Evolution of iron carbides during tempering of low-alloy tool steel studied with polarized small angle neutron scattering, electron microscopy and atom probe

The magnetic scattering of iron carbides in low-alloy tool steel was investigated ex-situ by polarized small angle neutron scattering measurements after tempering the steel at 550 \ub0C and 600 \ub0C. Magnetic features could be detected in the as-quenched sample resulting in a negative interference term, believed to be either θ-Fe3C, η-Fe2C, or ε-Fe2-3C. During tempering the evolution of cementite could be studied by the variation of the interference term and in γ-ratio, which is the ratio of the magnetic to nuclear scattering length density contrast. From scanning transmission electron microscopy (STEM) and atom probe tomography, it is evident that cementite (θ-Fe3C) is present directly when reaching the tempering temperature of either 550 \ub0C or 600 \ub0C. At longer tempering times, cementite gets enriched with substitutional elements like chromium and manganese, forming an enriched shell on the cementite particles. STEM and energy dispersive x-ray spectrometry show that the chemical composition of small cementite particles approaches that of Cr-rich M7C3 carbides after 24 h at 600 \ub0C. It is also seen that small non-magnetic particles precipitate during tempering and these correspond well with molybdenum and vanadium-rich carbides