Partially oxidized fcc FePd and FePt nanoparticles with mean diameters of 5 and 3 nm, respectively, were synthesized by a reverse micelle polyol process. In situ measurements of magnetic and structural properties during annealing showed a large increase in the magnetocrystalline anisotropy and in the Curie temperature of the nanoparticles due to (i) a phase transition from A1 to L1(0) and (ii) a simultaneous phase separation between a metallic core and an iron oxide shell. These occurred at 675 K in the FePd nanoparticles and at above 850 K for the FePt. The Curie temperature of the nanoparticles was found to be about 850 K, an increase of more than 100 K from the bulk L10 phase. The ferromagnetic resonance results are discussed and compared with a phenomenological model that makes it possible to estimate the magnetocrystalline anisotropy as 1.6 X 10(5) and 1.5 X 10(6) J m(-3) in FePd and FePt, respectively. Exchange coupling between the core and the shell explains both the high magnetocrystalline anisotropy of the core and the high Curie temperature of the shell. (c) 2009 American Institute of Physics. [doi:10.1063/1.3233936]