The Quality of Fe14Cr ODS Powder Alloys During Milling and Upon Heating and Its Impact on the Mechanical Properties of Consolidated Steels

Oxide dispersion-strengthened ferritic steels (ODSFSs) are promising structural materials for applications in fusion and fission power reactors, but further improvement in their (high-temperature) mechanical properties and ferrite phase stability is required. This work demonstrates that an approach to produce Fe14Cr ODSFSs with a stable ferrite phase and improved strength could involve grain size strengthening by long-term milling with a tiny amount of nitrogen. Fe-14Cr-3W-0.4Ti-0.25Y2O3 powders were ball-milled up to 170 hours under an argon atmosphere. In addition to X-ray diffraction, the change in product quality during milling and upon heating was thoroughly investigated by more sensitive magnetic and thermal analysis by measuring the saturation magnetization σs, coercivity Hc, Curie temperature Tc, and temperature of ferrite-austenite (α → γ) transition Tα→γ. A pronounced modification of magnetic and microstructure parameters was observed when milling over 70 hours and upon heating above 800 °C and was found to be generated by long-term milling with a tiny amount of nitrogen. Upon heating, the nitrogen, incorporated during milling, developed a α → γ transition region, with the decomposition of nitrides precipitated at the earlier stage of heating followed by austenite decomposition, nitrogen degassing, and microstructure refinement to a grain size of a few tenths of a nm (e.g., 28 nm by heating at 910 °C of 100-hour milled powder). The resulting ferrite phase with refined grains is highly stable to (further) heating. The powders milled for 70 and 100 hours containing 0.175 and 0.500 wt pct nitrogen, respectively, were consolidated at 1100 °C with subsequent annealing at 1050 °C and subjected to Vickers hardness and 3-point bending tests. The steel produced from the powder milled for 70 hours shows lower hardness, higher density (close to the theoretical value of 7.8 g/cm3), and fracture strain. The ductility of this ODS alloy (0.075 fracture strain) is comparable with Eurofer97 (0.075 fracture strain), whereas its strength (2070 MPa ultimate stress) is significantly higher than that of Eurofer97 (1222 MPa ultimate stress). This improvement was attributed to grain size strengthening—the refined grains (promoted by milling with nitrogen) could be effectively pinned by Y-Ti-O dispersoids.