A New XRD Method to Quantitatively Distinguish Non-Stoichiometric Magnetite: Influence of Particle Size and Processing Conditions

Abstract

Magnetite’s abilities rely on the quantitative phases present in the sample. Magnetite quality can strongly influence several physical properties, such as magnetism, catalytic performance, and Verwey transition. However, differentiation of magnetite and maghemite through the conventional X-ray diffractogram comparison are not relevant for the intermediate phases. In this study, the deviation from the ideal stoichiometric magnetite and the relative quantification of both phases were mathematically achievable through a new XRD technique. Various synthesis conditions were applied to obtain different crystallite sizes, in the range of 9 to 30 nm. Generally, the stoichiometric deviation and maghemite content would be significantly influenced by the final size, whereas system conditions (temperature of solution, agitation rate, and pH of solution) would only have minor significance. In this study, iron oxide nanoparticles prepared using the co-precipitation method was calculated to contain 100% magnetite for particles of 30.26 nm in size, while 100% maghemite was calculated for particles at 9.64 nm.