An Improved

Steel

Tint

Sheets

with

Etching
Mixed

Method

for High

Strength

Microstructures*

By Seishiro BANDOH,** Osamu MATSUMURA*** and Yasuharu

Synopsis
An improvedtint etching methodwas developedto obtain a quantitative
measure of the microstructure of high strength steel sheets with a mixed
structure. The proceduresof etching are presented with typical examples.
The present methodrevealsferrite in blue, martensite and retained austenite
in light yellow, and bainite in brown. Each constituentis identified by
electronmicroscopicobservationsof the same area on etchedmicrostructure.
The differentcolors are analyzed to be a result of differencein the thickness
of etchedfilms by means of Auger spectroscopy. The new methodis combined with image analysis to determine quantitatively the fraction and
morphologyof microconstituents.
Key words:
metallography; optical microscopy; etching method; coldrolled steel; composite structure.

I.

Introduction

Development of " dual-phase " steely with a mixed

microstructure of ferrite and martensite was an innovation in the history of efforts for enhancing the
strength of steel sheets for automobile use. Many
studies2'3~have been reported on this type of steel
sheets characterized by the continuous yielding and
good combination of high strength and ductility. Replacement of martensite by bainite4 was a further
improvement.
Recently steels containing about
10-.20 % retained austenite have been developed to
improve the strength-ductility balance by the transformation induced plasticity (TRIP).5? In order to
understand the effects of the chemical compositions
and heat treatments on the mechanical properties, the
microstructure such as morphology and fraction of
microconstituents must be characterized. Microstructural observations are usually made with optical microscopy, scanning and transmission electrom microscopy and X-ray diffraction. However, these methods
have difficulties in quantitative measurements of complicated microstructure with an order of a few micrometers. Tint etching techniques6-8~ to discriminate
the microstructure by colors have many merits. However, the conventional techniques are not satisfactory
because of the difficulty in distinguishing each structural component reliably and clearly for a wide variety of chemical compositions and heat treatments.
Table

**
***

1.

Chemical

composition (wt%) and estimated

SAKUMA***

The present authors intended to develop a new tint

etching technique for optimal characterization
of the
microstructures
in high strength steel sheets with a
mixed structure.
II.

Chemical
Composition
of Test Steel

and

Heat

Treatment

Cold-rolled steel sheets of 0.8-mm thickness were

used as the starting material.
The chemical composition is given in Table 1. Figure 1 shows the heat
treatment
cycle simulating continuous annealing in
intercritical
region and quasi-austemper
treatment.
The fraction of microstructural constituents was varied
to prepare a variety of microstructures
with the annealing temperature for ferrite and with soaking time
in the bainite transformation
temperature for martensite, bainite and retained austenite.
III.

Procedure

of New

Tint Etching

In the new tint etching technique, selection of holding resin, temperature of etchants, etching time, and
temperature and humidity of air used to dry the sample is important factors to obtain a satisfactory etch
figures.
A test piece, 20 mm x 15 mm, is adhered to acrylic

Fig.

transformation

1.

Schematic

temperature

dia gram

(C)

of heat

of

the

treatment

steel

cycles.

sheet.

Based on the paper presented to the 112th ISIJ Meeting, October 1986, 51302, at Nagoya University in Nagoya. Manuscript
received on October 7, 1987; accepted in the final form on December 12, 1987. 1988 ISIJ
Analysis Research Lab., Nippon Steel Corporation.
Now at Nippon Steel Techno Research, Ida, Nakahara-ku, Kawasaki 211.
Sheet & Coil Research Lab., Nippon Steel Corporation, Fuchinobe, Sagamihara 229.

Research

Article

( 569)

(570)

Transactions

ISIJ, Vol.

28,

1988

resin which stiffens at room temperature

with sufficient strength for handling.
The sequence of polishing is wet grinding, primary polishing with spraying
of liquid containing diamond powder, and final polishing with alumina.
The polished specimen must be
dried in air with a relative humidity below 45 %.
The etchant is a mixture of three ingredients with
the compositions shown in Table 2. The ingredients
must be removed solute oxygen by Ar gas and mixed
immediately before etching.
The etchant is necessary to be kept at a temperature
between 20 and
25C. The specimen is etched by holding vertically
in a bath.
At first the whole polished surface is light
brown, but in 2 or 5 s the microstructural
constituents
are colored differently.
However, overlong etching
reduces the contrast among the constituents to make
the identification difficult, as shown in Fig. 2. Immediately after rinse in water, the etched sample must be
Table

2.

Com position

and

mixing

ratio

of in gredients.

dried by a blow of warm air with a relative humidity

under 40 %. The humidity of drying air is an important factor for fixing of the etched figures. As
shown in Fig. 3, tinting is performed optimally when
the relative humidity is low; when the humidity exceeds 64 %, identification of microstructural constituents becomes difficult.
Figure 4 shows the appearance of samples optimally etched in accordance with the present method.
These photographs are taken in a metallurgical microscope with a high bright halogen lamp. The micrographs on the left (a), (c) and (e) are tint etched
images, and the corresponding images etched by nital
are (b), (d) and (f) on the right side. The blue regions indicated by the numbers 1, 2 and 3 in photographs (a), (c) and (e) are ferrite grains corresponding with the same numbered regions in photographs
(b), (d) and (f). From the comparison of corresponding photographs, it is recognized that the morphology
of ferrite grains is accurately reproduced and that the
ratio and distribution are demonstrated by tinting.
Martensite and retained austenite are colored light
yellow and bainite brown. The coloring is confirmed
by transmission electron microscopy of a two-stage
replica of the specimens etched at a constant voltage.9/
An example is the inside region of the white frame in
Fig. 5. In the electron micrographs, accurate identification is possible because an individual constituent

Fig.

2.

Optimum

etching

time.

Transactions

Fig.

3.

Effect

of humidity

on color

ISIJ,

Vol.

28,

1988

(571)

fi xmg.

Fig. 4.
Comparison of new tint etching and conventional
etching (2 ;, nital) for mixed microstructures.

shows

color

differently

by

pattern
The

tint

observed
method

chemical
found
0.6

G,

by

and

with

mixing

tion

to high-alloy

ratio

different
well

microstructures.

a composition

Si and

optimum

the

The

corresponds

by the electron
microscopy.
was applied
to steels
with

steels

0.1-2.0

pattern.

method

compositions
that

etched

etched

etching

0.1-1.0

selection
of

ingredients.

steels

was

difficult.

can
etching

However,

various
was

of 0.04be

IV.

the

Tinted
To

properly
time

and

applica-

by

and

Microstructure

clarify

tinted
It

range

Mn
of the

to

the

with

Figure

depth

to steel

in

for

Fe,

and

S in

that

the

implies

the

the

Film

by

this

of
films

No significant

through-the-thickness
spite
chemical

of

the

technique

electron

results

is

composition

etching

Auger

tinted

Thickness

microstructure

chemical

the

differently

substrate.

served
0,

film

Its

the

micro

6 shows

profiles

face

why

color,

of tinted

analyzed

scopy.

reason

a different

thickness

were

and

spectro-

compositional
from

the

difference

suris ob-

distribution
different

composition

colors.
of

of
This

differently

(572)

Transactions

Fig . 5.

Fig.

Research

6.

ISIJ, Vol.

Transmission

28,

electron

1988

rnicrograph

of two-stag

Compositional depth-profiles through blue (upper),

brown (middle), and light yellow (lower) colored
films measured with Auger electron spectroscopy.

Article

e replicated

from

the framed

area

on

optical

microg

raph

(left).

Transactions

colored films is the same. On the other hand, sputtering time to reach the steel substrate differs depending on the color of etched film : 19 min for blue, 17
for brown, and 14 for light yellow. Therefore, the
thickness of film is in the order of blue, brown, and
light yellow. The color of microstructures are shown
to be related significantly to the film thickness.
V. Observation of Various Microstructure Formed
after Soaking in Bainite
Transformation
Temperature
Bainite transformation in steels with about 1N 2 %
Si retains a substantial amount of austenite after cooling to room temperature at incomplete transformation.10~ The retained austenite is utilized effectively
for development of high-strength steel sheets with excellent strength-ductility balance.5~ The microstructures were studied by using this new etching technique
and image analysis. Figure 7 is the result of the
image analysis. Areal fraction of individual colors
was measured within the white margin of photograph
(a) by separating the blue, brown, and light yellow
areas as shown in Figs. 7(b) to 7(d). The measured
area fraction and the number of particles on separated
color image are presented in Fig. 7. The image analyzer is not capable to discern the microstructure

Fig. 7.

Etched figure of a mixed microstructure

(d) martensite and retained austenite.

Fig. 8.
Variations
uents during

of the fraction
isothermal

of microconstitholding

at 400C.

etched

by the

conventional

Is",

Vol.

methods.

28,

1988

However,

(573)

ap-

plication
of the new method
contrasts
distinctly
the
microstructure
by color to provide accurate
information.
Samples
held at 400C for periods
shown in
Fig. 1 were examined
by the present method.
Since
both martensite
and retained
austenite
are colored in
light yellow,
the amount
of retained
austenite
was
determined
with X-ray diffraction
to obtain the fraction of martensite
by subtracting
from the total area
of light yellow region.
Figure 8 shows the variation
of microconstituents
during
isothermal
holding
at
400C.
Transformation
of austenite
to bainite
and
stabilization
of retained
austenite
during
holding
at
400C are clearly recognized.
VI.

Conclusion

An improved
tint etching technique
was developed
as an easy and rapid characterization
of microstructure in high strength
steel sheets with a mixed structure.
Ferrite is tinted blue, martensite
and retained
austenite
light yellow,
and bainite
brown.
Appearance of the microstructures
in different
colors under

(a) and its separate image of each constituent, (b) ferrite, (c) bainite, and

Transactions

(574)

ISIJ, Vol.

28,

1988

optical microscopy
are thought
to be a result of the
difference
in thickness
of the tinted films formed on
the individual
microconstituents.
The etching method can be combined
with image analysis.
The new
method
will contribute
to further
improvements
and
developments
of high strength
steels.
REFERENCES
1)
2)

S. Hayami and T. Furukawa : Microalloying 75, Union

Carbide Corp., New York, (1975), 78.
Structure and Properties of Dual-phase Steels, ed. by R. A.
Kot and J. W. Morris, Metall. Soc, of RIME, New York,
(1979).

Research

Article

3)

Fundamentals of Dual-phase Steels, ed. by R. A. Kot and

B. L. Bramfitt, Metal!. Soc. of RIME, New York, (1981).
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Shibata : Trans. Iron Steel Inst. Jpn., 21 (1981), 820.
5) 0. Matsumura, Y. Sakuma and H. Takechi:
Trans. Iron
Steel Inst. Jpn., 27 (1987), 570.
6) F. S. Lepera:
Metallography,12 (1979), 263.
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Met.
Prog.,100 (1971), No. 6, 79.
9) S. Bandoh, 0. Matsumura and T. Herai:
Tetsu-to-Hagane,
69 (1983), 5338.
10) R. LeHouillier, G. Begin and A. Dube: Metall. Trans., 2
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