Molybdenum trioxide (MoO₃) is used in various applications including sensors, photocatalysts, and batteries owing to its excellent ionic conductivity and thermal properties. It can also be used as a precursor in the hydrogen reduction process to obtain molybdenum metals. Control of the parameters governing the MoO₃ synthesis process is extremely important because the size and shape of MoO₃ in the reduction process affect the shape, size, and crystallization of Mo metal. In this study, we fabricated MoO₃ nanoparticles using a solution combustion synthesis (SCS) method that utilizes an organic additive, thereby controlling their morphology. The nucleation behavior and particle morphology were confirmed using ultraviolet-visible spectroscopy (UV-vis) and field emission scanning electron microscopy (FE-SEM). The concentration of the precursor (ammonium heptamolybdate tetrahydrate) was adjusted to be 0.1, 0.2, and 0.4 M. Depending on this concentration, different nucleation rates were obtained, thereby resulting in different particle morphologies.