Insight on precipitate evolution during additive manufacturing of stainless steels via in-situ heating-cooling experiments in a transmission electron microscope

Abstract

During additive manufacturing of alloys, just after local heat-matter interactions, a molten material undergoes rapid solidification. Then, for the rest of the building time, it is subjected to cooling/heating cycles in the solid-state i.e., solid-state thermal cycling. The thermo-mechanical forces generated during solid-state thermal cycling can trigger a plethora of micro-mechanisms that can bring about significant microstructural changes that determine the eventual mechanical properties of as-built parts. In this work, the aim is to gain insight on solid-state thermal cycling-driven evolution of submicron-sized precipitates in an austenitic stainless steel using transmission electron microscopy. To that end, thin-film lamellae are extracted from a pre-built sample and subjected to different in-situ solid-state thermal cycles inside a transmission electron microscope. The solid-state thermal cycles are designed to understand the role of temperature amplitude and rate, number and type of thermal cycles, and post-process annealing on precipitate evolution. High angle annular dark field imaging and energy dispersive X-ray spectroscopy before and after each thermal cycle provide a deep insight on the contribution of different thermal cycling factors on the evolution of precipitate composition, size and morphology. Common trends include diffusion of Mn and Si from Mn-Si-rich oxides into the surrounding matrix, formation of Cr rings around oxide precipitates and S redistribution in non-oxide precipitates. Similar Cr rings and S distributions were also found in precipitates in as-built samples studied in (Upadhyay et al. [30]), which strongly supports the representativeness of these results with respect to what occurs during additive manufacturing.