摘要： The series of DyF3 nanoparticles was synthesized for the first time by a chloride-based route, using the water-soluble dysprosium chloride hexahydrate as a precursor. The synthesized nanoparticles have sizes of 3 to 7 nm, which is the smallest reported size for DyF3 nanoparticles. The influence of precursor concentration in an aqueous solution prior to the chemical reaction on the size of nanoparticles was studied. The influence of microwave-assisted hydrothermal treatment was also studied. The analysis of transmission electron microscopy (TEM) data revealed no correlation between the size of synthesized nanoparticles and the concentration of the aqueous solution. The AC/DC magnetic susceptibility of DyF3 nanoparticles was measured. The dipolar ferromagnetic transition for this sample was not observed down to 1.8 K that can be possibly explained by onset of superparamagnetism. The self-assembly of DyF3 nanoparticles was observed for the first time by analysis of XRD and TEM data and the evidence of superlattice formation along (020) and (210) lattice planes over the size of 20–30 nm (4–5 nanoparticles) was obtained.