Recently, magnetite nanoparticles have attracted much attention, due to their technological potential based on different optic, magnetic and catalytic sections. In particular, the magnetic properties of hybrid nanocrystals can be tailored by the combination of complementary magnetic materials like for example magnetite and FePt. In order to analyse the related magnetic and structural properties of the resulting bi-component systems, we present x-ray absorption and x-ray magnetic circular dichroism studies at the Fe L2,3 edges simultaneously performed in total electron yield and transmission mode, done at room and low temperatures. This provides in particular the separation of volume- and surface-related properties. The investigated system was made up of FePt/FeOx hybrid nanocrystals, which could be uniquely tuned in size and volume ratios. These measurements have been combined with magnetometry and high-resolution transmission electron microscopy studies. The separation between surface and bulk has been done by a deconvolution of the absorption spectra in terms of a linear superposition of reference spectra. With this universally applicable technique we are able to experimentally determine that the outer FeOx shell fraction at the surface has a strongly reduced magnetization and is of maghemite character, while the inner part is more magnetite like. So the technique shown here can be used to characterize nanoparticular systems and determine their structural and magnetic properties
