Direct observation of the evolution behavior of micro to nanoscale precipitates in austenitic heat-resistant steel via electron channeling contrast imaging

Precipitation directly determines the high-temperature properties of the austenitic heat-resistant steels. The precipitations of MX, Z-phase, M₂₃C₆ and σ-phase, ranging from micrometers to nanometers, are commonly characterized using the scanning electron microscopy (SEM) and transmission electron microscopy (TEM). However, details of their evolution behavior are still unclear due to the limited SEM resolution using the traditional sampling method and the limited spatial resolution of TEM. In this work, field emission SEM-based electron channel contrast imaging (ECCI) techniques with flexible sampling routes were introduced to observe the precipitation evolution behavior of HR3C steel after aging at 700 °C for 8095 h. We showed that the coarse primary-MX and Z-phase in the as-received steel are relatively stable during aging. The coarse M₂₃C₆ and tiny secondary Z-phase dispersions were rapidly formed along the grain/twin boundaries and within dislocation arrays inside the grain interior, respectively. We further found that the M₂₃C₆ at grain boundaries would change from continuous to semi-continuous due to the formation of σ-phases, while in twin boundaries, it would become continuous over aging. Moreover, we showed that the σ-phases were in-situ transformed from M₂₃C₆ at the grain boundaries via its dissolution, facilitating the nucleation of tiny Z-phase inside the σ-phase grains, and this phenomenon has not been reported so far. We have demonstrated that ECCI with an electrolytic-polishing-based sampling route is effective in revealing multi-scale precipitation with high-throughput efficiency, and it allows the direct observation of the complex behavior of precipitates down to the nanoscale using a bulk sample. This method can be used as an efficient way for the quantitative microstructure study.