3 research outputs found

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

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    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 beta-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, beta-TCMP, has been investigated by crystallization from a glass composed of 52.75 wt% 3CaO center dot 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. and 1100 degrees 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 degrees C and 1100 degrees C, and the formation of diopside in samples treated at 1100 degrees 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 beta-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 degrees C for 4 h, respectively

    Non-isothermal crystallization kinetics of a Si-Ca-P-Mg bioactive glass

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    In this work, the crystallization process of a SiO2-3CaO center dot P2O5-MgO glass was studied by non-isothermal measurements using differential thermal analysis carried out at various heating rates. X-ray diffraction at room and high temperature was used to identify and follow the evolution of crystalline phases with temperature. The activation energy associated with glass transition, (E (g)), the activation energy for the crystallization of the primary crystalline phase (E (c)), and the Avrami exponent (n) were determined under non-isothermal conditions using different equations, namely from Kissinger, Matusita \& Sakka, and Osawa. A complex crystallization process was observed with associated activation energies reflecting the change of behavior during in situ crystal precipitation. It was found that the crystallization process was affected by the fraction of crystallization, (x), giving rise to decreasing activation energy values, E (c)(x), with the increase of x. Values ranging from about 580 kJ mol(-1) for the lower crystallized volume fraction to about 480 kJ mol(-1) for volume fractions higher than 80 % were found. The Avrami exponents, calculated for the crystallization process at a constant heating rate of 10 A degrees C min(-1), increased with the crystallized fraction, from 1.6 to 2, indicating that the number of nucleant sites is temperature dependent and that crystals grow as near needle-like structures
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