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Polycrystalline niobium-doped molybdenum and tungsten diselenides were synthesized in silicatubes sealed under secondary vacuum. They were characterized by scanning electron microscopy, electrondiffraction, X-ray diffraction, chemical composition and EDX analyses. The morphology of niobium-dopedmolybdenum solid solutions was shown to depend strongly on the conditions of synthesis, whereas the structuralcharacterization did not.