The paper presents and discusses results of mechanical spectroscopy (MS) tests carried out on a Cr martensitic steel. The study regards the following topics: (i) embrittlement induced by Cr segregation; (ii) interaction of hydrogen with C–Cr associates; (iii) nucleation of Cr carbides. The MS technique permitted characterising of the specific role played by point defects in the investigated phenomena: (i) Cr segregation depends on C–Cr associates distribution in as-quenched material, in particular, a slow cooling rate (~150 K/min) from austenitic field involves an unstable distribution, which leads to Cr concentration fluctuations after tempering at 973 K; (ii) hydrogen interacts with C–Cr associates, and the phenomenon hinders hydrogen attack (HA) because hydrogen atoms bound by C–Cr associates are not able to diffuse towards grain boundaries and dislocation where CH4 bubbles may nucleate, grow, and merge to form the typical HA cracks; (iii) C–Cr associates take part in the nucleation mechanism of Cr7C3 carbides, and specifically these carbides form by the aggregation of C–Cr associates with 1 Cr atom.

An oxide dispersion strengthened (ODS) ferritic steel with nanometric grain size has been produced by low-energy mechanical alloying (MA) of steel powder (Fe-14Cr-1W-0.4Ti) mixed with Y 2 O 3 particles (0.3 wt %) and successive hot extrusion (HE). The material exhibits superior mechanical properties with respect to the unreinforced steel up to 400 • C; then such differences tend to progressively decrease and at 700 • C yield stress (YS) and ultimate tensile strength (UTS) values are very close. The microstructure and mechanical behaviour have been compared with those of ODS steels prepared by the most common process, high-energy MA, consolidation through hot isostatic pressing (HIP) or hot extrusion (HE), annealing around 1100 • C for 1-2 h. The main strengthening mechanisms have been examined and discussed to explain the different behaviour. In addition, heat treatments in the range 1050-1150 • C were carried out and a microstructural evolution with a relevant hardness decrease has been observed. TEM observations evidenced defect recovery and partial grain coarsening owing to the not perfectly homogeneous distribution of oxide particles.

The fracture surfaces of a 10.5 wt.% Cr martensitic stainless steel broken in Charpy tests have been investigated through X-ray photoelectron spectroscopy (XPS). The specimens have been examined in two different conditions: as-quenched and heat treated for 10 h at 700 °C. The trends of Fe/Cr ratio vs. test temperature are similar to the sigmoidal curves of absorbed energy and, after both ductile and quasi-cleavage brittle fractures, such ratio is always significantly lower than the nominal value of the steel chemical composition. Cr segregation does not occur on a macroscopic scale but takes place in microscopic zones which represent weaker spots in the steel matrix and a preferred path for moving cracks. Small area (diameter 300 µm) XPS measurements evidenced a higher density of such microscopic zones in the inner part of probes; this is explained by the different diffusion length of Cr atoms in the external and inner parts during quenching from austenitic field which has been calculated through FEM simulations. No significant differences of Cr concentration were observed in fracture surfaces of probes with and without heat treatment. The results highlight how Cr segregation plays a role not only in the intergranular mode of fracture but also in the quasi-cleavage and ductile ones.