Transparent oxyfluoride glass-ceramics obtained by the adequate heat treatment of Nd3+-doped glass with composition 70SiO2–7Al2O3–16K2O–7LaF3 (mol%) are investigated. Site-selective laser spectroscopy demonstrates that depending on the Nd3+ concentration, cubic (α-phase) and hexagonal (β-phase) KLaF4 nanocrystals precipitate from the starting glass. The presence of both crystalline phases are unambiguously identified from the emission and excitation spectra and lifetime measurements of the 4F3/2 state of Nd3+ ions. The spectroscopic results are in agreement with those obtained with XRD and HR-TEM techniques: α-KLaF4 nanocrystals are found to be present for all NdF3 concentrations whereas β-KLaF4 nanocrystals are predominant in the GC samples doped with 0.5 mol%.
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