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Oxyfluoride glass and glass‐ceramics are being studied due to the possibility of their utilization in many applications, such as thermoluminescent dosimeters, optical fibers, fluorescent concentrators, and temperature sensors. In order to improve the properties of glass, they are often crystallized. For this crystallization to be effective, knowledge and control of the structure of the starting material is required. Much work was done on silicate glass; however, a great interest exists in obtaining these kinds of materials in other matrices such as germanates, phosphates, and borates. Here, we present a structural study of some oxyfluoride borate glass with different concentrations of PbF2 by means of Nuclear Magnetic Resonance (NMR), Raman, and Fourier Transform Infrared (FTIR) spectroscopies. We also analyzed glass‐crystallization using Differential Scanning Calorimetry (DSC). The crystallization study was complemented with the use of Transmission Electron Microscopy (TEM) and Selected Area Electron Diffraction (SAED), for the purpose of identifying possible mechanisms of crystallization. Our results indicate, from the structural point of view, that the glass present groups with one or two BO4 species, such as diborate or pentaborate. The small variation in the BO4 fraction with the increase in PbF2 concentration would be an indication of the formation of F−BO3/2 species. Oxyfluoride borate glass containing BaO as a cation modifier and 30% PbF2 represents a good starting point for obtaining glass‐ceramics with a narrow size distribution of BaF2 nanocrystals. We also propose that the possible mechanism for oxyfluoride borate glass crystallization started with a separation of phases.

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A new lead strontium borate (B14O25Pb1.69Sr2.31) and lead barium borate (Pb5.33Ba10.67B44F4O80) have been prepared by crystallizing the corresponding glassy phases of the systems; SrO-B2O3-PbF2 and BaO-B2O3-PbF2 respectively. The glasses were prepared by the melting/quenching technique. The glass crystallization was studied by differential scanning calorimetry (DSC). We observed one exothermic event indicating that crystallization occurs in one steps. Glass samples were heat treated at temperature of crystallization determined by DSC. The crystal structure has been determined by powder X -ray diffraction. B14O25Pb1.69Sr231 (isostructural with B14O2Sr4 [1]) crystallizes in the Monoclinic space group C2/m with unit cell a = 16.4274 Å, b = 7.782215 Å, c=16.58075 Å and alfa = gamma and beta = 119.2482 º . Pb5.33Ba10.67B44F4O80 crystallizes in the Orthorhombic space group Cmc21 with unit cell a = 18.78672 Å, b = 10.69704 Å, c= 8.60674 Å and alfa=beta=gamma= 90 º (isostructural with Ba4B11O20F ) [2]. These crystals were doped with rare earth (Er3+ and Yb3+). As the dopants concentration increases the glass crystallization tendency diminish. The crystal structure determination was very important in the explaining of the difference luminescent properties of the corresponding glass ceramics materials.