Hexagonal Co₉S₈ nanocrystal and nanorods were synthesized using cobalt chloride (CoCl₂.6H₂O), dimethyl sulfoxide (DMSO) and non-aqueous alcohol as the starting materials, and taking dimethyl sulfoxide as both sulfur source and strong infiltrator in nanorods preparation. The Co₉S₈ samples were characterized by X-ray diffraction (XRD), scanning tunneling microscope (SEM), transmission electron microscope (TEM), vibrating sample magnetometer (VSM) and laser Raman spectrometer. The results show that the as-prepared Co₉S₈ nanocrystal with a size of 6 nm take on weak paramagnetism at room temperature. The lengths and diameters of the nanorods were about 4 𝜇m and 200 nm, respectively. The reason for the relative lower synthesis temperature of nanorods was discussed and a ‘micro-autoclave reactor’ model was suggested as well.

Three-dimensional (3D) flower-like cubic Ni3S4 nanoplates with single crystalline nature were successfully prepared through decomposing bis(thiourea) nickel(II) chloride crystals (BTNC). The samples were characterized by X-ray diffraction, scanning electron microscope, transmission electron microscope, selected area electron diffraction and Raman spectroscopy. Results show that the as-prepared products are pure cubic Ni₃S₄ and stable in range of 180–220°C with single crystal nature providing high surface areas, and higher reaction temperature leads to lower surface areas. Typical Raman peaks of the as-synthesized 3D flower-like cubic Ni₃S₄ at 200°C are located at 239, 286, 337, 379, 423, 478 and 630 cm^-1. Magnetization measurement indicates that single crystalline Ni₃S₄ nanoplates prepared at 200°C displays antiferromagnetic behaviour.