M E T A L L O G R A P H Y 12:263-268 (1979)

263

Improved Etching Technique for the Determination of Percent Martensite in High-Strength Dual-Phase Steels

F. S. LEPERA

National Steel Corporation, Research Lahorcitory, Weirton, WV 26062

An improved metallographic etchant and technique for delineating the various constituents in high-strength dual-phase steels has been developed as a result of the need for increased contrast w h e n using electronic image analysis equipment. With an etchant consisting of a 1% a q u e o u s solution of s o d i u m metabisulfite (NazS~O.d and 4% picric acid (C~H2(NO2)3OH) in ethyl alcohol, martensitic grains appear white, bainite appears black, ferrite appears tan, and in most cases, the grain boundaries are not strongly etched. C o n s e q u e n t l y , accurate m e a s u r e m e n t s of the a m o u n t of martensite and bainite can be made using electronic image analysis equipment,

The etching of martensite and associated structures for detailed quantitative metallography of high-strength dual-phase steels has always been a problem. Conventional techniques and etchants have many drawbacks when used in conjunction with electronic image analysis equipment: grain boundaries are revealed and counted in area measurements, specimens must be tempered or over-etched to develop sufficient contrast, and, when either of these is done, bainite "~takes on the same s h a d e " as the grain boundaries. Figures 1-4 illustrate some of the contrast problems encountered with a 2% nital etchant. Since image analysis equipment operates by using black and white and intermediate shades of gray, contrast is of the utmost importance. Considerable work on contrast improvement has been done in the past by the late Dr. Emanuel Beraha using tint etching solutions based on sodium metabisulfite, and recent work has proved again the advantages of these methods [1]. Many solutions based on this salt were tried in National Steel's Research Laboratory, but most failed to provide contrast needed for a positive differentiation of martensite from bainite. The circle
Elsevier North Holland, Inc., 1979 0026-0800/79/030263 . 5501.75

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F. S. LePera

FIG. 1.

High-strength dual-phase steel. 2% Nital.

FIG. 2.

Same sample as Fig. 1. 2% Nital.

Short C o m m t t , i c a t i o n s

265

FIG. 3. Nital.

High-strength dual-phase steel exhibiting a higher percentage of bainile. 2'i

FIG. 4.

Same Sample as Fig. 3. 2% Nital.

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F. S. LePera

Fro. 5. Same Field as Fig. 3. Improved etchant.

on Fig. 1 shows an example of an area where the martensite is not clearly delineated from the ferrite. H o w e v e r , it was found that a mixture of 1% aqueous sodium metabisulfite and 4% picric acid in ethyl alcohol in a 1 : 1 ratio, produced excellent contrast, as seen in the circled area in Fig. 6. The new etchant eliminates the need for tempering and clearly defines the martensitic grains when used on a properly p r e p a r e d sample (see Figs. 5-8). Specimens are p r e p a r e d in a conventional m a n n e r with a final polishing sequence of a series of polishings and short etching treatments (57 sec.) using 2% nital to r e m o v e any disturbed metal. E x t r e m e care must be exercised to r e m o v e all traces of the 2% nital etch before attempting to use the i m p r o v e d etchant. It was found that if any vestige of the nital etch remained, the surface appeared to be passive to the i m p r o v e d etchant. Generally, the final polishing time had to be doubled to ensure the complete r e m o v a l of the nital-etched metal. If the i m p r o v e d etchant fails to delineate the martensite uniformly throughout the sample, it is usually because the final polish was of insufficient duration, and therefore, failed to r e m o v e all of the 2% nital-etched metal. The etchant is mixed and the specimen is immediately i m m e r s e d for 7-12 sec at r o o m t e m p e r a t u r e . The specimen should exhibit a type of

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267

FIG. 6.

Same field as Fig. 1. Improved etchanl.

i

FiG. 7.

Same field as Fig. 2. Improved etchant.

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F. S. LePera

FIG. 8.

Same field as Fig. 4. Improved etchant.

effervescent action at the surface during the etching process. Following this, the specimen is rinsed with ethyl alcohol and blown dry. The specimen surface should appear blue-orange. If insufficient contrast is noted, the etching time needs to be increased. H o w e v e r , there is a limit to the duration of etching, since with increased time, the ferrite exhibits "'oriented grain luster" where some ferrite grains are darkened and others are not. This effect is the result of their differing crystallographic orientations and can be detrimental for use with image analysis systems. It has been noted that this etchant reveals large carbides in much the same way as it shows martensite grains. If an appreciable number of large carbides is present, erroneous counts can result. Our experience has shown that this technique is an excellent way to distinguish martensite, bainite, and ferrite in high-strength dual-phase steels when used with an image analysis system. Reference
I. J. R. Kilpatrick, A. O. Benscoter, and A. R. Marder, "'Tint Etching h n p r o v e s Resolution and Contrast of M i c r o s l r u c t u r e s " , Metal Pr~,~,resx 100:79-81 (1971).

Received t:ebrua~?" 1979.