The critical radius of particles of a new phase nucleated in a solution depends on the supersaturation and temperature of the solution. When the tempera ture varies in the process of nucleation, new factors that make it possible to control the growth of the new phase, as well as to obtain new data for developing the nucleation theory, can appear. In our preceding work [1], we revealed the effect of solution of nuclei of the CuCl phase in glass upon a sharp increase in the tem perature in the nucleation process and determined the critical radius of CuCl particles at temperatures from 500 to 650°C.In this work, the nucleation process is studied in a stepwise cooled solid solution. This makes it possible to create two distributions of CuCl nanoparticles with significantly different mean radii in glass. First, at a high temperature (700°C), the distribution with a mean radius of 14-18 nm is created. Then, the nucle ation temperature is stepwise decreased by 200 K; as a result, the critical nucleation radius decreases, and the formation of the second distribution with a mean radius of 1-3 nm becomes possible.As in [1], we study a solid solution of copper halo genide in a glass matrix. Samples 1and 2 with the ini tial distribution D1 of CuCl nanoparticles were pre pared at temperature T 1 = 700°C in 20 and 40 min, respectively. The fundamental absorption spectra of CuCl nanocrystals in samples 1 and 2 were measured at 80 K. Then, the second annealing was performed at temperature T 2 = 500°C, during which samples were periodically extracted from a furnace and their absorp tion spectrum was measured at 80 K.Lines 1 in Fig. 1 are the absorption spectra of sam ples (a) 1 and (b) 2 after the first annealing at 700°C. Lines 1 pronouncedly exhibit exciton absorption bands Z 1, 2 and Z 3 associated with CuCl nanocrystals [2] from distribution D1. The mean radii of CuCl nanocrystals in samples 1 and 2 were determined from the energy of Z 1, 2 excitons and the size quantization relation [3,4]. The size quantization parameter for CuCl nanocrystals larger than 10 nm was obtained from the data taken from [4]. The distributions D1 with the mean radii R 1 = 14 and 18 nm of CuCl parti cles are formed in 20 and 40 min in samples 1 and 2, respectively, annealed at 700°C. According to Fig. 1a, during the second annealing (at T 2 = 500°C), additional absorption bands appear and grow on the right of the absorption bands of Z 1, 2 and Z 3 excitons of CuCl nanocrystals from the distri bution D1 (lines 2-5). With an increase in the anneal ing time, the maxima of these additional bands are shifted toward lower energies. These changes in the absorption spectrum of sample 1 certainly indicate the appearance of the second distribution D2 of CuCl nanocrystals with the corresponding absorption bands of Z 1, 2 and Z 3 excitons (marked by arrows in Fig. 1a). The blue shift of these absorption bands with respect to similar absorption bands of CuCl particles in the dis tribution D1 indicates that the radius of CuCl particles in the distribution D2 is s...