In this study, strontium hexaferrite nanoparticles synthesized by sol–gel autocombustion method and the effect of high annealing temperature on produced nanoparticle have been studied. Powders were annealed at 1,000 and 1,300°C. Structural properties of synthesized powders were analyzed by X-ray diffraction (XRD). Hexagonal structure and shape of SrFe12O19 nanoparticles were analyzed from field-emission scanning electron microscope and transmission electron microscope figures. Fourier-transform infrared spectroscopy confirmed the formation of an M-type hexagonal structure. The thermal behavior of nanoparticles has been investigated by thermogravimetric analysis (TGA and DTG). Height measurement of nanoparticles with 2D and 3D images of the surface obtained from atomic force microscopy. XRD pattern of strontium hexaferrite nanoparticle was used for determining the crystal structure and examining the effect of high annealing temperature on powders by finding lattice parameters, densities, crystallite size, specific surface area, and strain. Crystallite size, strain, and bulk density decreased when produced nanoparticles annealed at 1,000°C with decreased porosity when nanoparticles were annealed at 1,300°C. The specific surface area was found to be increased when nanoparticles were annealed at 1,000°C. In this study, influence of high temperature on the structure of SrFe12O19 nanoparticles was studied.