Objectives. The present study aims to develop new methods for the synthesis of molybdenum(VI) oxide, which is a precursor for the synthesis of functional materials, as well as to investigate the physicochemical properties of the resulting oxide phases. Methods. The synthesized phases and the products of their thermolysis were studied by differential thermal analysis, IR spectroscopy, X-ray diffraction analysis, and granulometry. Results. Three methods for the synthesis of molybdenum(VI) oxide were developed, and the physicochemical properties of the oxide phases obtained were studied. The first method consisted in the reaction of molybdenum pentachloride with a 6.0–9.5 mol/L ammonia solution, the second one was the reaction of niobium pentachloride with a sulfuric acid solution, and the third method involved the reaction of ammonium molybdate with nitric acid, affording brown molybdenum(V) MoO(OH)3 hydroxide, a bright blue precipitate of molybdenum blue MoO2.75, and white hydrated oxide MoO3·H2O, respectively. Conclusions. A series of thermal and X-ray diffraction analysis demonstrated that in all cases the samples were amorphous phases. Heat treatment at 580 °C of the synthesized phases led to the formation of a rhombic modification of molybdenum trioxide. The lattice parameters and X-ray density were calculated for all thermolysis products. The effect of heat treatment on the particle size of the synthesized samples and their thermolysis products was studied. Particle size analysis demonstrated that particles of different diameters were formed depending on the synthetic method. The smallest particle size (0.3–0.6 µm) was found in molybdenum trioxide, a product of the thermolysis of the sample obtained by the reaction of molybdenum pentachloride with a concentrated ammonium solution.
Investigation of Changes in the Fine Structure of Graphitizing Carbon Materials during Heat Treatment by X-Ray Diffraction Analysis
