A phase transition, from orthorhombic Fe3C to hexagonal Fe7C3, was observed using a wet synthesis mediated by hexadecyltrimethylammonium chloride (CTAC). In this study, CTAC has been shown to control carbide phase, morphology, and size of the iron carbide nanostructures. Fe7C3 hexagonal prisms were formed with an average diameter of 960 nm, the thickness of 150 nm, and Fe3C nanostructures with an approximate size of 50 nm. Magnetic studies show ferromagnetic behavior with Ms of 126 emu/g, and Hc of 170 Oe with respect to Fe7C3 and 95 emu/g and 590 Oe with respect to Fe3C. The thermal studies using high temperature x-ray diffraction show stability of Fe7C3 up to 500 °C. Upon slow cooling, the Fe7C3 phase is recovered with an intermediate oxide phase occurring around 300 °C. This study has demonstrated a simple route in synthesizing iron carbides for an in depth magnetic study and crystal phase transition study of Fe7C3 at elevated temperatures.