NiFe 2 O 4 nanoparticles stabilized by porous silica shells (NiFe 2 O 4 @SiO 2 ) were prepared using a onepot synthesis and characterized for their physical and chemical stability in severe environments, representative of those encountered in industrial catalytic reactors. The SiO 2 shell is porous, allowing transport of gases to and from the metal core. The shell also stabilizes NiFe 2 O 4 at the nanoparticle surface: NiFe 2 O 4 @SiO 2 annealed at temperatures through 973 K displays evidence of surface Ni, as verified by H 2 TPD analyses. At 1,173 K, hematite forms at the surface of the metallic cores of the NiFe 2 O 4 @SiO 2 nanoparticles and surface Ni is no longer observed. Without the silica shell, however, even mild reduction (at 773 K) can draw Fe to the surface and eliminate surface Ni sites.