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Diplomsko delo prikazuje študijo sintetiziranja sulfidov prehodnih kovin 4. periode (MxSy M = Zn, Ni, Co) s pomočjo mehanokemijske metode. Pri tem smo uporabljali visokoenergijski kroglični mlin SPEX 8000M. Vzorce, dobljene z mletjem, smo analizirali s pomočjo rentgenske praškovne difrakcije (XRD), za segrevanje nekaterih produktov pa smo uporabili napravo za termogravimetrično analizo (TGA). Namen te študije je bil spoznavanje mehanokemijskih metod, rentgenske praškovne difrakcije in aparata za termogravimetrično analizo. To diplomsko delo opisuje rezultate vseh izvedenih sintez in metode s katerimi smo prišli do teh rezultatov. Ugotovili smo, da je uporaba mehanokemjskih metod za sintezo sulfidov prehodnih kovin 4. periode lahko učinkovita. This diploma thesis studies the synthesis of sulfides with transition metals from 4. period (MxSy M = Zn, Ni, Co) by using the mechanochemical method. We used a high energy ball mill SPEX 8000M. Samples, obtained by milling, were analyzed using X-ray powder diffraction (XRD), for heating of some products we used a device for thermogravimetric analysis (TGA). The purpose of this study was to get familiar with mechanochemical methods, X-ray powder diffraction and the machine for thermogravimetric analysis. This thesis describes the results of performed syntheses and methods that got us to those results. We found that mechanochemical synthesis of sulfides with transition metals from 4. period can be effective.