Influence of Temperature on the Structural Evolution of Iron–Manganese Oxide Nanoparticles in the Hydrothermal Method

This study is focused on the hydrothermal synthesis of iron–manganese oxide nanostructures, focusing on the influence of Fe:Mn precursor ratios, temperature, and reaction time on phase formation, morphology, and structural characteristics. Three molar ratios (Fe:Mn = 2:1, 1:1, and 1:2) were explored under variable conditions (80 °C, 120 °C, and 200 °C; 4, 12, and 24 h). X-ray diffraction (XRD) analysis revealed distinct phase selectivity depending on precursor composition: FeMn2O4 was obtained with 1:2 ratio, Fe3Mn3O8 with 1:1, and Fe2MnO4 with 2:1, each without phase mixing. Scanning electron microscopy (FESEM) showed a pronounced effect of temperature and time on nanoparticle morphology, ranging from compact agglomerates to well-defined rod-like structures at 200 °C/24 h. Dynamic light scattering (DLS) indicated narrow size distributions for samples synthesized at 120 °C/12 h, with hydrodynamic diameters between 20 and 50 nm. Raman spectroscopy confirmed the presence of characteristic vibrational modes of spinel-type structures and validated structural integrity. High-resolution transmission electron microscopy (HRTEM) evidenced well-ordered lattice fringes with interplanar spacings of ~0.48–0.52 nm, consistent with spinel phases and indicative of high crystallinity. These findings demonstrate that controlled atomic binding and thermal parameters enable selective synthesis of pure iron–manganese oxide phases with tailored morphologies, offering a scalable route for designing advanced functional materials in catalysis, energy, and biomedical applications.