Evolution of the precursor structure during the preparation of the nanopowders with perovskite-type LnLn’O3 (Ln, Ln’ = REE) complex oxide phase in the La2O3-Lu2O3-Yb2O3 system

The thermal decomposition of complex oxide phases, such as perovskite, in the La2O3-Lu2O3-Yb2O3 systemwith a specific surface area of 37 m2/g, synthesised by the heterogeneous precipitation method under non-isothermal conditions of linear heating at a rate of 5 deg/min, was studied to reveal the fea...

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Main Authors: Oleksandr V. Shyrokov, Tatiana F. Lobunets, Olga V. Chudinovych, Tamara V. Tomila, Andrey V. Ragulya
Format: Article
Language:English
Published: Taylor & Francis Group 2024-12-01
Series:Journal of Experimental Nanoscience
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Online Access:https://www.tandfonline.com/doi/10.1080/17458080.2024.2366269
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author Oleksandr V. Shyrokov
Tatiana F. Lobunets
Olga V. Chudinovych
Tamara V. Tomila
Andrey V. Ragulya
author_facet Oleksandr V. Shyrokov
Tatiana F. Lobunets
Olga V. Chudinovych
Tamara V. Tomila
Andrey V. Ragulya
author_sort Oleksandr V. Shyrokov
collection DOAJ
description The thermal decomposition of complex oxide phases, such as perovskite, in the La2O3-Lu2O3-Yb2O3 systemwith a specific surface area of 37 m2/g, synthesised by the heterogeneous precipitation method under non-isothermal conditions of linear heating at a rate of 5 deg/min, was studied to reveal the features of structure changes in intermediate products. Thermogravimetric and adsorption-structural analyses, infrared spectroscopy, powder diffraction and electron microscopy revealed that the decomposition of precursors occurs in two main stages. Up to 700 °C, the initial coordination spheres are destroyed in a sequential manner, resulting in the powders remaining amorphous in phase composition. However, with a gradual increase in the order of the atoms, the change in the pore structure is non-monotonic, with an inflection point observed at 450 and 675 °C. At 675 °C, the system undergoes a collapse, accompanied with decrease in both the pore volume (V∑) and the specific surface area (SBET), which attain the lowest values of 0.0415 cm3/g and 16.5 m2/g, respectively. The second stage of decomposition of the precursor in the temperature range of 750-825 °C is associated with the formation and accumulation of the crystalline phase of perovskite in the form of a nanodispersed mesoporous powder with a specific surface area of 18 m2/g and the average mesopore diameter of 17 nm corresponding to a particle size of 40 nm when using the calculated X-ray density of 8.26 g/cm3.
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spelling doaj-art-2886e2238e0f4a329ddee76a7cae766e2024-12-10T13:04:42ZengTaylor & Francis GroupJournal of Experimental Nanoscience1745-80801745-80992024-12-0119110.1080/17458080.2024.2366269Evolution of the precursor structure during the preparation of the nanopowders with perovskite-type LnLn’O3 (Ln, Ln’ = REE) complex oxide phase in the La2O3-Lu2O3-Yb2O3 systemOleksandr V. Shyrokov0Tatiana F. Lobunets1Olga V. Chudinovych2Tamara V. Tomila3Andrey V. Ragulya4Department of Physical Chemistry and Technology of Nanostructural Ceramics and Nanocomposites, Frantsevich Institute for Problems of Materials Science of the NAS of Ukraine Kyiv, Kyiv, UkraineDepartment of Physical Chemistry and Technology of Nanostructural Ceramics and Nanocomposites, Frantsevich Institute for Problems of Materials Science of the NAS of Ukraine Kyiv, Kyiv, UkraineDepartment of Rare Earth-based Functional Ceramics, Frantsevich Institute for Problems of Materials Science of the NAS of Ukraine Kyiv, Kyiv, UkraineDepartment of Physical Chemistry and Technology of Nanostructural Ceramics and Nanocomposites, Frantsevich Institute for Problems of Materials Science of the NAS of Ukraine Kyiv, Kyiv, UkraineDepartment of Physical Chemistry and Technology of Nanostructural Ceramics and Nanocomposites, Frantsevich Institute for Problems of Materials Science of the NAS of Ukraine Kyiv, Kyiv, UkraineThe thermal decomposition of complex oxide phases, such as perovskite, in the La2O3-Lu2O3-Yb2O3 systemwith a specific surface area of 37 m2/g, synthesised by the heterogeneous precipitation method under non-isothermal conditions of linear heating at a rate of 5 deg/min, was studied to reveal the features of structure changes in intermediate products. Thermogravimetric and adsorption-structural analyses, infrared spectroscopy, powder diffraction and electron microscopy revealed that the decomposition of precursors occurs in two main stages. Up to 700 °C, the initial coordination spheres are destroyed in a sequential manner, resulting in the powders remaining amorphous in phase composition. However, with a gradual increase in the order of the atoms, the change in the pore structure is non-monotonic, with an inflection point observed at 450 and 675 °C. At 675 °C, the system undergoes a collapse, accompanied with decrease in both the pore volume (V∑) and the specific surface area (SBET), which attain the lowest values of 0.0415 cm3/g and 16.5 m2/g, respectively. The second stage of decomposition of the precursor in the temperature range of 750-825 °C is associated with the formation and accumulation of the crystalline phase of perovskite in the form of a nanodispersed mesoporous powder with a specific surface area of 18 m2/g and the average mesopore diameter of 17 nm corresponding to a particle size of 40 nm when using the calculated X-ray density of 8.26 g/cm3.https://www.tandfonline.com/doi/10.1080/17458080.2024.2366269Precursorsheterogeneous co-precipitationinterlanthanidesperovskitesnanopowdersspecific surface area
spellingShingle Oleksandr V. Shyrokov
Tatiana F. Lobunets
Olga V. Chudinovych
Tamara V. Tomila
Andrey V. Ragulya
Evolution of the precursor structure during the preparation of the nanopowders with perovskite-type LnLn’O3 (Ln, Ln’ = REE) complex oxide phase in the La2O3-Lu2O3-Yb2O3 system
Journal of Experimental Nanoscience
Precursors
heterogeneous co-precipitation
interlanthanides
perovskites
nanopowders
specific surface area
title Evolution of the precursor structure during the preparation of the nanopowders with perovskite-type LnLn’O3 (Ln, Ln’ = REE) complex oxide phase in the La2O3-Lu2O3-Yb2O3 system
title_full Evolution of the precursor structure during the preparation of the nanopowders with perovskite-type LnLn’O3 (Ln, Ln’ = REE) complex oxide phase in the La2O3-Lu2O3-Yb2O3 system
title_fullStr Evolution of the precursor structure during the preparation of the nanopowders with perovskite-type LnLn’O3 (Ln, Ln’ = REE) complex oxide phase in the La2O3-Lu2O3-Yb2O3 system
title_full_unstemmed Evolution of the precursor structure during the preparation of the nanopowders with perovskite-type LnLn’O3 (Ln, Ln’ = REE) complex oxide phase in the La2O3-Lu2O3-Yb2O3 system
title_short Evolution of the precursor structure during the preparation of the nanopowders with perovskite-type LnLn’O3 (Ln, Ln’ = REE) complex oxide phase in the La2O3-Lu2O3-Yb2O3 system
title_sort evolution of the precursor structure during the preparation of the nanopowders with perovskite type lnln o3 ln ln ree complex oxide phase in the la2o3 lu2o3 yb2o3 system
topic Precursors
heterogeneous co-precipitation
interlanthanides
perovskites
nanopowders
specific surface area
url https://www.tandfonline.com/doi/10.1080/17458080.2024.2366269
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