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Improved Etching Technique to Emphasize Martensite and Bainite in High-Strength Dual-Phase Steel

Frank S. LePera National Steel Corporation

Weirton, West Virginia

Etching martensite and bainite for quantitative metal- lography of dual-phase steels presents unique problems. Standard etching techniques usually accent grain boundaries which are then counted in area measurements. Some speci- mens must be tempered or overetched to develop the contrast needed to differentiate between martensite and ferrite; when this is done, bainite cannot be quantitatively dif- ferentiated from grain boundaries. Since image analysis equipment operates by distinguishing differences between various shades of gray, contrast is of the utmost importance. Figure 1 illustrates the typical contrast problem encount- ered with a 2% nital etchant. The late Dr. Emanuel Beraha did a great deal of work on contrast enhancement by using various etchants, some of which were based on sodium metabisulfite. More recent work using this salt has again shown the advantages of tint etching.! Many etchants based on sodium metabisulfite were tried in National Steel's Research Laboratory on our chromium-bearing dual-phase steels, but most failed to dif- ferentiate martensite from bainite. However,excellent results were obtained from a mixture of 1% sodium metabisulfite (Na.S.O s ) in distilled water and 4% picric acid [C6H.(NO)30H] in ethyl alchol (either specially denatured alcohol S.D.A. 32, or completely denatured alcohol S.D.A. #1·) in a 1:1 volume ratio. With this etchant, martensite ap- pears white, bainite appears black, ferrite appears tan, and, in most cases, grain boundaries are not strongly etched. The circled area in Figure 2, which is the same field as the circled

area in Figure 1, illustrates the increased contrast developed by this improved method. Figure 3 illustrates how bainite can be readily identified. In order for the specimen to accept this new etchant, a preliminary sequence of operations consisting of grinding, polishing, and etching with 4% picric acid in ethyl alcohol is required. The specimen is prepared by wet grinding with silicon carbide paper, 180 through 600 grit. It is then rough polish- ed on a fine canvas cloth, such as Buehler's Metcloth, im- pregnated with 6-micron diamond compound. Filtered kero- sene is used as the lubricant. This step should be repeated using a fine diamond paste in the range of 0.5 - 2 microns. The specimen is then ready for the etching and final-polish- ing sequences. The specimen is etched for 6-8 sec using 4% picral, rinsed with water, and then polished using 0.3 micron alpha- alumina on a Jarrett Gold Micro-Supreme cloth, or its equivalent. This procedure should be repeated until all disturbed metal is removed, making sure each time to polish long enough to remove the "frosted" appearance created by the previous picral etching. It usually takes 2-3 etching and polishing sequences before all disturbed metal is remov-

·S.D .A. #32 requireo a U.S. government permit and, depending on the quantity used and kept on hand, may require a bond . It i. a formulation consisting of 5 gallons of ethyl ether added to every 100 gallons of ethyl alcohol. S.D.A. #1, which does not require a permit or bond, is a formulation consisting of 1 gallon of methyl isobutyl ketone, 1 gallon of ethyl acetate, and 1 gallon of gasoline added to every 100 gallon. of ethyl alcohol.

of gasoline added to every 100 gallon. of ethyl alcohol. Figure 1. High-strength dual-phase stHI, 2%

Figure 1. High-strength dual-phase stHI, 2% nital.

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Figure 1. High-strength dual-phase stHI, 2% nital. 38 Figure 2. Same field as Figure 1, improved

Figure 2. Same field as Figure 1, improved etchant

JOURNAL OF METALS • March, 1980

ed. After this requirement has been satisfied, the sample should be polished only using 0.05 micron gamma-alumina. The improved etchant is then blended, and the specimen immediately immersed for 5-10 sec. In most cases, etching times of 5-6 sec are adequate. The specimen should be oscil- lated while in the etchant, then rinsed in ethyl alcohol and blown dry. The sample should exhibit a light gold-orange to blue color on the surface. If, after etching, the ferrite grains are blue or exhibit "oriented-grain luster," where some grains are darkened and others are not, the specimen re- quires a shorter etching time. This effect is due to differing crystallographic orientations of the ferrite, and can be detri- mental when examining a specimen by image analysis equip- ment. Since the etchant must be used immediately after mixing, stock solutions of the ingredients, which have a shelf life of approximately one month, should be prepared and blended as needed. The blended etchant should be used only once, then discarded. Since the first publication of this technique,2 it has come to our attention that, depending upon alloy composi- tion, this etch sometimes develops insufficient contrast. In chromium-bearing dual-phase steels with chromium content below 0.1 wt. %, this problem can be overcome by increas- ing the etching time from 5-6 sec to 8-10 sec. Another concern has been passivation of the specimen surface caused by residues from the preliminary etching and polishing sequence. Originally, 2% nital was used dur- ing this step. However, it has been found that if any vestige of nital-etched metal remains after the final polish, the improved etchant will not delineate martensite and bainite uniformly .throughout the specimen. A final "over- polish" was previously recommended to solve this problem, but now with the use of 4% picral in the preliminary etching and polishing sequence, this problem has been eliminated. It should be noted that this etchant and associated tech- niques were developed for production-line dual-phase steels with 60% martensite or less. When a specimen contains more than 60% martensite, contrast between ferrite and martensite begins to degrade. It has also been observed that the etchant reveals large carbides in much the same way that it· shows martensite areas. If large carbides are present in appreciable number, erroneous counts can result. The application of this technique to dual-phase steels of other compositions is shown by the photomicrographs in Figures 4 and· 5. These steels, containing vanadium and molybdenum, were prepared in the same way and show excel- lent definition of the microstructure.

way and show excel- lent definition of the microstructure. Filllre 3_ High-strength dual-phase steel exhibiting a

Filllre 3_ High-strength dual-phase steel exhibiting a higher percentage of bainite, improved etchanl

JOURNAL OF METALS • March, 1980

This technique has proven to be highly satisfactory for distinguishing between martensite, bainite, and ferrite in production-line dual-phase steels when used with an image analysis system.

References

I. J.R Kilpatrick, A.O. Benscoter, and A.R Marder, "Tint Etching Improves Resolution and Contrast of Microstructures," Metal Progress, 100 (1971) pp. 79·81.

2. Frank S.

"Improved Etching Techniques for the Determination of Percent

Martensite in High·Strength Dual·Phase Steels," Metallography, 12 (2) (1979) pp . 263·

268.

LePera,

ABOUT THE AUTHOR

Frank LePera is a metaliographer in the Product

Research Division of the National Steel Research

and Development

Uberty State Coliege, and has been employed in the metaliographic field since 1973.

Laboratory . He attended West

field since 1973. Laboratory . He attended West Figure 4. High-strength dual-phase steel containing
field since 1973. Laboratory . He attended West Figure 4. High-strength dual-phase steel containing

Figure 4. High-strength dual-phase steel containing vanadium, improved etchanl

dual-phase steel containing vanadium, improved etchanl Figure 5. High-strength dual-phase steel containing

Figure 5. High-strength dual-phase steel containing molybdenum, improved etchanl

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