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Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor

Gibran Esquenazi, Andrew Barron Orcid Logo

Inorganics, Volume: 6, Issue: 4, Start page: 104

Swansea University Author: Andrew Barron Orcid Logo

Abstract

The thermolysis of the polyoxometalate cluster [HxPMo12O40⊂H4Mo72Fe30(O2CMe)15O254(H2O)90−y(EtOH)y] (1) under air, argon, and reducing conditions (5%, 10%, 50% H2 with Ar balance) has been investigated. The resulting products have been characterized by XRD, SEM, and EDX analysis. Thermolysis in air...

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Published in: Inorganics
ISSN: 2304-6740
Published: 2018
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URI: https://cronfa.swan.ac.uk/Record/cronfa48085
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spelling 2019-02-25T16:01:31.3225003 v2 48085 2019-01-08 Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor 92e452f20936d688d36f91c78574241d 0000-0002-2018-8288 Andrew Barron Andrew Barron true false 2019-01-08 CHEG The thermolysis of the polyoxometalate cluster [HxPMo12O40⊂H4Mo72Fe30(O2CMe)15O254(H2O)90−y(EtOH)y] (1) under air, argon, and reducing conditions (5%, 10%, 50% H2 with Ar balance) has been investigated. The resulting products have been characterized by XRD, SEM, and EDX analysis. Thermolysis in air at 1100 °C yields predominantly Fe2O3, due to sublimation of the molybdenum component; however, under Ar atmosphere, the mixed metal oxide (Fe2Mo3O8) is formed along with Mo and MoO2. Introduction of 5% H2 (1100 °C) results in the alloy Fe2Mo3 in addition to Fe2Mo3O8 and Mo; in contrast, reduction at a lower temperature (900 °C) yields the carbide (Fe3Mo3C) and the analogous oxide (Fe3Mo3O), suggesting that these are direct precursors of Fe2Mo3. Increasing the H2 concentration (10%) promotes carbide rather than oxide formation (Fe3Mo3C and Mo2C), until alloy formation (Fe7.92Mo5.08) predominates under 50% H2 at 1200 °C. The effect of temperature and H2 concentration on the composition, grain size, and morphology has been investigated by EDX, SEM, and XRD. The relationship of the composition of 1 (i.e., Fe:Mo = 30:84) with the product distribution is discussed. Journal Article Inorganics 6 4 104 2304-6740 mixed metal oxide; polyoxometalate; nanocluster; nanoalloys 27 9 2018 2018-09-27 10.3390/inorganics6040104 COLLEGE NANME Chemical Engineering COLLEGE CODE CHEG Swansea University 2019-02-25T16:01:31.3225003 2019-01-08T12:20:33.1935730 College of Engineering Engineering Gibran Esquenazi 1 Andrew Barron 0000-0002-2018-8288 2 0048085-08012019122345.pdf esquenazi2018v2.pdf 2019-01-08T12:23:45.0130000 Output 5051909 application/pdf Version of Record true 2019-01-08T00:00:00.0000000 true eng
title Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor
spellingShingle Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor
Andrew Barron
title_short Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor
title_full Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor
title_fullStr Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor
title_full_unstemmed Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor
title_sort Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor
author_id_str_mv 92e452f20936d688d36f91c78574241d
author_id_fullname_str_mv 92e452f20936d688d36f91c78574241d_***_Andrew Barron
author Andrew Barron
author2 Gibran Esquenazi
Andrew Barron
format Journal article
container_title Inorganics
container_volume 6
container_issue 4
container_start_page 104
publishDate 2018
institution Swansea University
issn 2304-6740
doi_str_mv 10.3390/inorganics6040104
college_str College of Engineering
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hierarchy_top_id collegeofengineering
hierarchy_top_title College of Engineering
hierarchy_parent_id collegeofengineering
hierarchy_parent_title College of Engineering
department_str Engineering{{{_:::_}}}College of Engineering{{{_:::_}}}Engineering
document_store_str 1
active_str 0
description The thermolysis of the polyoxometalate cluster [HxPMo12O40⊂H4Mo72Fe30(O2CMe)15O254(H2O)90−y(EtOH)y] (1) under air, argon, and reducing conditions (5%, 10%, 50% H2 with Ar balance) has been investigated. The resulting products have been characterized by XRD, SEM, and EDX analysis. Thermolysis in air at 1100 °C yields predominantly Fe2O3, due to sublimation of the molybdenum component; however, under Ar atmosphere, the mixed metal oxide (Fe2Mo3O8) is formed along with Mo and MoO2. Introduction of 5% H2 (1100 °C) results in the alloy Fe2Mo3 in addition to Fe2Mo3O8 and Mo; in contrast, reduction at a lower temperature (900 °C) yields the carbide (Fe3Mo3C) and the analogous oxide (Fe3Mo3O), suggesting that these are direct precursors of Fe2Mo3. Increasing the H2 concentration (10%) promotes carbide rather than oxide formation (Fe3Mo3C and Mo2C), until alloy formation (Fe7.92Mo5.08) predominates under 50% H2 at 1200 °C. The effect of temperature and H2 concentration on the composition, grain size, and morphology has been investigated by EDX, SEM, and XRD. The relationship of the composition of 1 (i.e., Fe:Mo = 30:84) with the product distribution is discussed.
published_date 2018-09-27T04:15:42Z
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