Intensification of sol-gel synthesis of Mn-containing MgO-Al₂O₃-ZrO₂-SiO₂ system materials

Glass and glass-crystalline MgO-Al₂O₃-SiO₂ system materials have many practical applications including their use as luminophores. To lower the synthesis temperature of such materials is an actual task. In this work, Mn-containing materials of MgO-Al₂O₃-ZrO₂-SiO₂ system were synthesized by sol-gel method. The analytical chemical composition, crystal structure, morphology and luminescence spectra were investigated by X-ray phase analysis, scanning electron microscopy, energy dispersive analysis and luminescence spectroscopy. It was found that the introduction of fluoride component into sols significantly accelerates the crystallization of Mn-containing gels during their heat treatment and has a significant effect on the morphology of xerogels. Fluorides play the role of additional nucleation centers and ensure the formation of numerous small oxide crystals. Energy dispersive analysis showed that fluoride is completely removed from the structure of materials during heat treatment of gels up to 900 °C. According to the data of X-ray phase analysis, the introduction of manganese ions into the structure of forming oxide crystals and deformation of their crystal lattice occurs at the initial stages of the crystallization process. Emission bands of both manganese ions and structural defects formed in the crystal lattice of oxide crystals are observed in the photoluminescence spectra of xerogels. It was shown that in addition to using the sol-gel method, which is a well-known approach, the addition of fluorine-containing precursor significantly accelerates crystallization of gels of MgO-Al₂O₃-ZrO₂-SiO₂ system, promotes formation of dispersed structure of materials, increases intensity, and improves resolution of emission bands in luminescence spectra.

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