Controlled oxidation of iron nanoparticles in chemical vapour synthesis

In the present study, iron oxide nanoparticles (primary particle size of 80–90 nm) with controlled oxidation state were prepared via an atmospheric pressure chemical vapour synthesis (APCVS) method. Iron pentacarbonyl [Fe(CO)5], a precursor material, was thermally decomposed to iron in the APCVS reactor. Subsequently, the iron was oxidized with controlled amount of oxygen in the reactor to produce nearly pure magnetite or haematite particles depending on the oxygen concentration. Size, morphology and crystal structure of the synthesized nanoparticles were studied with scanning mobility particle sizer (SMPS), transmission electron microscopy (TEM) and X-ray diffraction (XRD). In addition, thermodynamic equilibrium calculations and computational fluid dynamics model were used to predict the oxidation state of the iron oxides and the reaction conditions during mixing. Aggregates of crystalline particles were formed, determined as magnetite at the oxygen volumetric fraction of 0.1 % and haematite at volumetric fraction of 0.5 %, according to the XRD. The geometric mean electrical mobility diameter of the aggregates increased from 110 to 155 nm when the volumetric fraction of oxygen increased from 0.1 to 0.5 %, determined using the SMPS. The aggregates were highly sintered based on TEM analyses. As a conclusion, APCVS method can be used to produce nearly pure crystalline magnetite or haematite nanoparticles with controlled oxidation in a continuous one-stage gas-phase process.