| Abstract | Coupling electron microscopy techniques with insitu heating ability allows us to study phase transformations on the single-nanoparticle level. We exploit this setup to study disorder-to-order transformation of Pt-Fe alloy nanoparticles, a material that is of great interest to fuel-cell electrocatalysis and ultrahigh density information storage. In contrast to earlier reports, we show that Fe (instead of Pt) segregates towards the particle surface during annealing and forms a Fe-rich FeOx outer shell over the alloy core. By combining both exsitu and insitu approaches to probe the interplay between ordering and surface-segregation phenomena, we illustrate that the surface segregation of Fe precedes the ordering process and affects the ordered phase evolution dramatically. We show that the ordering initiates preferably at the pre-existent Fe-rich shell than the particle core. While the material-specific findings from this study open interesting perspectives towards a controlled phase evolution of Pt-Fe nanoalloys, the characterization methodologies described are general and should prove useful to probing a wide-range of nanomaterials. Surface-segregation vs atomic-ordering: By using atomic-resolution imaging and electron energy loss spectroscopy and employing both exsitu and insitu approaches, an ongoing interplay between segregation and ordering during the thermal annealing of Pt - Fe alloy nanoparticles is studied. Findings reveal a surface segregation of Fe that is in contrast to earlier reports suggesting Pt surface segregation. |
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