Papers by Author: José Carlos Bressiani

Abstract: Y-TZP presents excellent properties at room temperature but these properties decrease as the temperature increases. This paper studies the behavior 20vol%Si3N4-SiC when added in YTZP matrix and heated under no pressure system. Al2O3 and Y2O3 were used to maintain the stability of the matrix and as sintering aids. The addition of Si3N4 and SiC in a Y-TZP matrix leads to formation of silicon oxynitride and it increases the mechanical properties like toughness and hardness. The mixture was milled and molded by CIP. Samples were heated at 1500°C, 1600°C and 1700°C for 2h without pressure under atmospheric conditions in bed-powders of Si3N4. Samples were characterized by XRD. Density, hardness, toughness, bending strength were measured. The structure of the material was observed in SEM/EPMA to verify the distribution of the materials in the composite. The formation of Si2N2O was observed in the sintered material and it showed an increment of both hardness and toughness as temperature increases. The samples presented considerable resistance of oxidation at 1000°C.

Abstract: In many in-vivo and in vitro studies, the behavior of calcium phosphate ceramics like β - tricalcium phosphate in biological environments has been reported to be predictive and positive. In terms of bone tissue growth, this ceramic can be more attractive presenting a porous microstructure. To obtain biomaterial quality ceramics, in this investigation β- TCP porous ceramics were prepared by a special consolidation method with albumin as a foam generating agent. This technique enables preparation a variety of formats with complex geometries. To obtain porous samples using albumin, heat had to be introduced into the system during the consolidation stage. After consolidation, the samples were sintered at 1250oC for 30 minutes and characterized using X-ray diffractometry, scanning electron microscopy and mercury porosimetry. The foams that were obtained by this method exhibited spherical and interconnected pores, characteristics desirable in biomedical implants.

Abstract: Nanocrystalline hydroxyapatite was prepared by a precipitation method with add of ultrasonic irradiation. In this work the effect of H3PO4 addition rate during synthesis and the influence of the magnesium incorporation into apatite were studded. The results revealed that the morphology and cristalinity of synthesized nanopowders are significantly affected by ultrasonic irradiation. Monophase hydroxyapatite was obtained when magnesium was added into HA lattice during the synthesis with ultrasonic irradiation.

Abstract: The shear bond strength between a ceramic material (Titankeramik®, Vita Zahnfabrik, Germany) and two biocompatible titanium alloys was investigated. Ti-13%Nb-13%Zr (TNZ) and Ti-35%Nb-7%Zr-5%Ta (TNZT) alloys were obtained based on the blended elemental technique followed by a sequence of cold uniaxial and isostatic pressing and sintering. Characterization involved microstructural analysis (SEM) and crystalline phase identification (XRD). Subsequently, samples were machined to 4 x 4 mm with a base of 5 x 1 mm. The base metals were blasted with Al2O3 particles followed by the application of a coupling agent and opaque ceramic. After ceramic firing, the specimens were loaded in a universal testing machine (0,5mm/min). XRD revealed the presence of α and β-phases for TNZ, and peaks related to β phases and Nb and Ta for the TNZT alloy. SEM evaluation (TNZ) depicted remaining pores and biphasic microstructure formation. SEM micrographs of the TNZT alloy revealed good densification and a homogeneous β structure. Shear bond strength data (MPa) were statistically analyzed (one-way ANOVA and Tukey test, α=.05) revealing that TNZT (37.6 ± 2.91) presented significant higher values (p=0.0002) compared to TNZ (26.03 ± 2.92). In conclusion, it seems that Ti alloy composition plays a significant role on ceramic bonding.

Abstract: Comparing to hydroxyapatite (HA), which forms a strong chemical bond with the bony tissues, metallic materials are not able to bond with bone. For this reason, a great variety of complex coating methods, such as pulse-laser deposition, ion-beam assisted deposition and plasma-spray has been used to form a HA layer onto metallic surfaces. This study evaluated the performance of the biomimetic technique on apatite-based coating formation on two Tialloys. Ti-13Nb-13Zr and Ti-35Nb-7Zr-5Ta were obtained via powder metallurgy. The Tibased alloys were biomimetically coated using a technique which was modified from the conventional ones using a sodium silicate solution as the nucleant agent. Both alloys presented similar behavior in the evaluated conditions which means the formation of a homogeneous and well defined HA coating. These results show that these new non-toxic Tialloys seem to be very promising for biomedical applications.

Abstract: Calcium phosphates with different Ca/P molar ratio can be obtained depending the precipitation conditions such as pH and temperature. In this work the effect of the pH’s variation during the H3PO4 addition in the synthesis of hydroxyapatite-HA, (Ca/P molar ratio 1.67) by neutralization method, was studied. The H3PO4 addition’s rate was 1.0, 1.5, 8.0 mL.min-1 and in other experiment the H3PO4 was added at a time. After the addition was completed the pH ranged from 7-12. The suspensions were kept during 24 hours for ripening. The precipitate was separated from the suspension by vacuum filtration, washed with distilled water and dried at 70°C/24h. Afterwards the materials were analyzed by thermogravimetric analysis (TGA) with heating rate of 10°C/min in air. The calcination of the powders was accomplished at 800°C/3h with heating rate of 10°C.min-1. The powders were characterized by X-ray diffraction (XRD), infrared spectrometry (FTIR), specific surface area (BET), and scanning electron microscopy (SEM). The results indicated that the ratio of addition of the acid can influence both the morphology and the formation of the phases (HA and TCP) in the obtained powders.

Abstract: In the last years, the porosity in ceramic materials for implants production has motivated the development of various technologies. Calcium phosphate ceramics, in special the tricalcium phosphate - TCP, are very promising as bone substitutes and scaffolds for tissue engineering. The macroporosity incorporation in TCP ceramics by porogenic, foaming and consolidator agent, as globular protein (ovalbumin) was the focus of this work. Preliminary studies of zeta potential were made to have a suitable suspension. Ovalbumin amounts (5-7 wt%) were added to the ceramic slurries and suspensions with a solid percentage higher than 60 wt% were obtained. The interaction albumin/surfactant with detergency properties was evaluated by pH and viscosity measurements. The foam was produced by mechanical stirring. The results suggested that the presence of the surfactant increase the volume and stability of foam. After drying, burnout and sintering (1200oC/30 min.) the phase composition of the foams was determined by X-ray diffraction. The microstructure and porosity were evaluated by scanning electron microscopy. SEM micrographs of the foam show that the structure consists of a permeable porous network, being observed spherical and interconnected pores.

Abstract: The sintering behavior of silicon carbide using alumina, silica and yttria as additives was investigated. Powders containing 90 vol. % SiC and 10 vol. % additives (keeping 1Y2O3:1Al2O3 molar ratio) were sintered at 1950°C/1h, in a dilatometer or a graphite resistance furnace. Thermal treatments were also done from 1500°C/1h up to 1800°C/1h, in order to evaluate the formation of transient crystalline secondary phases. The sintered samples were characterized through XRD, SEM and TEM analysis. The results showed that sintering behaviour is clearly related to the additive composition investigated, as demonstrated by linear shrinkages and linear shrinkages rate curves. Temperatures of particle rearrangment, solution-reprecipitation of SiC grains, as well as secondary crystalline phase(s) formation and dissolution could be revealed after dilatometric analysis. These temperatures are in good agreement with XRD results. Microstructural observations through SEM and TEM analysis are also related to the sintering behaviour.

Abstract: Densification curves of silicon nitride specimens with varying composition were determined with the aid of a dilatometer and these curves are presented in this paper. A novel procedure has been used to determine the densification curves as well as the temperature at which the rate of densification was highest. From these data, sintering profiles have been proposed to produce silicon nitride based ceramics with high apparent density (above 96% of theoretical density) at temperatures as low as 1520º C, with incipient grain growth. This procedure also enabled efficient separation of the densification and grain growth phenomena and it can be used in other two-step sintering studies.

Abstract: The influence of polymer precursor additions on liquid phase sintering of SiC:Al2O3:Y2O3 has been evaluated. Two polymer precursors were used: polymethylhydrogensiloxane and D4Vi (1,3,5,7-tetramethyl-1,3,5,7-tetraviniylcyclotetrasiloxane). The ceramic phase had the following composition in wt%: 91.6 SiC, 4.2 Al2O3 and 4.2 Y2O3. The composites were prepared using the following ceramic phase to polymer ratios in wt%: 82.7: 17.3; 74.0: 26.0 and 71.5: 28.5. Density measurements were carried out using a helium picnometry and the Archimedes method. The crystalline phases were identified by X-ray diffraction analysis and the microstructures were observed by optical and scanning electron microscopy.