Color Light Metallography Versus Electron Microscopy for Detecting and Estimating Various Phases in a High-Strength Multiphase Steel

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 austenitization at 900 degrees C for 5 min, followed by quenching and low-temperature bainitizing (Q&B) at 350 degrees C for 200 s. Several techniques were employed using different chemical etching reagents either individually (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 selectivity 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 degrees 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 Iota reagent at 40 degrees 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-carbon 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.

Automated summary

Fresh attempts were made to identify and estimate phase constituents in a high-silicon, medium carbon multiphase steel through color metallography using various etching techniques. The complex microstructures comprising a mixture of bainite, martensite, and retained austenite were selectively stained, with good contrasting resolution observed via light optical microscopy. Different etching techniques were required to differentiate between the various phase constituents, with the quadruple-step etching technique showing the best contrast and agreement in estimating the volume fraction of retained austenite.