Journal article 1136 views 118 downloads
Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor
Gibran Esquenazi,
Andrew Barron
Inorganics, Volume: 6, Issue: 4, Start page: 104
Swansea University Author: Andrew Barron
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DOI (Published version): 10.3390/inorganics6040104
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...
| Published in: | Inorganics |
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| ISSN: | 2304-6740 |
| Published: |
2018
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| Online Access: |
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| URI: | https://cronfa.swan.ac.uk/Record/cronfa48085 |
| 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 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. |
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| Keywords: |
mixed metal oxide; polyoxometalate; nanocluster; nanoalloys |
| College: |
Faculty of Science and Engineering |
| Issue: |
4 |
| Start Page: |
104 |