Esquenazi, Gibran L.Barron, Andrew R.2018-11-122018-11-122018Esquenazi, Gibran L. and Barron, Andrew R.. "Investigation of the Reduction of a Molybdenum/Iron Molecular Nanocluster Single Source Precursor." <i>Inorganics,</i> 6, no. 4 (2018) MDPI: https://doi.org/10.3390/inorganics6040104.https://hdl.handle.net/1911/103319The 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.engThis is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).Journal articlemixed metal oxidepolyoxometalatenanoclusternanoalloysinorganics-06-00104https://doi.org/10.3390/inorganics6040104