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.

The present study prepared molybdenum trioxide (MoO3), the most important intermediate of molybdenum metal, by using a fluidized bed reactor for the thermal decomposition of ammonium molybdate (AM) in the presence of an air flow. During the process of fluidizing the sample inside the reactor, the reaction time and temperature were optimized with a close analysis of the X-ray diffraction (XRD) data and with thermogravimetric analysis (TGA). In particular, the temperature level, at which the AM decomposition is completed, is very important as a primary operating parameter. The analysis of the XRD and TGA data showed that the AM decomposition is almost completed at ~350 oC with a reaction time of 30 min. A shorter reaction time of 10 min. required a higher reaction temperature of ~500 oC with the same air flow rate to complete the AM decomposition. A sharp rise in the decomposition efficiency at a temperature ranging between 320 and 350 oC indicated a threshold for the AM decomposition. The operating conditions determined in this study can be used for future scale-ups of the process.

The effect of the preparation factors, such as the feeding mode and rate of raw materials, the reaction temperature and the surfactant on the size distribution of molybdenum trioxide particle were investigated by orthogonal test. The optimum conditions for the preparation of precursors are as following; opposite feeding fast, reaction temperature of and adding dispersant.