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FePt/Fe3O4 nanoparticles can be used as building blocks to obtain, uponthermal annealing, magnetic nanocomposites with combined magnetic properties.Although the pre- and post-annealed samples are usually well characterized, adetailed investigation during annealing is necessary to reveal the role ofintermediate processes to produce a desirable composite. We present analternative method using in situ XANES to investigate the thermal evolution ofoleic acid and oleylamine coated Pt-rich FePt/Fe3O4 heterodimers. As thetemperature increases, a progressive reduction of Fe3O4 to FeO occurs helped bythe thermolysis of the surfactants; while above 550 K Fe3Pt starts to beformed. At 840 K an abrupt increase of FeO further drives the phasetransformation to stabilize the iron platinum soft phase. Thus, the Fe3O4reduction acts as catalyst that promotes the Fe and Pt interdiffusion betweenthe Pt-rich FePt and Fe3O4/FeO to form Fe3Pt instead of exchange coupledFePt/Fe3O4 with hard magnetic properties. In addition, the role of theinterface of the heterodimer ends is discussed. The pre- and post-annealedsamples were also characterized by TEM, XRD, EXAFS, magnetometry andM\"ossbauer spectroscopy.

Thermal evolution of Pt-rich FePt/Fe3O4 heterodimers studied using x-ray absorption near edge spectroscopy