly the presence of beryllium. Thus, eight commercial alloys were characterized by chemical analysis, thermal analysis, X-ray diffraction (XRD), scanning electron microscopy - back-scattered electron images (SEM/BSE), energy-dispersive spectroscopy (EDS). The results indicate that the presence of beryllium can be inferred from microstructural analysis via XRD and SEM/BSE. The X-ray diffractograms of the beryllium-containing alloys showed clearly the existence of the NiBe intermetallic phase. SEM/BSE images of these alloys show a very characteristic eutectic microstructure which also indicates the presence of this element. These characteristics are not observed in the beryllium-free alloys.

AIM: To investigate the effect of the cooling rate on flexural strength of monolayer and bilayer porcelain/zirconia (Y-TZP) bars.METHODS: Forty-five specimens were made for each design group: (PM) monolithic specimens of veneer porcelain Vita VM9 (Vita, Germany); (ZM) monolithic specimens of zirconia (ZiHP; ProtMat, Brazil); (PB) bilayer specimens zirconia/porcelain with porcelain on lower surface; and (ZB) bilayer specimens porcelain/zirconia with zirconia on lower surface. Each group was cooled by three different methods after porcelain sintering: slow specimens were cooled inside the turned-off furnace; normal specimens were removed from the furnace and cooled in air at room temperature; and fast specimens were removed from the furnace at 910°C and cooled by compressed air for 10 s. Specimens were polished and flexural strength was measured in water at 37 °C (n=15). Maximum load at fracture was recorded, and equations for simple (monolayer) and composite (bilayer) structures were used to calculate the flexural strength. RESULTS were analyzed using one-way ANOVA (p<0.05) and Tukey test separately for each design.RESULTS: The results of one-way ANOVA were statistically significant only for the PB group. The post-hoc Tukey test showed the highest flexural strength for fast cooling and the lowest for slow cooling; the normal cooling was statistically similar to both.CONCLUSIONS: Cooling methods affected only the flexural strength of bilayer specimens with porcelain on low surface (under tension) when the slow cooling method was used.

In this work, the static mechanical properties and cyclic fatigue life of 3 mol. (%) Y2O3-stabilized tetragonal zirconia polycrystalline (3Y-TZP) ceramics were investigated. Pre-sintered samples were sintered in air at 1600 °C for 120 minutes, and characterized by X ray diffraction and scanning electronic microscopy. Hardness and fracture toughness were determined by Vicker's indentation method, and Modulus of Rupture was determined by four-point bending testing. Fully dense sintered samples, near to 100% of theoretical density, presented hardness, fracture toughness and bending strength of 13.5 GPa, 8.2 MPa.m½ and 880 MPa, respectively. The cyclic fatigue tests were also realized using four-point bending testing, within a frequency of 25 Hz and stress ratio R of 0.1. The increasing of load stress lead to decreasing of the number of cycles and the run-out specimens number. The tetragonal-monoclinic (t-m) ZrO2-transformation observed by X ray diffraction contributes to the increasing of the fatigue life. The 3Y-TZP samples clearly presents a range of loading conditions where cyclic fatigue can be detected.