Manganese oxides were synthesized during 40 min at 140 ºC via Microwave-Assisted Hydrothermal (MAH) method and treated at different temperatures in order to evaluate the phase evolution using structure refinement (Rietveld method). The samples obtained were heat treated at temperatures defined by means of thermal analysis (160 ºC, 480 ºC, 715 ºC, 870 ºC, 920 ºC and 1150 ºC) and analyzed by X-Ray Diffractometry (XRD), X-Ray Fluorescence (XRF), Fourier Transform Infrared (FTIR) spectroscopy, Raman scattering, UV-Vis absorption and Scanning Electron Microscopy (SEM). Structural characterizations allowed to identify five distinct phases:
Glass-ceramic materials were obtained by heat treatment (960 ºC for 2, 4, and 6 hs) of glasses with CaCO 3 47.50 wt%-TiO 2 23.75 wt%-SiO 2 23.75-Al 2 O 3 5.00 wt% formulation produced by the melt-quenching technique (melting at 1650 ºC and subsequent annealing at 650 ºC). The materials' structural characterization and crystallization kinetics (Kissinger method) indicate the presence of CaTiO 3 , CaSiO 3, and CaTiSiO 5 crystalline phases with activation energies 217, 281, and 446 kJ/mol, respectively. The structure refinement (Rietveld method) suggests metastability for the CaSiO 3 and CaTiSiO 5 phases as a function of the heat treatment time. The increase in time favors CaTiO 3 crystallization, from 62.97 wt%, in the 2 hs treated sample, to 79.21 wt%, in the 6 hs treated sample. EDS and microstructure analyses confirm the glass-ceramic production and indicate segregation of the CaTiO 3 phase for longer heat treatment times.
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