One-pot synthesis of iron oxide–carbon core–shell particles in supercritical water

Abstract

The quantitatively limited use of hydrogen peroxide in supercritical water allows for the in situ formation of iron oxides and graphitic carbon from ferrocene in one step. The structure of the particles prepared at 400–500 °C is comprised of nano- to micro-meter size of magnetite and maghemite cores covered with graphitic carbon shells. The morphology and size of the core–shell particles and the phase composition of iron-oxide cores are different dependent on the preparation conditions. The particles prepared at 400 °C contain, as dominant iron-oxide phase, the magnetite core particles ranging from nano- to micro-meter scales with no morphological regularity, while those prepared at 500 °C are comprised of hexagram shape and micro-meter size of maghemite cores. The observed morphology, the dimension of the core particles, and the dominant phase composition suggested that the iron-oxide cores would be formed through the oxidation of iron(II) to iron(III) and two different hydrolysis paths. Furthermore, the higher preparation temperature of 500 °C has shown a tendency to form smaller crystallite sizes of polycrystalline iron-oxide cores. The decrease of subcrystal sizes in the vicinity of superparamagnetic thresholds effects the reduction of coercivity in the ferromagnetic hysteresis.