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EFFECT OF GRAIN SIZE DISTRIBUTION ON RECRYSTALLISATION

KINETICS INOF A MODEL ALLOYFe-30Ni


Mo Ji1, Vit Janik1, Martin Strangwood2 and Claire Davis1
1

University of Warwick, Coventry, CV4 7AL, United Kingdom


University of Birmingham, Birmingham, B15 2TT, United Kingdom

Keywords: JMAK model, recrystallisation, In-situ EBSD

Abstract
The high strength and toughness of microalloyed steels are derived by controlled rolling
schedules, using recrystallisation to give grain refinement. A number of relationships (based on
the JMAK equations) for the rate of recrystallisation, with a range of Avrami parameter values,
have
been reported previously. This paper discusses the role of grain size distribution on the
recrystallisation rates and Avrami values for an austenitic model steel (Fe-30 Ni), which has been
heat treated to generate different starting grain size distributions. Cold deformation and
annealing (at 850 950C) has been used to provide uniform macroscopic starting strain
distributions (deformed at room temperature to the strains of 0.2 and 0.3, which are equivalent
to 0.27 and 0.45 strain if deformed at 850C), followed by .recrystallisation during annealing at
850 950C. It is shown that the Avrami parameter is directly related to the grain size
distribution, with a lower Avrami exponent, i.e. 1.1 -1.4, being seen for a larger average and
wider grain size distribution. In-situ heating in an SEM with EBSD has been used to show
thatshown the recrystallisation kinetics is to be affected by both heterogeneity of nucleation sites
and local strain heterogeneity.

Introduction
Controlling recrystallisation during rolling is important in generating a fine and uniform grain
size microstructure. It has been widely accepted that recrystallisation primarily initiates in the
heavily deformed material around grain boundaries; is driven by the stored energy; and its
reaction kinetics can be expressed as a function of nucleation rate N and growth rate G. Thus,
grain size and strain are two key parameters in predicting the recrystallisation kinetics [1]. The
classical model for recrystallisation kinetics is the sigmoidal time dependence of recrystallised
volume fraction (JMAK model), where the recrystallised fraction X can be expressed as:
X =1exp (k t n )
3
f N G
is the rate parameter (f is shape factor,
4
is the Avrami exponent.
Where, k =

4
3

for spherical nucleus) and n

The model assumes that the nucleation sites are randomly distributed and all nuclei isotopically
grow isotropically at a constant rate. The rate parameter k is temperature- and composition
-dependent meaning various factors, such as nucleation kinetics, growth kinetics, and dimensions
of growth can affect the value, whereas the Avrami exponent n is only time-dependent for the
nucleation and growth rate of recrystallisation (i.e. temperature independent);, for example,
Sellars reported that the exponent showed independence of to temperature and strain rate [1].
Given the assumption of continuous / site saturated nucleation and three-dimensional growth
with a constant rate for recrystallisation, then the n value should be four or three, respectively
[2]. However, the majority of the published data give exponent values lower than two or even
one [3, 4]. Sellars gave reported a value of two for C-Mn steels [1]. Medina, Laasraoui and
Jonas tested examined microalloyed steels recrystallising at 1100-900 C and reported that the n
value was lower than one [4, 5]. Moreover, n is in many cases not a constant value but decreases
as recrystallisation progresses [1].
Recovery, which could removes stored energy before recrystallisation, has been considered
responsible for the low reported Avrami exponent values [6]. However, recently experiments
have shown that low Avrami exponents are still observed in the absence of any recovery [3].
Some authors have proposed that the heterogeneous distribution of stored energy and
variationsying in grain size distributioncan cause the low Avrami exponent values [2, 3, 7].
Strain inhomogeneity has been widely observed in deformed products; Furu observed that
heavily deformed regions tends to recrystallise quicker than less deformed regions in aluminium
[2]. And A grain size effect, i.e. heterogeneous distribution of nucleation sites, has also been
observed during recrystallisation:. Hutchinson reported that, under the same conditions, finegrained copper (average grain size of 15 m), gave an n value of 2.7 whereas the coarse-grain
size copper, (average grain size of 50 m) gave an n value of 1.7 [8].
Whilst computational modelling and interrupted tests have been widely used to study
recrystallisation kinetics, there is no comprehensive explanation for the grain size effect,whilst
also considering including strain inhomogeneity. Thus, this paper reports on the recrystallisation
kinetics at 850 950C, following 0.3 and 0.2 room temperature strain, in a model Fe-30Ni steel
with different starting grain size distributions. The Fe-30Ni steel, which is fully austenitic
allowing the deformation structure and partially recrystallised austenitic microstructure to be
observed at room temperature. In addition, in-situ heating in an SEM with EBSD has been used
to examine the grain size and strain heterogeneity effect on recrystallisation.
Materials and experimental procedures
The material used in this work is a laboratory cast ingot of composition: 0.06 C, 30.0 Ni, 0.53
Mn, 0.01 S, all in wt %. Specimens of 10 mm in diameter and 15 mm in height were machined
from the slab and then reheated to 1100C and 1300C for 30 and 5 minutes separately
respectively to relieve any residual stress in the sample and to provide different starting grain
size distributions for the deformation trials. The specimens were deformed to 0.2 or 0.3 strain by
uniaxial compression at room temperature, strain rate of 2/min, before being reheated to 950C,
900C or 850C for various times to give partial and full recrystallisation, followed by quenching
into water. The heat-treated and deformed specimens were then sectioned, mounted in Bakelite
and ground, polished and etched with Kallings reagent to reveal the austenite grain structures.
These samples were examined with a Nikon MA200 inverted optical microscopey and hardness

tested using a Wilson VH1150 machine, Hv10 kg load. The recrystallisation fraction was
determined by the point counting method from optical images. EBSD samples were prepared
using VibroMet 2 Vibratory Polisher from Buehler for two hours after general polishing to
remove any deformation induced during the polishing procedures. EBSD was performed by on a
ZEISS SIGMA FEG-SEM with Nordlys EBSD detector and samples were mounted onto a
GATAN in-situ heating stage (capable of heating to 700C); the, sample size was 5 mm squared
and 1 mm thick.
Results and discussion
Specimens with two different grain size distributions have been used to examine the grain size
effect on recrystallisation kinetics, after cold deformation, during heat treatment. The initial grain
size distributions can be seen in Figure 1. The fine-grained specimen has a mode grain size of
100 m with an area fraction of 0.32 and, 95% of grains are sized between 60 and 160 m.
Whereas the coarse-grained specimen has a mode grain size of 160 m, which with an area
fraction ofis 0.12, and 95% of grains are sized between 60 and 320 m.
0.35
0.3
0.25
Area fraction

0.2
0.15

1300-5 mins

1100-30mins

0.1
0.05
0

Figure1 Grain size distribution for Nb-free steels heat treated at different conditions.
The recrystallisation kinetics for the coarse-grained Fe-30Ni steel are shown in Figure 2 and for
the fine-grained Fe-30Ni steel in Figure 3. The curves were fitted by the JMAK model based on
the recrystallisation fraction experimental data obtained from the partially recrystallised samples.
It can be seen that the coarse-grained specimens recrystallisation starting and finishing times are
one order of magnitude slower at lower strain. For the coarse-grained specimens, at all
temperatures and strains, the Avrami exponents are between 1.1 and 1.4, Table 1, which are
within the range reported in the literature for steels [9]. It The results suggestsindicate that the n
value for Fe-30Ni is relatively constant for recrystallisation in this temperature range after 0.2 0.3 strain, which agrees with experimental data done obtained by Zadeh [10]. F As for the finegrained specimen after deformation to 0.2 strain, the Avrami exponent is 2.3, which is
considerably higher than for the coarse grained sample. The results are summarised in Table 1.
The difference in Avrami exponent is comparable to the results of fine / coarse grain copper
reported by Hutchinson [8]. And Ffrom the 0.2 and 0.3 strain test results it can be seen that and
other literature data, increasing strain does not lead to a higher Avrami exponent, consistent with
literature results [refs] suggesting that differences in strain are not the reason. In addition, in both
all cases, the Avrami exponents measured are significantly lower than the theoretical value for
site saturation nucleation and three dimensional linear growth, i.e. n=3. It has been reported that
mMacroscopic strain inhomogeneity after rolling can result in a variation inof recrystallisation
rate [3, 9, 11],. hHowever, microhardness mapping of the samples after deformation indicated

that there is no obvious macroscopic strain variation, Figure 4. Therefore, macroscopic strain
inhomogeneity cannot explain the low values of Avrami exponent.
In the JMAK approach a randomly nucleated matrix recrystallisation is assumed, however, the
grain boundary regions act as primary nucleation sites for recrystallisation. Due to the typical
log-normal distribution of grain size, the nucleation sites will not be evenly distributed within the
matrix. Thus, different grains will give different recrystallisation behaviours. Figure 5 shows an
example of the grain size distribution evolution during recrystallisation, where the an initial
starting distribution, partially recrystallised (30%) and fully recrystallised samples have been
shown. It can be seen that the area fraction of larger grains (180 m 320 m) has not changed
significantly after 30% recrystallisation indicating that the larger grains have not been consumed
by the newly formed recrystallised grains. This suggests that the recrystallisation kinetics could
be different for the different grain size classes in a distribution, that is, finer grains recrystallise
quicker and coarser grains recrystallise slower, and this could be either due to the effect of higher
nucleation sites available per unit area in the fine grains region and / or higher stored energy in
these finer grains affecting the growth rate.

JMAK 950

JMAK 900

JMAK 850

950FN

900FN

850FN

950 optical

JMAK 950

JMAK 900

Figure 2. Recrystallisation kinetics for coarse grain samples deformed to 0.3 strain (a), 0.2 strain
(b) at room temperature, then held for various times at three temperatures (850, 900 and 950C).

900 mode 100

850 mode 100

JMAK 900

JMAK 850

Figure 3. Recrystallisation kinetics for coarse fine grain samples deformed to 0.2 strain at room
temperature, then held for various times at three two temperatures (850 and 900C).
Hv 245

Hv 190

Figure 4. Microhardness mapping of Fe-30Ni specimen deformed to 0.3 strain at room


temperature, step size 0.5mm. (Examination area 3.5 mm * 7mm)
Table1 Summary of experimental Avrami exponents at for the coarse and fine grained
samples.various conditions.
Temperature (C)
Strain
Experimental n value
950 (coarse)
0.3
1.2
900 (coarse)
0.3
1.3
850 (coarse)
0.3
1.4
950 (coarse)
0.2
1.1
900 (coarse)
0.2
1.1
900 (fine)
0.2
2.3
850 (fine)
0.2
2.3

fully recrystallised

40s

homogenised

Figure 5. The grain size distribution of homogenised, 40s (30% recrystallised), and fully
recrystallised samples
To examine theis furtherrole of grain size and strain distribution further, EBSD analysis of in-situ
recrystallisation during in-situ heating EBSD analysis has been carried out to examine the effect
of grain size distribution on theto observe any heterogeneity of in nucleation sites and strain
distribution. Local misorientation has been considered as an indication of the stored energy, and
thewhere misindexeding white pixels (white in the maps in figure 6) were are assumed to be
caused by high levels of local deformationstrain. Figure 6 shows the local misorientation map of
at the onset of recrystallisation and after 25 minutes afterat 700C. It Figure 6 (a) reveals shows
that, in general, fine grains were are more deformed than coarse grains, and these highly
deformed regions recrystallised considerably faster, . As seen in Figure 6 (b)., i.e. all newly
formed grains, arrowed, were are located on in the highly deformed region shown in Figure 6(a).
Thus, the resultsit indicates that higher strain in fine grains does accelerate its their
recrystallisation kinetics. In addition, Figure 7 shows the progress of recrystallisation after 40, 60
and 80 minutes at 700C at for same region (grains 1 and 2 in these figures correspond to those
in figure 6). The fine grain 1 was is fully recrystallised and the coarse grain 2 was only 70%

recrystallised after 80 minutes, and the recrystallised grains formed in grain 1 were are much
finer than the recrystallised grains in grain 2, Figure 7 (c) . Thus, the difference in
recrystallised grain sizes it showsindicate that there are more active nucleation sites per unit area
in the fine grain region, which may also leads to a faster recrystallisation kinetics of the fine
grains.
5

1
2
200m
b

a 200m

Figure 6. Local misorientation mapsping of samples deformed to 0.3 at room temperature, then
reheated and held at 700C for 5 minutes (a), after and 25 minutes (b).

a 200m

200m

200m
c

Figure 7. Band contrast EBSD images for sample reheated at 700C for 40 mins (a), 60 mins (b)
and 80 mins (c).
Conclusions
The effect of initial grain size distribution on the recrystallization kinetics, in particular the
Avrami exponent, has been determined using a model Fe-30Ni austenitic steel. For Fe-30Ni
model alloy within strain range ofRoom temperature deformation to 0.2 and- 0.3 strain and
followed by recrystallisation at temperature range of 850 - 950C for samples with different
initial grain sizes (fine with mode grain size of 100 m and coarse with mode grain size of
160 m) has been examined., Tthe Avrami exponents were measured to be between 1.1-1.4 for
samples with the coarse grain size range 20- 320m, and 2.3 with for samples with a fine grain
size range 20-200um. The Avrami exponent under these conditionswas found to be is
independent from of strain and temperature. The hHigher Avrami exponents have been observed
for the fine grain specimens under the same conditions compared toas for the coarse grain
specimens, which iswas found to be due to a combination of microscopic strain variation and
heterogeneity of potent nucleation sites among the different grain size classes. Finer grains tend
to accumulate higher stored energy and have higher nucleation sites per unit area. Therefore,
grain size distribution plays an important role on recrystallisation kinetics and shall need to be
taken into consideration when predicting recrystallisation kinetics.
Acknowledgements

The authors would like to thank the WMG at the University of Warwick for the provision of
research facilities, and Tata Steel Europe for the provision of test material, data and financial
support of the project along with EPSRC for financial support
The author is grateful to his supervisors, Prof. Claire Davis and Dr. Martin Strangwood, for their
valuable help and supervision, to technical staff from Warwick university manufacturing group
for assistance on sample preparation and to Dr. Vit Janik for assistance on In-Situ EBSD and
valuable discussion.
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