Hydrogen-based direct reduction of multicomponent oxides: Insights from powder and pre-sintered precursors toward sustainable alloy design
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| Format: | Preprint |
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2025
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| _version_ | 1866912829654695936 |
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| author | Shankar, Shiv Ratzker, Barak Ma, Yan Raabe, Dierk |
| author_facet | Shankar, Shiv Ratzker, Barak Ma, Yan Raabe, Dierk |
| contents | The co-reduction of metal oxide mixtures using hydrogen as a reductant in conjunction with compaction and sintering of the evolving metallic blends offers a promising alternative toward sustainable alloy production through a single, integrated, and synergistic process. Herein, we provide fundamental insights into hydrogen-based direct reduction (HyDR) of distinct oxide precursors that differ by phase composition and morphology. Specifically, we investigate the co-reduction of multicomponent metal oxides targeting a 25Co-25Fe-25Mn-25Ni (at.%) alloy, by using either a compacted powder (mechanically mixed oxides) comprising Co3O4-Fe2O3-Mn2O3-NiO or a pre-sintered compound (chemically mixed oxides) comprising a Co,Ni-rich halite and a Fe,Mn-rich spinel. Thermogravimetric analysis (TGA) at a heating rate of 10 °C/min reveals that the reduction onset temperature for the compacted powder was ~175 °C, whereas it was significantly delayed to ~525 °C for the pre-sintered sample. Nevertheless, both sample types attained a similar reduction degree (~80%) after isothermal holding for 1 h at 700 °C. Phase analysis and microstructural characterization of reduced samples confirmed the presence of metallic Co, Fe, and Ni alongside MnO. A minor fraction of Fe remains unreduced, stabilized in the (Fe,Mn)O halite phase, in accord with thermodynamic calculations. Furthermore, ~1 wt.% of BCC phase was found only in the reduced pre-sintered sample, owing to the different reduction pathways. The kinetics and thermodynamics effects were decoupled by performing HyDR experiments on pulverized pre-sintered samples. These findings demonstrate that initial precursor states influence both the reduction behavior and the microstructural evolution, providing critical insights for the sustainable production of multicomponent alloys. |
| format | Preprint |
| id |
arxiv_https___arxiv_org_abs_2507_01242 |
| institution | arXiv |
| publishDate | 2025 |
| record_format | arxiv |
| spellingShingle | Hydrogen-based direct reduction of multicomponent oxides: Insights from powder and pre-sintered precursors toward sustainable alloy design Shankar, Shiv Ratzker, Barak Ma, Yan Raabe, Dierk Materials Science The co-reduction of metal oxide mixtures using hydrogen as a reductant in conjunction with compaction and sintering of the evolving metallic blends offers a promising alternative toward sustainable alloy production through a single, integrated, and synergistic process. Herein, we provide fundamental insights into hydrogen-based direct reduction (HyDR) of distinct oxide precursors that differ by phase composition and morphology. Specifically, we investigate the co-reduction of multicomponent metal oxides targeting a 25Co-25Fe-25Mn-25Ni (at.%) alloy, by using either a compacted powder (mechanically mixed oxides) comprising Co3O4-Fe2O3-Mn2O3-NiO or a pre-sintered compound (chemically mixed oxides) comprising a Co,Ni-rich halite and a Fe,Mn-rich spinel. Thermogravimetric analysis (TGA) at a heating rate of 10 °C/min reveals that the reduction onset temperature for the compacted powder was ~175 °C, whereas it was significantly delayed to ~525 °C for the pre-sintered sample. Nevertheless, both sample types attained a similar reduction degree (~80%) after isothermal holding for 1 h at 700 °C. Phase analysis and microstructural characterization of reduced samples confirmed the presence of metallic Co, Fe, and Ni alongside MnO. A minor fraction of Fe remains unreduced, stabilized in the (Fe,Mn)O halite phase, in accord with thermodynamic calculations. Furthermore, ~1 wt.% of BCC phase was found only in the reduced pre-sintered sample, owing to the different reduction pathways. The kinetics and thermodynamics effects were decoupled by performing HyDR experiments on pulverized pre-sintered samples. These findings demonstrate that initial precursor states influence both the reduction behavior and the microstructural evolution, providing critical insights for the sustainable production of multicomponent alloys. |
| title | Hydrogen-based direct reduction of multicomponent oxides: Insights from powder and pre-sintered precursors toward sustainable alloy design |
| topic | Materials Science |
| url | https://arxiv.org/abs/2507.01242 |