Low-dimensional iron chalcogenide Fe
7S
8 and FeSe
2 microcrystals and FeTe
2 bulk singlecrystals were synthesized via the reactions of FeCl
3 with S or Se or Te powders in hydrazinehydrate solution (85%, v/v) at 140
C for 36 h. The products were characterized by means ofX-ray powder diffraction,
rocking curve, transmission electron microscopy, electron diffraction, and scanning electron microscopy techniques. In the reaction process, hydrazine hydratecan coreduce Fe
3+ and elemental chalcogen to Fe
2+ and chalcogen anions, respectively, thecombination of which can lead to the reaction proceeding completely. The morphologies ofthe products are affected by the temperature, pressure, and pH values. Moreover, a suitablespeed of decreasing the temperature and proper supersaturation are two important factorsin the formation of single-crystal FeTe
2. Mössbauer spectra show the
magnetism of Fe
7S
8and nonmagnetic properties for FeSe
2 and FeTe
2 at room temperature.