Structural, surface and magnetic properties of chalcogenide Co9S8 nanoparticles prepared by mechanochemical synthesis

In this study, the mechanochemical synthesis of Co9S8 nanoparticles from cobalt and sulphur by high-energy milling in a planetary mill in an argon atmosphere is reported. Structural characterization of the synthesized nanoparticles by XRD was performed. Co9S8 nanoparticles crystallize in the cubic structure with the crystallite size of about 16 nm. The microstructure of the Co9S8 nanoparticles was further studied using TEM, HRTEM and EDS-HAADF-STEM techniques. Co9S8 nanoparticles consist of nanocrystals exhibiting size in the range of 10–30 nm that are densely aggregated into spherical-like objects. The highest specific surface area value observed was 4 m2g-1 and the pore properties of this sample are quite poor. The magnetic properties of mechanochemically synthesized nanoparticles were investigated using SQUID magnetometer. The room temperature magnetic data supported the paramagnetic spin structure of Co9S8 nanoparticles. The transition from paramagnetic to weak ferromagnetic or ferrimagnetic behaviour was indicated from temperature dependence of magnetization at cryogenic temperatures. It is demonstrated that mechanochemical synthesis can be successfully employed in the one-step solid-state preparation of Co9S8 nanoparticles.