chemicallytechFine Chemical TechnologiesТонкие химические технологии2410-65932686-7575MIREA – Russian Technological University (RTU MIREA).10.32362/2410-6593-2020-15-2-67-76chemicallytech-1598Research ArticleCHEMISTRY AND TECHNOLOGY OF INORGANIC MATERIALSХИМИЯ И ТЕХНОЛОГИЯ НЕОРГАНИЧЕСКИХ МАТЕРИАЛОВMolybdenum(VI) oxide: New methods of synthesis and propertiesОксид молибдена(VI): Hовые методы синтеза и свойстваhttps://orcid.org/0000-0003-3579-2194НикишинаЕ. Е.NikishinaE. E.

Никишина Елена Евгеньевна, доцент кафедры химии и технологии редких и рассеянных элементов, наноразмерных и композиционных материалов 

 Scopus Author ID 6602839662, ResearherID О-7115-2014

119571, Москва, пр-т Вернадского, д. 86

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

86, Vernadskogo pr., Moscow, 119571

helena_nick@mail.ruhttps://orcid.org/0000-0003-1532-8845ЛебедеваЕ. Н.LebedevaE. N.

Лебедева Елена Николаевна, инженер кафедры химии и технологии редких и рассеянных элементов, наноразмерных и композиционных материалов

Scopus Author ID 7102162057

119571, Москва, пр-т Вернадского, д. 86

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

86, Vernadskogo pr., Moscow, 119571

https://orcid.org/0000-0002-0379-2926ДроботД. В.DrobotD. V.

Дробот Дмитрий Васильевич, профессор кафедры химии и технологии редких и рассеянных элементов, наноразмерных и композиционных материалов

  Scopus Author ID 35580931100

119571, Москва, пр-т Вернадского, д. 86

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

86, Vernadskogo pr., Moscow, 119571

МИРЭА – Российский технологический университет (Институт тонких химических технологий имени М.В. Ломоносова)РоссияNanoscale and Composite Materials, M.V. Lomonosov Institute of Fine Chemical Technologies, MIREA – Russian Technological UniversityRussian Federation2020200520201526776Copyright © Nikishina E.E., Lebedeva E.N., Drobot D.V., 20202020Никишина Е.Е., Лебедева Е.Н., Дробот Д.В.Nikishina E.E., Lebedeva E.N., Drobot D.V.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.finechem-mirea.ru/jour/article/view/1598Objectives

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

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

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

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. 

Цели

Цели. Целью работы была разработка новых методов синтеза оксида молибдена(VI), являющегося предшественником для синтеза функциональных материалов на его основе, а также исследование физико-химических свойств полученных фаз.

Методы

Методы. Синтезированные фазы и продукты их термолиза изучали методами дифференциально-термического анализа, ИК-спектроскопии, рентгенофазового анализа, гранулометрии.

Результаты

Результаты. Разработаны три метода синтеза оксида молибдена(VI) и исследованы физико-химических свойства полученных оксидных фаз. Первый способ заключался во взаимодействии пентахлорида молибдена с раствором аммиака концентрацией 6.0–9.5 моль/л, второй – во взаимодействии пентахлорида ниобия с раствором серной кислоты, третий – во взаимодействии молибдата аммония с азотной кислотой. В первом случае образовался гидроксид молибдена(V) MoO(OH)3 бурого цвета, во втором случае наблюдалось образование осадка ярко-синего цвета – молибденовой сини MoO2.75, в третьем случае образовался гидратированный оксид MoO3·H2O белого цвета.

Выводы

Выводы. Дифференциально-термический и рентгенофазовый анализы показали, что во всех случаях образцы представляют собой аморфные фазы. Термическая обработка (Т = 580 ºС) синтезированных фаз приводит к образованию триоксида молибдена ромбической модификации. Для всех продуктов термолиза рассчитаны параметры решетки и рентгеновская плотность. Проведено исследование влияния термической обработки на размер частиц синтезированных образцов и продуктов их термолиза. Гранулометрический анализ показал, что в зависимости от способа получения триоксида молибдена, образуются частицы разного диаметра. Наименьший размер частиц (0.3–0.6 мкм) обнаружен у триоксида молибдена – продукта термолиза образца, полученного при взаимодействии пентахлорида молибдена с концентрированным раствором аммиака.

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The authors declare that there are no conflicts of interest present.