Optimized carbon extraction replicas for transmission electron microscopy of nanoprecipitates in microalloyed low-carbon steels

Abstract

Nanoprecipitates play a decisive role in strengthening of microalloyed low-carbon steels. The direct carbon extraction replica (CER) method is a promising way to extract the nanoprecipitates from the surrounding iron matrix for a detailed characterization of their structure and chemistry using electron microscopy. Better results can generally be obtained by electron microscopy when the magnetic matrix is removed. However, there are challenges in the preparation of relatively thin CERs, especially during stripping and cleaning stages of the procedure. In this contribution, a systematic study of different parameters associated with the direct CER preparation method was performed on a vanadium-microalloyed low-carbon model steel to improve the replication procedure. Relatively low nanoscale surface kurtosis of the iron matrix with respect to the thickness of the deposited carbon layer was found to be important for successful replications from different crystallographic planes of the matrix during the stripping stage. Furthermore, modified water-based stripping and cleaning solutions were introduced that minimized wrinkling, coalescence, and disintegration of ∼8 nm thick CERs. These results are supported by (scanning) transmission electron microscopy observations, which showed successful extraction of V-rich nanoprecipitates in a size range of 1–50 nm from both the ferritic and bainitic microstructures. The modified method improves the common direct CER preparation procedure and can be used to study precipitates in a wide range of microalloyed low-carbon steels.