Silica has sparked strong interest in hydrometallurgy, catalysis, the cement industry, and paper coating. The synthesis of silica particles was performed at 900 °C using the ultrasonic spray pyrolysis (USP) method. Ideally, spherical particles are obtained in one horizontal reactor from an aerosol. The controlled synthesis of submicron particles of silica was reached by changing the concentration of precursor solution. The experimentally obtained particles were compared with theoretically calculated values of silica particles. The characterization was performed using a scanning electron microscope (SEM) and energy-dispersive X-ray spectroscopy (EDS). X-ray diffraction, frequently abbreviated as XRD, was used to analyze the structure of obtained materials. The obtained silica by ultrasonic spray pyrolysis had an amorphous structure. In comparison to other methods such as sol–gel, acidic treatment, thermal decomposition, stirred bead milling, and high-pressure carbonation, the advantage of the ultrasonic spray method for preparation of nanosized silica controlled morphology is the simplicity of setting up individual process segments and changing their configuration, one-step continuous synthesis, and the possibility of synthesizing nanoparticles from various precursors.