This study investigated the use of ethylene glycol to form α-MoO3
(molybdenum trioxide) from ammonium molybdate tetrahydrate at various sintering temperatures for 1 h. During the sintering process, the morphologies of the constituents were observed using scanning electron microscopy (SEM), and Fourier transform infrared (FTIR) spectroscopy was used to explain the reaction process. In this work, the results obtained using X-ray photoelectron spectroscopy (XRD) demonstrated that, when the molybdenum trioxide powder was treated thermally at 300 °C, the material exhibited crystallinity. The peaks were indexed to correspond with the (110), (040), (021), (111), and (060) crystallographic planes, and the lattice parameters of a, b, and c were about 3.961, 13.876, and 3.969 Å. Using these observations, we confirmed that orthorhombic α-MoO3
was formed for sintering temperatures from 300 to 700 °C. Pattern images were obtained by the selected area electron diffraction pattern (SAED) technique, and the d distance of the high resolution transmission electron microscopy (HRTEM) images were almost 0.39 and 0.36 nm, and the Mo 3d5/2
, Mo 3d3/2
, and O 1s of X-ray photoelectron spectroscopy (XPS) were located at 233.76, 237.03, and 532.19 eV, which also demonstrated that α-MoO3
powder had been synthesized.