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<p>In this communication we demonstrate the fast and facile preparation of nanoparticles hydrated and anhydrous iron trifluoride by solvotermal synthesis using the surface active substances. The iron fluoride/acytelen black composites were prepared by ultrasonic treatment. The analysis of the crystal microstructure and morphological properties of the material received.</p><p>Keywords: iron fluoride, nanoparticles, solvotermal synthesis, crystal structure, dehydration, Mössbauer spectroscopy.</p>