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The T91 grade and similar 9Cr tempered-martensitic steels (also known as ferritic-martensitic) are leading candidate structural alloys for fast fission nuclear and fusion power reactors. At low temperatures (300–400 °C) neutron irradiation hardens and embrittles these steels, therefore it is important to investigate the origin of this mode of life limiting property degradation. T91 steel specimens were separately neutron irradiated to 2.14 dpa at 327 °C and 8.82 dpa at 377 °C in the Idaho National Laboratory Advanced Test Reactor. Atom probe tomography was used to investigate the segregation driven formation of Mn–Ni–Si-rich (MNSPs) and Cu-rich (CRP) co-precipitates. The precipitates increase in size and, slightly, in volume fraction at the higher irradiation temperature and dose, while their corresponding compositions were very similar, falling near the Si(Mn,Ni) phase field in the Mn–Ni–Si projection of the Fe-based quaternary phase diagram. While the structure of the precipitates has not been characterised, this composition range is distinctly different than that of the typically cited G-phase. The precipitates are composed of CRP with MNSP appendages. Such features are often observed in neutron irradiated reactor pressure vessel (RPV) steels. However, the Si, Ni, Mn, P and Cu solutes concentrations are lower in the T91 than in typical RPV steels. Thus, in T91 precipitation primarily takes place in solute segregated regions of line and loop dislocations. These results are consistent with the model for radiation induced segregation driven precipitation of MNSPs proposed by Ke et al. Cr-rich alpha prime (α’) phase formation was not observed.

Atom probe tomography (APT) and scanning transmission electron microscopy (STEM) techniques were used to probe the long-time thermal stability of nm-scale Mn-Ni-Si precipitates (MNSPs) formed in intermediate and high Ni reactor pressure vessel steels under high fluence neutron irradiation at ≈320 °C. Post irradiation annealing (PIA) at 425 °C for up to 57 weeks was used to determine if the MNSPs are: (a) non-equilibrium solute clusters formed and sustained by radiation induced segregation (RIS); or, (b) equilibrium G or Γ2 phases, that precipitate at accelerated rates due to radiation enhanced diffusion (RED). Note the latter is consistent with both thermodynamic models and x-ray diffraction (XRD) measurements. Both the experimental and an independently calibrated cluster dynamics (CD) model results show that the stability of the MNSPs is very sensitive to the alloy Ni and, to a lesser extent, Mn content. Thus, a small fraction of the largest MNSPs in the high Ni steel persist, and begin to coarsen at long times. These results suggest that the MNSPs remain a stable phase, even at 105 °C higher than they formed at, thus are most certainly equilibrium phases at much lower service relevant temperatures of ≈290 °C.