The R-Fe nanoparticle was successfully synthesized by a solventless thermal decomposition method. The metal 2+ -oleate 2 complex prepared with metal salts and surfactant in aqueous solution was transformed to metal oxide. The metal oxide nanoparticle synthesized from the metal 2+ -oleate 2 complex was mixed with salt powder as a separating media. The metal oxide mixture was reduced to R-Fe nanoparticles by Ar + 4% H 2 mixture gas, and then it was annealed under a high-vacuum system of 1.8 × 10 -5 Torr at 700 °C. The NaCl powder that was used instead of a surfactant plays an important role to keep the size and shape of the nanoparticles. The magnetization value of the prepared R-Fe nanoparticles is 213 emu/g, and the mean particle size of the R-Fe nanoparticles is 35 nm.