Color light metallography versus electron microscopy for detecting and estimating various phases in a high-strength multiphase steel

Abstract

In this study, fresh attempts have been made to identify and estimate the phase constituents of a high-silicon, medium carbon multiphase steel (DIN 1.5025 grade) subjected to austenitiza-tion at 900 °C for 5 min, followed by quenching and low-temperature bainitizing (Q&B) at 350 °C for 200 s. Several techniques were employed using different chemical etching reagents either indi-vidually (single-step) or in combination of two or more etchants in succession (multiple-step) for conducting color metallography. The results showed that the complex multiphase microstructures comprising a fine mixture of bainite, martensite and retained austenite phase constituents were se-lectivity stained/tinted with good contrasting resolution, as observed via conventional light optical microscopy observations. While the carbon-enriched martensite-retained austenite (M/RA) islands were revealed as cream-colored areas by using a double-step etching technique comprising etching with 10% ammonium persulfate followed by etching with Marble's reagent, the dark gray-colored bainite packets were easily distinguishable from the brown-colored martensite regions. However, the high-carbon martensite and retained austenite in M/RA islands could be differentiated only after resorting to a triple-step etching technique comprising etching in succession with 2% nital, 10% ammonium persulfate solution and then warm Marble’s reagent at 30 °C. This revealed orange-colored martensite in contrast to cream-colored retained austenite in M/RA constituents, besides the presence of brown-colored martensite laths in the dark gray-colored bainitic matrix. A quadruple-step technique involving successive etching with 2% nital, 10% ammonium persulfate solution, Marble’s reagent and finally Klemm’s Ι reagent at 40 °C revealed even better contrast in comparison to the triple-step etching technique, particularly in distinguishing the RA from martensite. Observations using advanced techniques like field emission scanning electron microscopy (FE-SEM) and electron back scatter diffraction (EBSD) failed to differentiate untempered, high-carbon martensite from retained austenite in the M/RA islands and martensite laths from bainitic matrix, respectively. Transmission electron microscopy (TEM) studies successfully distinguished the RA from high-car-bon martensite, as noticed in M/RA islands. The volume fraction of retained austenite estimated by EBSD, XRD and a point counting method on color micrographs of quadruple-step etched samples showed good agreement.