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Molybdenum(VI) oxide: New methods of synthesis and properties

https://doi.org/10.32362/2410-6593-2020-15-2-67-76

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Abstract

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. 

About the Authors

E. E. Nikishina
Nanoscale and Composite Materials, M.V. Lomonosov Institute of Fine Chemical Technologies, MIREA – Russian Technological University
Russian Federation

Elena E. Nikishina, Assistant Professor, Department of Chemistry and Technology Rare and Dispersed Elements

86, Vernadskogo pr., Moscow, 119571



E. N. Lebedeva
Nanoscale and Composite Materials, M.V. Lomonosov Institute of Fine Chemical Technologies, MIREA – Russian Technological University
Russian Federation

Elena N. Lebedeva, Engineer, Department of Chemistry and Technology Rare and Dispersed Elements

86, Vernadskogo pr., Moscow, 119571



D. V. Drobot
Nanoscale and Composite Materials, M.V. Lomonosov Institute of Fine Chemical Technologies, MIREA – Russian Technological University
Russian Federation

Dmitry V. Drobot, Professor, Department of Chemistry and Technology Rare and Dispersed Elements

86, Vernadskogo pr., Moscow, 119571



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Supplementary files

1. Structures of polymorph modifications of molybdenum trioxide: a) α-MoO3, b) β-MoO3, c) h-MoO3. In all structures, a unit cell is shown as a thin black line, oxygen atoms are indicated by black spheres, molybdenum atoms are located inside the gray MoO6 octahedra.
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2. This is to certify that the paper titled Molybdenum(VI) oxide: New methods of synthesis and properties commissioned to Enago by Elena E. Nikishina, Elena N. Lebedeva, Dmitry V. Drobot has been edited for English language and spelling by Enago, an editing brand of Crimson Interactive Inc.
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Three methods for the synthesis of molybdenum(VI) oxide were developed, and the physicochemical properties of the obtained oxide phases were evaluated. A series of thermal and X-ray diffraction analyses demonstrated that in all cases, the samples were amorphous phases. Heat treatment of the synthesized phases at 580°C led to the formation of a rhombic modification of molybdenum trioxide. The lattice parameters and X-ray density were calculated for all thermolysis products. Moreover, the effect of heat treatment on the particle size of the synthesized samples and their thermolysis products was investigated.

For citation:


Nikishina E.E., Lebedeva E.N., Drobot D.V. Molybdenum(VI) oxide: New methods of synthesis and properties. Fine Chemical Technologies. 2020;15(2):67-76. https://doi.org/10.32362/2410-6593-2020-15-2-67-76

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ISSN 2410-6593 (Print)
ISSN 2686-7575 (Online)