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In the work synthesized materials Pb1-xEuxF2+x (0.0001≤x≤0.2): nanopowders (by coprecipitation from aqueous solutions [2]) и micro-sized powders (by solid-phase synthesis at 450–500°C), their structural, optical and spectral-luminescent properties of were investigated. A solid solution (by coprecipitation) based on cubic (Fm3m) PbF2 was obtained from a solution with nominal Eu concentration x = 0.07 and more. The samples with a lower Eu concentration in the initial solution are two-phase and contain a solid solution based on cubic PbF2 and orthorhombic PbF2 (Pnma). The particles size of the cubic structure is 20-30 nm, the size of the orthorhombic particles is about 1 μm. GSs were made by heat-treatment based on lead fluoroborate glasses doped with Eu3+ (79PbF2–20B2O3–1EuF3). In a glass-ceramic the rare-earth ions were located in fluoride crystal nanoparticles distributed in a borate glass. The composition of the nanoparticles was determined as Pb0.88Eu0.12F2.12, a size of 40-50 nm.