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It is known that when studying the catalyzed crystallization of glasses by various methods, there is a large effect of heat treatment in the pre-crystallization period on the subsequent crystallization and properties of the final materials. However, systematic studies of the effect of the heat treatment regime on the kinetics of phase separation and the properties of nanostructured glasses are lacking. In this work, the pretreatment conditions of Ni2+-doped glasses of the Li2O-Na2O-Ga2O3-SiO2-GeO2 system, under which the rate of nucleation is maximized,are revealed. The decrease in the size of nanocrystals and the growth of their number result in lower concentration of Ni2+ per nanocrystal and lead to a significant increase of the luminescence efficiency in the nearIR region of studied nanostructured glasses.