Pyrrhotite nanoparticles with 5C and 3C superstructures were synthesized via a simple one-step thermal decomposition method in which hexadecylamine was used as a solvent at various reaction temperatures (TR). Structural analysis showed that at TR = 360 °C, almost uniform in size and shape Fe7S8 nanoparticles with 3C superstructure are formed, and an increase in the reaction temperature leads to the formation of Fe9S10 nanoparticles (5C superstructure), herewith a significant increase in the size of nanoparticles is observed. High-temperature magnetic measurements in 5 repeated heating-cooling cycles revealed that after the first heating branch in the Fe9S10 samples, the λ-Peak transition disappears, and the magnetization has a Weiss-type behavior characteristic of the Fe7S8 sample. The change in the behavior of magnetization can be explained by the redistribution of iron vacancies, which changes the initial phase composition of nanoparticles.
Keywords: Fe1-xS nanoparticles; magnetic properties; synthesis conditions; thermal decomposition; vacancy distribution.