Unraveling the Effect of Annealing on the Structural and Microstructural Evolution of NiFe2O4@SiO2 Core-Shell Type Nanocomposites

The comparison between as-received and multistage annealed NiFe2O4@SiO2 (NFO@SiO2) core-shell nanoparticles is presented. The studied ferrites were synthesized by co-precipitation followed by microemulsion. The presence of cubic inverse spinel ferrite structure with tetrahedral and octahedral iron occupancy is confirmed in all analyzed samples. The structural characterization revealed the gradual crystallization of NFO cores up to about 12 nm crystallite size at the last annealing stage. Simultaneously, a partial crystallization of the silica matrix is evidenced. The superparamagnetic (SPM) behaviour is demonstrated based on complex magnetic performance and confirmed by Mossbauer spectrometry. The spin-canting phenomenon on the surface dead magnetic layer (MDL) is revealed based on the Yafet-Kittel model. A slight change in MDL thickness versus heat treatment is proved. The X-ray photoemission and absorption studies confirmed the complex nature of the Febased states. The Si-O-Ni/Fe intermixing on the NFO - SiO2 nanoparticles interface is revealed by the corelevel lines analysis, proving the existence of a disordered layer on the NFO surface.