Neutron powder thermo-diffraction in mechanically alloyed Fe64Ni36 invar alloy

Nanostructured Fe64Ni36 alloy has been obtained using high-energy ball milling for 35 h of milling time, Fe64Ni36 MA-35 h. The initial as-milled Fe64Ni36 MA-35 h powders are inhomogeneous, showing a majority phase with a face-centred cubic (fcc) crystal structure [88(2)%] and a minority phase with body-centred cubic (bcc) crystal structure [7(2)%]. The evolution of the microstructure with temperature between 300 K and 1100 K has been followed by means of in situ neutron powder thermo-diffraction experiments. The room temperature values for the mean crystalline size and the mechanical-induced microstrain of the fcc phase in the as-milled sample are ∼10 nm and ∼0.7%, respectively. Moreover, after heating the Fe64Ni36 MA-35 h powders up to 1100 K, an increase of around 65 K in the Curie temperature respect to that of the commercial coarse-grained alloy of the same composition is observed. The latter together with the observed temperature dependence of the lattice parameter suggests that the Fe64Ni36 MA-35 h sample subjected to the heating process exhibits invar behaviour. On heating up to 1100 K thermal relaxation of the microstructure occurs giving rise to grain growth above 100 nm, nearly vanishing values for the maximum strain, and the transformation of the bcc phase into the fcc one above 800 K, being the latter stable in subsequent heating–cooling processes.