J.K.M.F. Daguano

Development and characterization of 3CaO·P2O5-SiO2-MgO glass-ceramics with different crystallization degree

The CaO-P2O5-SiO2-MgO system presents several compounds used as biomaterials such as hydroxyapatite (HA), tricalcium phosphate (TCP) and TCP with magnesium substituting partial calcium (TCMP). The β-TCMP phase with whitlockite structure has interesting biological features and mechanical properties, meeting the requirements of a bioactive material for bone restoration. In this work, the production of Mg-doped TCP, β-TCMP, has been investigated by crystallization from a glass composed of 52.75 wt% 3CaO·P2O5, 30 wt% SiO2 and 17.25 wt% MgO (i.e., 31.7 mol% CaO, 10.6 mol% P2O5, 26.6 mol% MgO and 31.1 mol% SiO2) using heat treatments between 775 °C and 1100 °C for up to 8 h. The devitrification process of the glass has been accompanied by differential scanning calorimetry (DSC), high-resolution X-ray diffraction (HRXRD), relative density and bending strength measurements. The characterization by HRXRD and DSC revealed the occurrence of whitlockite soon after the bulk glass preparation, a transient non-cataloged silicate between 800 °C and 1100 °C, and the formation of diopside in samples treated at 1100 °C as crystalline phases. The overall crystalline fraction varied from 26% to 70% depending on the heat treatments. Furthermore, contraction of the a-axis lattice parameter and expansion of the c-axis lattice parameter of the whitlockite structure have been observed during the heat treatments, which were attributed to the β-TCMP formation with the partial substitution of Ca2+ by Mg2+. Relative densities near 99% and 97% for the glass and glass-ceramics respectively indicated a discrete reduction as a function of the devitrification treatment. Bending strengths of 70 MPa and 120 MPa were determined for the glass and glass-ceramic material crystallized at 975 °C for 4 h, respectively.

Improvement of the Mechanical Properties of Glasses Based on the 3CaO.P2O5-SiO2-MgO System after Heat-Treatment

Glasses based on the 3CaO.P2O5-SiO2-MgO system present high bioactivity aiming the use as bone restorations. On the other hand, the low mechanical properties reduce the importance of this glass aiming the use as restoration bulk specimens. In this work, glass-ceramics were obtained by devitrification of this glass using different temperatures. CaCO3, SiO2, MgO and Ca(H2PO4).H2O were used as starting-powders. Powder mixture was milled/homogenized and melted at 1600°C, for 2h and annealed at 700°C for 4h with cooling rate of 3°C/min. Glass specimens of 151550mm3 were characterized by DTA and XRD analysis. Specimens were heat-treated in different temperatures between 7000C and 1050°C, for 4 hours, obtaining glass-ceramics with different crystallized phase content. Hardness and fracture toughness were determined and correlated with crystalline phase content. The results indicated that crystallization-degree increase with the temperature, and the mechanical properties are improved: Hardness values present increases lower than 20% as function of the crystallization. Fracture toughness may increase 100% as function of temperature (crystallization degree).

Effect of Isothermal Sintering Time on the Properties of the Ceramic Composite ZrO2-Al2O3

In this work the influence of isothermal sintering time on the microstructural development of ZrO2-Al2O3 composite was studied. Powder mixture of ZrO2 containing 20 wt% Al2O3 was prepared by milling, compaction and sintering at 16000C, in air. The isothermal sintering time at 16000C was varied between 0 and 1440 min. The sintered samples were characterized in terms of phase composition and relative density. Their microstructures were characterized by grain size distributions and average grain size. These results were evaluated using the classic grain growth equation as a function of time, determining the grain growth exponent of these materials. Furthermore, the microstructural aspects were related to the mechanical properties (Vicker’s hardness and fracture toughness) of these composites.

O compósito ZrO2-Al2O3 para aplicação como implante odontológico

In the present work, the influence of the temperature and sintering time on the microstructural development of ZrO2-Al2O3 ceramic composite was studied, aiming at the viability of the application of this material as dental material. Tetragonal ZrO2 powder (Y-TZP) with additions of 20wt.% of Al2O3 were mixed, pressed and sintered at 1500 or 1600°C. In each temperature, the isothermal sintering time varied between 0 and 480 minutes. Sintered samples were characterized by crystalline phases, microstructure, relative density, hardness and fracture toughness. For primary biological evaluation, cytotoxicity tests based on cellular culture of mammals were carried through. The results indicated that in all sintering conditions the samples presented only two crystalline phases, tetragonal -ZrO2 e a-Al2O3. An increase of the mechanical properties values as a function of the sintering temperature increase was observed, due to the increase on the densification. On the other hand, the increase of the isothermal sintering time causes a considerable reduction in the hardness and fracture toughness, which can be related to the ZrO2 and Al2O3-grain growth. The biological evaluation demonstrated that these bioceramics are biocompatible, presenting cellular growth during the cytotoxic test, indicating that these ceramic composite can be characterized as biomaterials adjusted for the application in implantations.