alternativeАльтернативная энергетика и экология (ISJAEE)Alternative Energy and Ecology (ISJAEE)1608-8298Международный издательский дом научной периодики "Спейс10.15518/isjaee.2017.25-27.071-087alternative-1185Research ArticleКАТАЛИЗ В АЭЭCATALYSIS FOR AEEЭНЕРГОЭФФЕКТИВНЫЙ СПОСОБ ПОЛУЧЕНИЯ LaCrO3 ИЗ ГЛИЦИН-НИТРАТНОГО ПРЕДШЕСТВЕННИКАENERGY-EFFICIENT METHOD OF LaCrO3 PREPARATION FROM GLYCINE-NITRATE PRECURSORСимагинаВ. И.SimaginaV. I.

д-р хим. наук, главный научный сотрудник, заведующая лабораторией исследования гидридных соединений

D.Sc. (chemistry), Professor, Chief Researcher, Head of Laboratory of Hydrides Investigation

simagina@catalysis.ruКомоваО. В.KomovaO. V.

канд. хим. наук, научный сотрудник лаборатории исследования гидридных соединений

Ph.D. (chemistry), Scientific Researcher at Laboratory of Hydrides Investigation

simagina@catalysis.ruНецкинаО. В.NetskinaO. V.

канд. хим. наук, старший научный сотрудник лаборатории исследования гидридных соединений

Ph.D. (chemistry), Senior Researcher at Laboratory of Hydrides Investigation

simagina@catalysis.ruОдеговаГ. В.OdegovaG. V.

канд. физ.-мат. наук, научный сотрудник лаборатории спектральных методов

Ph.D. (physics and mathematics), Scientific Researcher at Laboratory of Spectral Methods

simagina@catalysis.ruБулавченкоО. А.BulavchenkoO. A.

канд. хим. наук, научный сотрудник лаборатории структурных методов исследования

Ph.D. (chemistry), Scientific Researcher at Laboratory of Structural Methods

simagina@catalysis.ruИщенкоА. В.IshchenkoA. V.

канд. хим. наук, инженер лаборатории структурных методов исследования

Ph.D. (chemistry), Engineer at Laboratory of Structural Research Methods

simagina@catalysis.ruИнститут катализа им. Г.К. Борескова СО РАНРоссияBoreskov Institute of CatalysisRussian Federation201710122017025-277187Copyright © Международный издательский дом научной периодики "Спейс, 20172017Международный издательский дом научной периодики "СпейсМеждународный издательский дом научной периодики "Спейсhttps://www.isjaee.com/jour/about/submissions#copyrightNoticehttps://www.isjaee.com/jour/article/view/1185

Работа посвящена разработке методов синтеза нанодисперсных материалов. Предложен новый энергоэффективный подход к синтезу нанодисперсного LaCrO3 (размер кристаллитов 350 Å, удельная поверхность 27 м2 /г) методом горения в одну стадию без дополнительной стадии высокотемпературного прокаливания с низким содержанием примесей. Этот подход заключается в получении твердофазных глицин-нитратных предшественников, их прессовании и последующем разложении в режиме послойного горения. На основе данных элементного анализа и инфракрасной спектроскопии установлены основные типы взаимодействия компонентов в составе Cr- и LaCr-содержащих предшественников в зависимости от способа их получения. Впервые изучено влияние добавления водного раствора аммиака в состав предшественников и представлены результаты данного исследования, которые позволили проинтерпретировать данные их термического анализа. Полученные продукты горения анализировали рядом физико-химических методов: рентгенофазовый анализ, инфракрасная спектроскопия нарушенного полного внутреннего отражения, просвечивающая электронная микроскопия высокого разрешения, термический анализ, измерение удельной поверхности. Установлено, что состав предшественника, режим и скорость горения определяют дисперсность и чистоту формирующейся оксидной фазы. В режиме послойного горения продукт формируется при более высокой температуре, что обеспечивает высокий выход хорошо окристаллизованной фазы перовскита по сравнению с режимом объемного горения. Показано негативное влияние введения раствора аммиака в состав Cr-предшественника на фазовый состав продукта горения, которое приводит к формированию соединений с более высокой температурой начала термолиза. Полученные результаты могут быть использованы при синтезе материалов твердооксидных топливных элементов, нового поколения фотокатализаторов и фотоэлектродов для получения водорода под видимым светом, мембран, а также катализаторов широкого ряда процессов.

 

The work deals with the development of methods for the synthesis of nanosized materials and proposes a novel approach to the synthesis of nano-dispersed LaCrO3 (crystallite size 350 Å, specific surface area 27 m2 /g) with a small content of impurities by one-step combustion without the stage of high-temperature calcinations. The method involves preparation of solid-state glycine-nitrate precursor, its pelletization and subsequent decomposition during self-propagating high-temperature synthesis. Based on the results of elemental analysis and infrared spectroscopy, the main types of the components’ interactions in Cr- and LaCr-containing precursors have been established depending on the method of their preparation. For the first time, the results of the influence of the addition of ammonia water solution to the composition of the precursors have been presented. These results have allowed for an interpretation of their thermal analysis data. The obtained products of the combustion have been analyzed by a series of physicochemical methods: X-ray diffraction, attenuated total reflection infrared spectroscopy, high-resolution transmission electron spectroscopy, thermal analysis, measurements of the specific surface area. It is established that the precursors composition, the conditions and rate of combustion determine the dispersion and purity of the forming oxide phase. Under the conditions of the self-propagating high-temperature synthesis the product forms at a higher temperature which ensures a high yield of a well-crystallized phase of the perovskite as compared with the volume combustion synthesis. It has been demonstrated a negative influence of the addition of an ammonia solution to the Cr-containing precursors on the phase composition of the combustion product which leads to formation of compounds with a higher onset temperature of their thermolysis. The obtained results may be useful in the synthesis of materials for solid-oxide fuel cells, a new generation of photocatalysts and photoelectrodes for the production of hydrogen under visible light, of membranes and of catalysts for a wide range of various processes.

 

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