Microstructural Evolution During Normal/Abnormal Grain

Growth in Austenitic Stainless Steel

MOHAMMAD SHIRDEL, HAMED MIRZADEH, and MOHAMMAD HABIBI PARSA

The grain growth behavior of 304L stainless steel was studied in a wide range of annealing
temperatures and times with emphasis on the distinction between normal and abnormal grain
growth (AGG) modes. The dependence of AGG (secondary recrystallization) at homologous
temperatures of around 0.7 upon microstructural features such as dispersed carbides, which
were rich in Ti but were almost free of V, was investigated by optical micrographs, X-ray
diffraction patterns, scanning electron microscopy images, and energy dispersive X-ray analysis
spectra. The bimodality in grain-size distribution histograms signified that a transition in grain
growth mode from normal to abnormal was occurred at homologous temperatures of around
0.7 due to the dissolution/coarsening of carbides. Continued annealing to a long time led to
completion of secondary recrystallization and the subsequent reappearance of normal growth
mode. Another noticeable abnormality in grain growth was observed at very high annealing
temperatures, which may be related to grain boundary faceting/defaceting. Finally, a versatile
grain growth map was proposed, which can be used as a practical guide for estimation of the
resulting grain size after exposure to high temperatures.

DOI: 10.1007/s11661-014-2426-7
 The Minerals, Metals & Materials Society and ASM International 2014

I. INTRODUCTION AGG are second-phase particles,[7,10] texture[3] and surface

AUSTENITIC stainless steels (ASSs) exhibit excellent
corrosion resistance, weldability, and versatile mechanical
properties.[1,2] Since the properties of a material depend on
the microstructure, the microstructural evolution during
grain growth at elevated temperatures has to be investi-
gated. There are two grain growth modes: (1) normal grain
growth (NGG) and (II) abnormal grain growth (AGG) or
secondary recrystallization. NGG is defined as a uniform
increase in the average grain size of a polycrystalline
aggregate by grain boundary migration as a result of
annihilation of smaller grains. Therefore, the distribution
of grain size remains relatively uniform and a monomodal
grain-size distribution will be attained. Conversely, AGG
is characterized by a bimodal grain-size distribution as a
result of the rapid growth of a small number of large
grains.[3–9] Apparently, secondary recrystallization occurs
when NGG is restrained. The main factors which lead to
MOHAMMAD SHIRDEL, Master Student, is with the School of
Metallurgy and Materials Engineering, College of Engineering,
University of Tehran, P.O. Box 11155-4563, Tehran, Iran. HAMED
MIRZADEH, Assistant Professor, is with the School of Metallurgy
and Materials Engineering, College of Engineering, University of
Tehran, and also with the Advanced Metalforming and Thermo-
mechanical Processing Laboratory, School of Metallurgy and Materi-
als Engineering, University of Tehran, Tehran, Iran. Contact e-mail:
hmirzadeh@ut.ac.ir MOHAMMAD HABIBI PARSA, Professor, is
with the School of Metallurgy and Materials Engineering, College of
Engineering, University of Tehran, and also with the Advanced
Metalforming and Thermomechanical Processing Laboratory, School
of Metallurgy andMaterials Engineering, University of Tehran, and
Center of Excellence for High Performance Materials, School of
Metallurgy and Materials Engineering, University of Tehran, Tehran,
Iran.
Manuscript submitted March 11, 2014.
Article published online July 4, 2014
effects,[11] and grain boundary faceting.[12–14]
Some research works have been published on the
kinetics of grain growth of different materials during
exposure to high temperatures.[15–19] However, the micro-
structural evolution during grain growth and correspond-
ing kinetics analysis, for the separation and determination
of the grain growth mode, in ASSs has received less
attention and a general conclusion based on the reported
research works cannot be obtained. There are several
criteria to distinguish between AGG and NGG. For
instance, according to one criterion, in NGG the majority
of grains are less than two to three times the mean grain
size,[20] whereas based on another criterion, AGG com-
mences when the ratio of Dmax/Daverage becomes >5,[10]
where Dmax and Daverage are the sizes of the maximum
observed grain and the average grain size, respectively.
Rios[21,22] has established a useful criterion, which con-
siders that when the relative size of the candidate grain for
abnormal growth (DAbnorm) increases, in such a way that
dðDAbnorm =Daverage Þ=dt>0, the AGG occurs.
The aim of this study is to investigate the microstruc-
tural evolution during NGG and AGG in an AISI 304L
ASS, elucidating the metallurgical phenomena behind it,
and development of a practical grain growth map for
this important engineering material.
II. EXPERIMENTAL MATERIALS
AND PROCEDURES
A. Material and Annealing Treatment
Commercial type 304L stainless steel was used in this
study and its chemical composition is shown in Table I.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 45A, OCTOBER 2014—5185

 Table I. Chemical Composition (Weight Percent) of the Investigated Material
Element C Si Mn P S
wt pct 0.023 0.476 1.430 0.019 0.0002
Fig. 1—Optical micrograph of the sample annealed at 1423 K
(1150 C) for 4 h.
As can be seen, the amount of microalloying elements is
relatively high in the investigated material. The micro-
alloy additions have been found to inhibit grain growth
due to finely dispersed carbides or carbonitrides.[23,24]
The samples were annealed at temperatures between
973 K and 1473 K (700 and 1200 C) for soaking times
between 1 and 4 hours and then immediately quenched
in water. Afterwards, the specimens were pickled in a
solution containing 15 pct HNO3 (65 pct strength),
5 pct HF (50 pct strength) and 80 pct water to dissolve
the oxide layer formed at the surface.[25] This operation
reduced the requirement of severe mechanical grinding.
Therefore, the strain-induced martensitic transforma-
tion[26] at the surface layer was largely inhibited. Due to
the metastability nature of austenite in ASSs, severe
mechanical grinding might produce some strain-induced
martensite on the surface, especially in coarse austenite
grains,[27,28] as shown in Figure 1.
B. Metallography
Standard metallographic techniques were employed
for the preparation of samples for optical microscopy
(OM) and scanning electron microscopy (SEM). The
following electrolytic etching techniques were used to
characterize the microstructural details. Electrolytic
etching was carried out in 60 pct HNO3 solution at
2 V[29] to reveal austenite grain boundaries as shown in
Figure 2(a) and electrolytic etching in ammonium
hydroxide solution 32 pct at 8 V[30] was used to etch
carbides (Figure 2(b)). Ultimately, for cross checking of
the presence of carbides, electrolytic etching in a
solution containing 1 g CrO3 solved in 100 mL water[31]
was used (Figure 2(c)). The CrO3 solution is toxic;
nonetheless, it reveals the carbides much more clearly.
Therefore, it is advised to use this solution to reveal
5186—VOLUME 45A, OCTOBER 2014
Cu Cr Ni Mo Ti V Nb Fe
0.110 18.470 8.050 0.089 0.003 0.129 0.128 bal.
carbides in stainless steels. The 60 pct HNO3 solution
was also found to be suitable to depict strain-induced
martensite as shown in Figure 1. The ammonium
hydroxide and CrO3 solutions can also etch annealing
twins (Figures 2(b) and (c)). Finally, for simultaneous
revealing of precipitates, grain boundaries, and anneal-
ing twins, the combination of the 60 pct HNO3 and
ammonium hydroxide solutions was found to be useful
as shown in Figure 2(d). More details of these methods
are shown in Table II. It can be concluded that each
technique has its own advantage.
The samples were observed using an optical micro-
scope and the average grain size was determined by the
standard linear intercept method.[32] About 400 random
grains were used for measurement of grain size in each
specimen. It is worth noting that at temperatures higher
than 1373 K (1100 C), because of the very large size of
the grains, calculation was limited to about 100 grains.
III. RESULTS AND DISCUSSION
A. The As-received State
The as-received initial microstructure is shown in
Figure 3(a), which reveals equiaxed austenite grain
structure with average intercept length of 10 lm. XRD
analysis has been performed using a Philips PW-3710
diffractometer with Cu Ka radiation to show that initial
microstructure is completely austenitic and the result is
shown in Figure 3(b).
B. The Effect of Annealing Temperature
The optical micrographs at a wide range of annealing
conditions are shown in Figures 4 and 5. At tempera-
tures below 1073 K (800 C), no significant grain
growth was observed. A tangible grain growth was
detected at 1073 K (800 C) for annealing times over
4 hours due to the synergic effect of the annealing time
and temperature on the grain growth. This effect can be
better seen in Figure 6. At higher annealing tempera-
tures, the time for a considerable grain growth decreases
with increasing annealing temperature as it is evident in
Figure 4. For instance, Figure 6 shows that the grain
size after annealing at 1273 K (1000 C) for 4 hours is
equivalent to that of 1423 K (1150 C) for 2 hours.
Grain growth kinetics highly depends on the grain
boundary migration and hence the atomic diffusion.
Moreover, the dissolution/coarsening of precipitates
occurs at higher temperatures.[3,23] Furthermore, the
solute drag effect of alloying elements is not effective
enough at very high temperatures due to their higher
frequency of vibration and mobility.[33] Therefore, the
grain growth kinetics is intensified by increasing anneal-
ing temperature. At very high annealing temperature of
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 2—The microstructure of AISI 304L stainless steel annealed at 1173 K (900 C) for 1 h revealed with different etching solutions: (a) 60 pct
HNO3 solution, (b) ammonium hydroxide solution 32 pct, (c) 1 g CrO3 solved in 100 mL water, and (d) ammonium hydroxide solution 32 pct
followed by 60 pct HNO3 solution.

Table II. Etching Solutions and Methods Used to Reveal the Microstructural features Of 304L Stainless Steel

Etchant Composition Details Etch time (s) Usage

Electrolytic 60 pct HNO3 2 V, 304L SS electrode 30 revealing grain boundary
solution
Electrolytic ammonium hydroxide 8 V, 304L SS electrode 100 to 150 revealing precipitates
solution 32 pct and annealing twins
Electrolytic 1 g CrO3 solved 8 V, 304L SS electrode 60 to 90 revealing precipitates
in 100 mL water and annealing twins

1473 K (1200 C), the austenite grains have coarsened
significantly, in such a way that after 4 hours, the grain
size has increased by a factor of ~30 in comparison with
the initial grain size.
Based on Figures 4 and 5, the occurrence of AGG
(secondary recrystallization) can be detected at temper-
atures around 1123 K and 1223 K (850 C and 950 C)
(~0.7Tm) and at temperatures higher than 1373 K
(1100 C) (>0.8Tm). The criterion established by
Rios[21,22] and also the criterion based on Dmax/Daverage
>5[10] were applied to differentiate between NGG and
AGG, which were consistent with each other. These
abnormal behaviors may have been related to several
reasons, which will be discussed separately for two
typical cases: annealing temperatures of 1173 K and
1473 K (900 C and 1200 C).
C. The Effect of Annealing Time
At high-enough temperatures, a considerable grain
growth happens by increasing annealing time. However,
in accordance with Figure 7, the majority of grain
growth at each temperature occurs in the first 1 hour of
annealing time. Therefore, it can be concluded that the
grain growth kinetics becomes slower during annealing,
which is connected to the reduction in the driving force
for grain growth (the total grain boundary area).[33] The
data presented in Figure 7 also imply that the effect of
annealing temperature on grain growth is more notice-
able than annealing time. The slope of the plot of grain
size (D) vs annealing time (t) at each t represents the
grain growth rate (dD/dt). It is clear that at each
temperature, the grain growth rate decreases during
annealing treatment as mentioned before. Moreover, at
each instance of time, the growth rate is greater for
higher temperatures. This is consistent with the results
of Section III–B.
D. Secondary Recrystallization at Temperatures Around
0.7Tm
Figure 8 shows the microstructural evolution during
annealing at 1173 K (900 C) with corresponding grain-
size distribution histograms. A much wider range of
annealing time was considered here to elucidate the
abnormality of the grain growth at 1173 K (900 C). At
the first 15 minutes of annealing at temperature of
1173 K (900 C), no considerable coarsening of particles
was resulted and the grain growth mode was NGG as
can be seen in Figure 8(a). However, as indicated in
Figure 8(b), by further annealing till 30 minutes, a
transition of NGG to AGG was observed, which
resulted in a bimodal distribution of grain size. One of
the basic features of AGG is bimodal appearance of its
histogram.[9,23,34,35] By continued annealing to 60
minutes, the bimodality of the histogram became more
evident as a result of further progress in secondary
recrystallization (Figure 8(c)). These observations can
be ascribed to the dissolution/coarsening of carbides as
will be discussed later. Figure 8(d) shows that by long
time annealing (12 hours) at 1173 K (900 C), the grain
growth mode has reverted to NGG. This can be
attributed to the completion of secondary recrystalliza-
tion.[33]

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 45A, OCTOBER 2014—5187

 Fig. 5—The microstructural evolution of AISI 304L stainless steel
after annealing at homologous temperatures higher than 0.74.

Fig. 3—Optical micrograph and the corresponding XRD pattern of

the as-received 304L ASS.

Fig. 6—Grain size vs annealing temperature at different annealing

times for 304L ASS.

Precipitation of second-phase particles is found to be

a crucial factor dominating the grain growth mode in
many cases. AGG has been reported mostly in alloys
Fig. 4—The microstructural evolution of AISI 304L stainless steel containing particles, e.g., in low carbon steels containing
after annealing at homologous temperatures lower than 0.74. Nb.[8,36,37] It has been reported that a slow decrease in

5188—VOLUME 45A, OCTOBER 2014 METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 7—Grain size vs annealing time curves for 304L ASS.
pinning force by slow coarsening of particles makes the
material more susceptible to AGG than a rapid decrease
in pinning force by fast dissolution/coarsening.[21,38]
When the materials with considerable amount of dis-
persed particles are annealed at a certain temperature, a
few coarse grains are formed by secondary recrystalli-
zation as a result of the dissolution/coarsening of the
second-phase particles. Depending on the chemical
composition, the ASSs may contain some precipitates
such as carbides, nitrides, and intermetallic phases,[39]
which may result in the same abnormal growth effect.
As discussed before, the investigated 304L stainless
steel in the current study contains several carbonit-
ride forming elements such as Ti, V, and Nb. As
shown in Figure 2, some carbide particles were
detected after annealing at 1173 K (900 C) for
1 hour by two metallographic methods. The X-ray
diffraction (XRD) pattern of the same sample is
shown in Figure 9. The analysis of the pattern
revealed that a new diffraction peak pertaining to a
complex carbide (composed of Ti, Cr, Fe, and C) is
present along with the austenite diffraction peaks. To
distinguish the carbide particles among the dark
etched spots of Figure 2(c), observations were carried
out in a Vega Tescan scanning electron microscope
(SEM) equipped with an energy dispersive X-ray
analyzer (EDAX). Figure 10(a) shows the typical
morphology of the carbides in the studied alloy at
high magnification.
To characterize the type of the elements present in the
carbide particles, EDAX analyses were performed on
the carbide particles. The results are shown in
Figure 10(b). The carbide particles are rich in Ti and
also have other elements such as V, Cr, Fe. This is
consistent with the XRD results shown in Figure 9. The
abovementioned analyses were also performed on the
austenite matrix (Figure 11) and its elements were found
to be Fe, Mn, Cr, Ni, V, Si, and C. Apparently, titanium
METALLURGICAL AND MATERIALS TRANSACTIONS A
only exists in carbides in the investigated alloy. Sha and
Sun[40] have studied the grain growth behavior of a
0.06 wt pct Nb-0.03 wt pct V-0.014 wt pct Ti microal-
loyed steel and have shown that the carbide particles are
rich in Ti and have small amount of Nb but were free of
V. However, they believed that this effect may be related
to the low amount of nitrogen and vanadium in their
steel. But, a relatively similar effect was observed in the
studied steel in the present work with 0.129 wt pct V,
which shows that V does not incorporate in such carbide
particles, significantly.
At the first 15 minutes of annealing at 1173 K
(900 C), the small and widely dispersed carbide parti-
cles seem to be effective in inhibition of grain growth, as
indicated before. Further annealing to 30 minutes,
results in partial dissolution/coarsening of carbides,
which leads to AGG. This situation becomes severe by
continued annealing to 1 hour.
The optical micrographs of samples annealed at
1173 K (900 C) for 1 and 12 hours are shown in
Figure 12. Careful inspection of Figures 12(a) and (b)
makes this point clear that by annealing beyond a
critical time (probably 1 hour at 1173 K (900 C)), the
growth rate of AGG significantly drops. This is due to
this fact that the number of consumable small matrix
grains available for abnormal growth decreases. It
means that when the size of abnormal grains reaches
to a critical value, their size will not change too much
and the grain growth behavior becomes practically
stagnant. For example, the ratio of the largest detected
grain after 12 hour annealing at 1173 K (900 C) to the
largest observed grain in 1 hour annealing at 1173 K
(900 C) is about 1.1.
E. Secondary Recrystallization at Temperatures Above
0.8Tm
As discussed in the previous section, at temperatures
around 0.7Tm, AGG happens in the investigated mate-
rial due to dissolution/coarsening of carbides. The
observed grain growth behavior at temperatures be-
tween 0.7Tm and 0.8Tm for annealing times between 1
and 4 hours was detected as normal. However, at very
high annealing temperatures (above 0.8Tm), AGG was
observed again. An extreme case is shown in Figure 13
for a specimen annealed at 1473 K (1200 C) for
4 hours, which is an optical micrograph that is made
of 17 individual metallographic images by an image
manipulation method. The size of the giant grain shown
in the center of this micrograph is about 3 mm, which is
about 300 times larger than the initial grain size and
exhibits a tenfold increase in comparison with average
grain size after annealing at 1473 K (1200 C) for
4 hours. The probability of AGG due to the coarsening
or dissolution of precipitates at such a very high
temperature is negligible. Therefore, the abnormality
VOLUME 45A, OCTOBER 2014—5189
Fig. 8—Optical micrographs and the corresponding grain-size distribution histograms obtained upon annealing at (a) 1173 K (900 C) for
15 min, (b) 1173 K (900 C) for 30 min, (c) 1173 K (900 C) for 60 min, and (d) 1173 K (900 C) for 720 min.

5190—VOLUME 45A, OCTOBER 2014 METALLURGICAL AND MATERIALS TRANSACTIONS A

in grain growth at these high temperatures may be less steel[13] and other metals.[12–14] More experimental
attributed to the grain boundary faceting/defaceting work is required to verify this phenomenon in the case
phenomenon as has been demonstrated for 316L stain- of the present material.

F. Grain Growth Map

In order to propose a useful map[41] to follow the
grain growth in 304L stainless steel, a grain growth
parameter (PG) was defined in this study as
PG = (D  D0)/D0. The contour lines of PG against
the homologous temperature (T/Tm) and annealing time
are shown in Figure 14. Between homologous temper-
atures of 0.66 to 0.69 (corresponding to temperature
range of 1123 K to 1173 K (850 C to 900 C)), by
considering a horizontal line at a constant homologous
temperature, the grain growth parameter changes
abruptly. At such low temperature range for grain
growth, this can be caused by AGG. At higher temper-
atures, PG is considerably higher due to occurrence of
grain growth. The developed map can be used as a guide
Fig. 9—The XRD pattern of 304L ASS annealed at 1173 K (900 C)
for 1 h.
for prediction of final grain size as a function of
annealing temperature and time.

Fig. 10—The SEM image showing carbides dispersed in the matrix and its corresponding EDAX spectra.

Fig. 11—The SEM image of the austenite matrix and its corresponding EDAX spectra.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 45A, OCTOBER 2014—5191


Fig. 12—Optical micrographs obtained after annealing at (a) 1173 K
(900 C) for 1 h and (b) 1173 K (900 C) for 12 h.
Fig. 13—Optical micrograph of a typical huge grain obtained by
merging 17 small micrographs, taken from the sample annealed at
1473 K (1200 C) for 4 h.
IV. CONCLUSIONS
The following results can be drawn from the study of
the grain growth behavior of 304L stainless steel in a
5192—VOLUME 45A, OCTOBER 2014
Fig. 14—The grain growth map for AISI 304L stainless steel repre-
sented by the contour lines of grain growth parameter as a function
of annealing temperature and time.
wide range of annealing temperatures and times with
emphasis on the distinction between NGG and AGG
modes:
1. At homologous temperatures lower than 0.65, no
considerable grain growth was observed due to the
low mobility of grain boundaries.
2. At homologous temperature of about 0.7, a transi-
tion in grain growth mode from normal to abnor-
mal was observed due to the dissolution/coarsening
of the dispersed carbides. This was demonstrated by
the appearance of a bimodal grain-size distribution
histogram. However, continued annealing to a long
time led to completion of secondary recrystalliza-
tion and the subsequent reappearance of normal
growth mode.
3. The carbide particles in the microstructure of the
304L stainless steel were found to be rich in Ti.
However, V does not incorporate in such carbide
particles, significantly. Apparently, titanium only
exists in carbides in the investigated alloy.
4. The grain growth mode was detected as normal
after annealing at homologous temperatures be-
tween 0.7 and 0.8 for annealing times between 1
and 4 hours. This can be ascribed to the complete
dissolution of carbides.
5. The mode of grain growth reverts to abnormal after
annealing at homologous temperature higher that
0.8. It maybe resulted from the grain boundary fac-
eting/defaceting as suggested by previous works.
6. It was found that the AGG happens by a rapid
growth of a few large grains at the expense of con-
suming small matrix grains. However, by further
annealing, large grains impinge and the grain
growth behavior becomes practically stagnant.
7. A versatile grain growth map was proposed,
which can be used as a guide for prediction and
METALLURGICAL AND MATERIALS TRANSACTIONS A
 estimation of the resulting grain size after exposure
to high temperatures.
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