Nanostructure and compositional segregation of soft magnetic FeNi‐based nanocomposites with multiple nanocrystalline phases

Soft magnetic metal amorphous nanocomposite alloys are produced through rapid solidification and thermal annealing yielding nanocrystals embedded within an amorphous precursor. Similar free energies in Co‐rich and FeNi‐based alloy systems result in multiple nanocrystalline phases being formed during devitrification. Studies of multi‐phase crystallization processes have been reported for Co‐rich alloys but relatively few have investigated FeNi‐based systems. A detailed characterization of compositional partitioning and microstructure of an optimally annealed FeNi‐based MANC (Fe 70 Ni 30 ) 80 Nb 4 Si 2 B 14 alloy is presented through complementary high‐resolution transmission electron microscopy (HRTEM) and atom probe tomography (APT). HRTEM demonstrates orientation relationships between FCC and BCC nanocrystals, suggesting heterogeneous nucleation of nanocrystals in the amorphous matrix or a cooperative mechanism of nucleation between BCC and FCC nanocrystallites. APT results show evidence for (i) the segregation of Fe and Ni between nanocrystals of different phases, (ii) B partitioning to the amorphous phase, and (iii) an Nb‐enriched shell surrounding nanocrystals.