61

METALLOGRAPHY 20:61-73 (1987)

Retained Austenite in Intercritically Annealed HSLA Steel

Q. Y. LONG, D. TSENG, AND K. TANGRI

Metallurgical Sciences Laboratory, Department of Mechanical Engineering, University

of Manitoba, Winnipeg, Manitoba, Canada R3T 2N2

The effects of processing parameters on austenite retention in intercritically annealed

HSLA steels have been investigated. Low-temperature tempering was found to be necessary
for successful tint etch of high-carbon martensite in dual-phase structure with sodium metabisulfite. Cold working before the intercritical anneal increases the nucleation sites for
transformation to austenite and, thereby, the amount of retained austenite is generally increased. The microstructural evolution during postanneal cooling is detrimental to austenite
retention. Both the particle size effect and the chemical stabilization by carbon are responsible for the suppression of martensitic transformation.

Introduction
Commercially produced dual-phase steels, which are usually derived
from high-strength low alloy (HSLA) steels by intercritical annealing,
often contains a few volume percent of retained austenite particles. These
particles transform into martensite during deformation. The effect of retained austenite on the mechanical properties of dual-phase steels has
been the focus of several recent studies [1-3]. The content of retained
austenite is known to vary with processing parameters such as the intercritical annealing temperature and the postanneal cooling rate [2, 3]. The
x-ray diffraction technique [4] is commonly used to determine the volume
fraction of retained austenite. However, this technique is time-consuming
and presents some difficulties in heavily deformed samples because of
the presence of strong texture. The alternative is to use quantitative metallography. The objectives of the present study were to develop a reliable
etching technique for distinguishing martensite from retained austenite
and to investigate systematically the effect of processing parameters on
austenite retention.
Elsevier Science Publishing Co., Inc., 1987
52 Vanderbilt Ave., New York, NY 10017

0026-0800/87/$03.50

62

Q. Y. Long et al.

Experimental Procedure
The material used in this study was a commercial H S L A steel with a
wt.% composition of 0.07 C, 1.63 Mn, 0.018 S, 0.012 P, 0.11 Si, 0.062 V,
and 0.024 Nb. The as-received steel plate of 11 mm thickness was annealed
at 925C for 0.5 h and quenched in water. It was then tempered at 690C
for 0.5 h and air-cooled. After this heat treatment, the steel contained
spheroidized carbides distributed mainly at ferrite grain boundaries. The
steel plate was subsequently cold-rolled to 7 mm thickness. The intercritical anneal was done in the temperature range of 700-850C for 300
s, followed by cooling in still air. The average cooling rate from the annealing temperature to 500C was approximately 4C/s. The cooling rate
gradually slowed down at temperatures below 500C.
Metallographic specimens were mechanically polished and then electrolytically polished in 10% chromic acid. The etching procedure included
a pre-etch in 2% Nital for 2 s and a tint etch in 10% sodium metabisulfite
for 20 s [5]. The quantitative metallographic analysis was carried out with
a Leitz image analyzer.

Results and Discussion

TINT ETCHING OF MARTENSITE
The etching response of martensite in dual-phase steels to tint etchants
such as sodium metabisulfite varies considerably with the postanneal cooling rate. For cooling rates faster than 5C/s, the martensite islands are
stained black by sodium metabisulfite and the retained austenite remains
as light as the ferrite matrix. For cooling rates slower than 5C/s, the
martensite phase cannot be stained by sodium metabisulfite and therefore
is indistinguishable from retained austenite. This is demonstrated in Fig.
l(a) for a sample that was annealed at 720C and air-cooled. The martensite phase can be stained black by sodium metabisulfite only after lowtemperature tempering at 150C for 10 min (Fig. 1[b]). The x-ray analyses
of the retained austenite content made before and after tempering did not
show any detectable change. Therefore the martensite particles in Fig.
l(b) are not the product of tempering. The retained austenite particles
readily transform into martensite during deformation. However, martensite induced by deformation cannot be tint etched by sodium metabisulfite
either. In fact, the retained austenite particles resulting from slow postanneal cooling (<5C/s) are enriched with austenite-stabilizing elements
such as carbon and manganese and thus their Ms temperatures fall below
27C [7]. The martensite derived from this type of austenite is a highcarbon plate martensite [2]. It is concluded that low-temperature tern-

Retained Austenite in HSLA Steel

63
.=.

e--

*~

It**
e.,

ql~ ~

,0

~L~, ~

....

E
I

e-,

e-,

E
0

,.A
ekr~

64

Q. Y. Long et al.

pering is necessary for properly tint etching high-carbon martensite in

dual-phase steels with sodium metabisulfate.
E F F E C T OF COLD WORKING
Figure 2 shows the effect of cold working before the intercritical anneal
at 780C on the nucleation of austenite. The sample was cold-worked
before annealing and had a consistently smaller average particle size, but
a higher density of retained austenite particles (Fig. 2[b]) than that which
was not cold-rolled (Fig. 2[a]). Austenite has been found to nucleate preferentially at the carbide-ferrite interface [8]. However, not every carbide
particle serves as a nucleation site. This indicates that the carbide-ferrite
interface may not always be a favorable nucleation site for austenite. It
is known that dislocations are trapped around hard particles during deformation. These dislocations are probably responsible for the nucleation
of austenite during the intercritical anneal, as it has been shown in Fig.
2 that a preanneai cold working greatly increases the density of nuclei for
austenite.
M I C R O S T R U C T U R A L EVOLUTION DURING COOLING
Austenite resulting from intercritical anneal undergoes a continuous
decrease in particle size, with alloy elements partitioning between ferrite
and austenite during slow cooling in air. The typical microstructural evolution during cooling is shown in Fig. 3. The samples were annealed at
810C for 300 s, followed by air cooling to predetermined temperatures
and quenching in water. The larger austenite particles transformed into
martensite (the dark particles in Fig. 3) after quenching in water, whereas
the smaller particles remain austenitic (light particles in Fig. 3[d]). The
two factors that may affect the resistance of austenite to martensitic transformation are (1) the particle size and (2) the concentrations of austenite
stabilizers such as carbon and manganese in the present alloy. The size
stabilization effect has been observed in submicron-sized ~/iron particles
[9] and fct zirconia particles [10], both in the copper matrix. This indicates
that the size effect alone is sufficient to suppress the martensitic transformation of austenite particles if the particle size is smaller than 1 ~m.
The size stabilization effect of austenite in the present alloy is clearly
demonstrated in Fig. 3, wherein only small particles are seen to be retained austenite. However, Tseng et al. [7] have shown that the stability
of retained austenite also varies with carbon content. Furthermore, larger
retained austenite particles up to 5 ~m have been observed, particularly
in those samples annealed at higher intercritical temperatures such as

l:l

e-.

Ii.a"

,,:

i~i :

4'

:e~ ;..-_, :.Z':

2~

(b)

FIG. 3. Microstructural evolution during postanneal cooling. The larger austenite particles transform into martensite (dark particles) after
ater quench, whereas the smaller particles remain austenitic. (a) 810C; (b) 720C; (c) 550C; (d) 400C; (e) schematic representation of heat
:reatment to produce the microstructures shown in (a) to (d),

(a)

G,x

Retained Austenite in HSLA Steel

67

68

Q. Y. Long et aI.

810"C/5 rain

F20 Coolingrote = 4*C/sec

II

~550
It
w
w
Fo

TIME
(e)
FIG. 3.

(Continued)

840C. Therefore, in addition to the particle size effect, chemical stabilization due to carbon and manganese also plays a role in the retention
of austenite. However, because of the short annealing times (300-360 s)
in the intercritical temperatures and the relatively slower diffusion of manganese, the enrichment of austenite by manganese may not be very significant [2]. Therefore, the chemical stabilization of austenite in the
present case resulted mainly from carbon enrichment. Transmission electron microscopy [2] has revealed that twinned martensite, characteristic
of high carbon content, is observed in air-cooled samples but not in oilquenched samples. This is indirect evidence that further carbon enrichment of austenite occurs during postanneal cooling. This also indicates
that a higher solubility of carbon in austenite is still maintained below the
eutectoid temperature, which is about 700C for this alloy. Furthermore,
peadite formation has not been observed in air-cooled samples that are
annealed below 840C. It is therefore visualized that the processes occurring during air cooling are the migration of the ferrite-austenite interphase boundaries and, at the same time, the diffusion of carbon atoms
into the remaining austenite grains. Alternatively, the movement of the
interphase boundaries might be controlled by carbon diffusion. It is inferred from the results of present study that the final particle size of
austenite can be effectively controlled by controlling the postanneal cooling rate.
I N F L U E N C E OF ANNEALING TEMPERATURE
Figure 4 shows the morphologies of retained austenite after annealing
at various intercritical temperatures. All the samples were given a 36%

"Ib

FIG. 4.

(a)

(b)

Microstructures illustrating the influence of annealing temperature. (a) 720C; (b) 760C; (c) 810C; (d) 840C.

r : ' , , , r t~ "

r~

ic)
FIG. 4.

(Continued)

(d)

71

Retained Austenite in H S L A Steel

area reduction before annealing. The contents of retained austenite and

martensite vary within a narrow range (14-17 vol.%). However, more
austenite particles are seen to transform into martensite (dark particles
in Figs. 4[a] and [b]) during postanneal cooling from lower annealing temperatures, such as at 720C and 7600C. The amount of martensite decreases with increasing annealing temperature. At annealing temperatures
of 840C and higher, the large dark particles as seen in Fig. 4(d) are either
tempered martensite or carbide resulting from decomposition of austenite
because they can be tint etched by sodium metabisulfite without tempering
at 150C before etching.
Accordingly, the content of retained austenite increases initially with
increasing annealing temperature, reaches a maximum around 7900C and
decreases for higher annealing temperatures (Fig. 5). The annealing temperature corresponding to the maximum retention of austenite varies with
heat-treatment conditions such as heating and cooling rates and the holding time at the annealing temperature. Rigsbee and Vander Arend [1]
found this temperature for maximum austenite retention to be 850C for
18
16

w
z~12
Q
I,i,I
Z

0 6

/.

I 4
t)
2 D

7OO

75O

8OO

850

ANNEALING TEMPERATURE (*C)

FIG. 5. Content of retained austenite versus annealing temperature.

Q. Y. Long et al.

72

a steel of similar composition, but using a different heat-treatment

scheme. The variation of the amount of retained austenite with annealing
temperature as shown in Fig. 5 may be rationalized in terms of the particle
size and the chemical stabilization effects. As the heat-treatment routine
is a nonequilibrium type, the detailed processes involved during annealing
and cooling are not completely understood.

Summary and Conclusions

1. Low-temperature tempering is found to be necessary for a successful
tint etch of high-carbon martensite in dual-phase steels with sodium
metabisulfite.
2. Cold working before the intercritical anneal increases the density of
nuclei for austenite and, therefore, generally increases the content
of retained austenite after intercritical annealing.
3. During postanneal cooling, the austenite particle size continuously
decreases and at the same time the particles are enriched by fastdiffusing carbon atoms. Both the particle size effect and the chemical
stabilization by carbon are responsible for the suppression of martensitic transformation.

The authors are grateful to the lnterprovincial Steel and Pipe Corporation, Regina, Saskatchewan, for providing the HSLA steel. The research
was supported by NSERC.

References
1. J. M. Rigsbee and P. J. Vander Arend, Laboratory studies of microstructure and structure-property relationships in dual-phase HSLA steels, in Formable HSLA and DualPhase Steels (A. T. Davenport, Ed.) TMS/AIME, New York (1979), pp. 56-86.
2. N. R. V. Bangaru and A. K. Sachdev, Influence of cooling rate on the microstructure
and retained austenite in an intercritically annealed vanadium-containing HSLA steel,
Met. Trans. 13A:1899-1906 (1982).
3. J. J. Yi, K. J. Yu, I. S. Kim, and S. J. Kim, Role of retained austenite on the deformation
of an Fe-0.07 C-1.8 Mn-l.4 Si dual-phase steel, Met. Trans. 14A: 1497-1504 (1983).
4. C. F. Jatczak, J. A. Larson, and S. W. Shin, RetainedAustenite andlts Measurements
by X-Ray Diffraction, Society of Automotive Engineers, Warrendale, PA (1980).
5. A. R. Marder and A. O. Benscoter, Quantitative microanalysis of dual-phase steels,
Metallography 15:73-85 (1982).
6. A. R. Marder and B. L. Bramfitt, Processing of a molybdenum-bearing dual-phase steel,
in Structure and Properties of Dual-Phase Steels, (R. A. Kot and J. W. Morris, Eds.),
TMS-AIME, New York (1979), p. 242.
7. D. Tseng, Q. Y. Long and K. Tangri, An acoustic emission study of martensitic transformation of retained austenite, (to be published).

R e t a i n e d A u s t e n i t e in H S L A S t e e l

73

8. C. I. Garcia and A. J. Deardo, Formation of austenite in 1.5 pct Mn steels, Met. Trans.
12A:521-530 (1981).
9. K. E. Easterling and H. M. Miekk-oja, The martensitic transformation of iron precipitates in a copper matrix, Acta Metall. 15:1133-1141 (1967).
10. I. W. Chen and Y. H. Chiao, Martensitic nucleation in ZrO2, Acta Metall. 31:16271638 (1983).

Received December 1985; accepted April 1986.