In this study, manganese ferrite (MnFe2O4) nanoparticles were produced through flame spray pyrolysis (FSP). To investigate the effects of heat treatment, the nanoparticles were annealed between 400 and 650°C for 4 h in air in a comparative manner. The structural, chemical, morphological, and magnetic properties of the nanoparticles were evaluated using X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), dynamic light scattering (DLS), and vibrating sample magnetometry (VSM), respectively. The XRD results showed that the nanoparticles synthesized by the FSP method exhibited the MnFe2O4 spinel ferrite structure. The annealing process led to the decomposition of MnFe2O4 into various phases. According to the morphological analysis, the as‐synthesized particles were hemispherical–cubic in shape and had an average particle size of less than 100 nm. In addition, the chemical bond structures of the nanoparticles were confirmed in detail by XPS elemental analysis. The highest saturation magnetization was recorded as 33.50 emu/g for the as‐produced nanoparticles. The saturation magnetization of the nanoparticles decreased with increasing annealing temperature, while coercivity increased.