Priyansh N. Brahmbhatt, Mehul S. Dave, Shivani R. Bharucha, Sunil H. Chaki
Abstract This study investigates the structural and microstructural characteristics of magnetite (Fe 3 O 4 ) and cobalt ferrite (CoFe 2 O 4 ) nanoparticles synthesized via the sol–gel auto-combustion method using ferric nitrate and cobalt nitrate as metal precursors. X-ray diffraction (XRD) analysis confirmed the formation of single-phase crystalline nanoparticles with a cubic inverse spinel structure. Transmission electron microscopy further validated the nanocrystalline nature and morphological uniformity of the particles. To gain deeper insight into the crystallite size and lattice strain, multiple XRD-based analytical approaches Williamson–Hall, size-strain plot, and Halder–Wagner methods were employed. The novelty of this work lies in the first systematic side-by-side comparison of Fe 3 O 4 and CoFe 2 O 4 nanoparticles synthesized under identical conditions and evaluated using four complementary XRD models, ensuring cross-validated accuracy. The comparative evaluation of these models revealed slight discrepancies in size estimations, attributed to their varied assumptions regarding strain and instrumental broadening. Notably, CoFe 2 O 4 nanoparticles exhibited marginally larger crystallite sizes and higher lattice strain compared to Fe 3 O 4 , imply compositional influence on structural properties. The combined application of these analytical techniques enabled accurate estimation of crystallite size, microstrain, and energy density, providing insights into the mechanical stability and potential functional behavior of the synthesized nanoparticles.