In this work, Zr addition is proposed to refine the nanoparticle dispersion in an ODS RAF steel of composition Fe-14Cr-2W-0.3Zr-0.24Y (wt.%). Three batches of material are obtained using pre-alloyed atomized powder, where yttrium is directly introduced in the melt, and manufactured through three different processing routes. First route is based on the newly developed STARS route that aims to avoid subsequent mechanical alloying. The second route explores the impact of mechanical alloying in pre-oxidized powders. The third route uses mechanically alloyed powders without the pre-oxidation process. The ODS-powders were individually consolidated by hot isostatic pressing and later hot rolled. The obtained materials were characterized by small-angle neutron scattering (SANS) and X-ray absorption spectroscopy (XAS) techniques. SANS and XAS analysis point out the absence of oxide nanoparticles in the material based on the STAR route. SANS analysis confirms that the mechanically alloyed materials do exhibit the presence of nanoparticles. These are identified as Zr-O-rich nanoprecipitates by XAS and the calculated A-ratio by SANS is linked with the phase Y2Zr2O7. Their radii are in the range of 3–3.6 nm. XAS results show that mechanical alloying minimizes the initial differences regarding the oxidation state between the ODS powders with and without pre-oxidation.

An oxide dispersion strengthened (ODS) steel with nominal composition Fe–14Cr–2W–0.4Ti–0.3Y₂O₃ (wt%) has been manufactured by mechanical alloying of pre-alloyed powders with nanosized Y₂O₃, compacted by hot isostatic pressing and hot cross rolled. In order to evaluate the long-term thermal resistance of the alloy, it has been subjected to 2000 h of thermal aging at 873 K, which is a relevant temperature for nuclear reactor applications. A thermodynamic equilibrium simulation indicates the precipitation of Laves phase under the aging parameters used. This prediction is confirmed from the detailed multi-technique characterization performed. Before aging, Ti-rich oxides, Cr-W-rich precipitates (M₂₃C₆ type) and a homogeneous Y-rich nanoprecipitate dispersion are observed. After aging, some W-rich precipitates are identified as Laves phase, while M₂₃C₆ carbides, Ti-rich oxides and Y-rich nanoprecipitates remain stable. Mechanical characterization performed in a previous research showed higher hardness, a loss of total elongation and a slight shift of the ductile-to-brittle transition temperature (DBTT) towards a higher value after aging, with similar strength values before and after the long-term thermal treatment. These changes can be due to the redistribution of precipitates together with the Laves phase formation. The mechanical properties not being dramatically affected seem to be due to the observed stability of Y-rich nanoprecipitates distribution.

An ODS steel with nominal composition Fe–14Cr–2W–0.4Ti-0.3Y2O3 (wt.%) was produced by mechanical alloying and compacted by hot isostatic pressing (HIP) followed by hot cross rolling (HCR). To check the effects of thermal aging at relevant temperatures of operation in fusion power plants, the alloy was thermally aged at 873 K for 2000 h. In this work, small-angle neutron scattering (SANS) and X-ray absorption spectroscopy (XAS) techniques are used for the advanced characterization of secondary phases and the oxide nanoparticle dispersion. SANS results show that the oxide nanoparticles remain stable after the thermal aging treatment. Composition of the oxide nanoparticles was identified as Y2TiO5 or Y2Ti2O7 by SANS, while non-stoichiometry was found by XAS analysis. Laves phase precipitation after the thermal aging treatment is further confirmed by SANS, from the magnetic anisotropic contribution to the scattering intensity associated to this metallic phase, and by XANES.