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Modeling of austenite grain growth behavior for AISI 302

stainless steel
BENMAZIANE Sara1, BEN LENDA Omar1, 1SAAD Elmadani.
1
University Hassan 1st, laboratory of Physico-Chemistry of Processes and Materials, , Faculty
of Sciences and Techniques Settat, Morocco.

Abstract
In this paper, the austenite grain growth process of AISI 302 steel was studied in a
temperature range of 900 to 1000 °C and a holding time up to 360 minutes. From the
experimental part, it was found that the increase of the heating temperature caused the
dissolution of carbides, therefore the austenite grain size grew faster implying a higher
growth rate. The prolongation of the holding time also led to an increase in the size of the
austenite grains. Based on the experimental results and a combination of Arrhenius and
Sellars type equations in this paper, a model of austenite grain growth has been developed
taking into consideration the effects of heating temperature, of holding time and initial
austenite grain size on austenite grain growth. The ability of the model to predict austenite
grain growth was confirmed by statistical indicators.

Keywords: AISI 302 steel, austenite grain growth, heating temperature, holding time,
mathematical model.

1. Introduction
Stainless steels are used in many fields such as medicine, shipbuilding, aeronautics,
mechanical industry, food industry, chemical industry, transportation, etc., due to their
durability, resistance to high temperatures and U.V., as well as being completely recyclable
[1].
Among these steels we find the austenitic stainless steels which are the most widespread
thanks to their better ductility, their resistance to cold and heat as well as to corrosion due to
the presence of chromium and nickel [2].
The processes of manufacturing or using stainless steels are generally based on hot forging
and pressing to refine the grains. These treatments can affect the structure of the steels and

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consequently their mechanical properties [2–4]. From this point of view, the control of the
effects of the heating temperature and the holding time on the growth of the austenite grains
is primordial.
Several works are performed to study the behavior of austenite grain growth for different
materials and different heating conditions. Among which we cite the work of Beck et al.
[5,6], which treated the growth of the average size of high purity aluminum grains, for
different heating temperatures from 350 °C to 650 °C and for different holding times from 20
seconds to 11 days. From their study they concluded that the time index increases linearly
with increasing heating temperature, thus an empirical formula is set up for the prediction of
aluminum grain growth. The major drawback of their model is the negligence of the effect of
temperature on grain growth, and the focus only on the effect of holding time. Sellars and
Whiteman [7] have in turn proposed a model for the prediction of grain growth of a C-Mn
steel in short normalization treatments, while considering the influence of the initial grain
size. The grain growth index in their study is 10 for a very short time, this value is higher than
expected, but it decreases for longer times. Li et al. [8] studied the behavior of austenite grain
growth while visualizing the effect of homogenization on grain size, for a GCr15 bearing
steel cast billet, the homogenization heat treatments are carried out for a range of temperature
and holding time from 1000 to 1250 °C and from 30 to 180 min respectively. In areas of high
concentration they notice the presence of small grains as opposed to areas of low
concentration where large grains are present. Dong et al. [9] modeled the growth kinetics of
austenite grains in a low-alloy steel by taking into consideration the effect of heating
temperature, holding time, and heating rate on grain growth. The effects of pinning were also
studied by transmission electron microscopy, this analysis revealed a dissolution of the
precipitates with the increase of the temperature, consequently a fast growth of the austenite
grains. Ettore Anelli [10] established a mathematical model to predict the microstructure
during hot rolling as well as the effects of temperature, deformation, deformation rate and
time on the microstructural and thermal homogeneity of wires and bars. According to Anelli
the formation of heterogeneous austenitic structures is due to the effects of recrystallization
mechanisms and the thermal gradient present along the diameter of the bar. R. C. Chen et al.
[11] developed a mathematical model to predict the behavior of austenite grain growth in
300M steel, combining the Sellars and Anelli models. Normal and abnormal grain growth
was analyzed while considering the influence of temperature, time, and initial grain size on
growth. The results of this study indicated that the main mechanism of austenite grain growth
is migration of grain boundaries. Guang Ji et al. [12] analyzed the austenite grain growth for
high carbon steel with Nb-Ti and without Nb-Ti at different heating temperatures and holding
times. For the steel containing Nb-Ti, they found a decrease in austenite grain size and rate
when compared with the steel that does not contain Nb-Ti. This reduction is due to the
pinning effect caused by the Nb-Ti carbides.
In this study the austenite grain growth of AISI 302 steel was treated thermally by
considering the influence of initial grain size, heating temperature, and holding time on grain
growth. A mathematical model is established to predict the growth of austenite grains, the
predicted and experimental results are in good agreement.

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2. Material and experimental procedures
The chemical composition (weight percentage) of AISI 302 steel is presented in Table 1.
The austenite grain growth process was studied using square specimens of size 15 x 15 x 15
mm, these specimens were cut vertically by grinding wheels, then heat treated at heating
temperatures of 900 to 1000 °C during different holding times up to 360 minutes, in an
electric box furnace. Then they are directly quenched in water.
For the microscopic study, the specimens are ground, polished and etched with an aqueous
aqua regia solution composed of 5 ml nitric acid HNO3, 15mL hydrochloric acid HCl and 100
ml water. Then, the microscopic examination of the specimens was carried out with an
OPTIKA metallograph equipped with a high resolution AIPTEK camera, as well as a
scanning electron microscope coupled with an energy dispersive electron microprobe. The
average austenite grain size was measured by the linear intercept method.
Table 1: Chemical composition of AISI 302 steel (wt.%)

Cr C Ni Si Mn P S Fe
18 0.15 8 0.4 0.61 0.03 0.012 Balance

3. Experimental results
3.1. Influence of holding time on the microstructure and grain size of austenite
Figure 1 shows the optical micrograph of AISI 302 steel after treatment at 1000 °C at
different holding times. From the figures 1a and 1b, the presence of fine and coarse grains can
be noticed, whose boundaries present curvatures. By prolonging the holding time, we notice
an increase in the size of the austenite grains, as well as the transformation of the austenite
grain boundaries from curved to polygonal shape with straight edges as shown in figures 1c
and 1d.

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Figure 1: Optical micrograph of AISI 302 steel after treatment at 1000 °C at different holding
times. (a) 5 min, (b) 20 min, (c) 60 min and (d) 200 min.

Figure 2 represents the growth of the average austenite grain size as a function of the holding
time. While fixing the heating temperature it can be observed that the average austenite grain
size increases with the increase of the holding time. This growth becomes more important at
higher heating temperatures. It can also be seen from figure 2 that the growth of the austenite
grain occurs in 2 stages. The first stage of rapid growth which occurs during a relatively short
holding time, and the second stage of slower growth which occurs during a relatively long
holding time. The prolongation of the holding time implies a decrease in the growth rate of
the austenite grains [13]. This means that most of the austenite grain growth occurs in the first
stage, which allows us to conclude that the driving force in this stage is more important and it
decreases by prolonging the holding time.
To validate the relationship between the rate and driving force of austenite grain growth, we
will refer to the following equations:
First, the driving force equation „ ‟ is expressed as follows [8,14] :

(1)

Where is a dimensionless geometric constant, is the grain boundary energy and is the
average austenite grain size.
From Equation 1, it is evident that the driving force increases with decreasing average
austenite grain size, and it decreases with its increase.
Secondly, the relationship between the rate and driving force of austenite grain growth is
represented as follows [8] :

(2)

Where is the pre-exponential coefficient, is the activation energy for austenite grain
growth (J/mol), is the temperature (K), and is the gas constant (8.314 J/mol.K).

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It can be seen from equation 2 that the rate and driving force of grain growth are proportional.
Consequently, the decrease in driving force implies a decrease in the rate of grain growth,
which is in good agreement with the results in figure 2.

Figure 2: Evolution of the average austenite grain size with different holding times after heat
treatment at 900 °C, 950 °C and 1000 °C.

3.2.Influence of heating temperature on austenite grain size


Figure 3 represents the evolution of the average austenite grain size at different heating
temperatures. From this figure it can be seen that the increase of the heating temperature
implies the increase of the average size of the austenite grains. This increase is more evident
at longer holding times. It can also be noticed that the growth of the austenite grains becomes
more exponential with the extension of the holding time. From figure 3 we can also reveal the
influence of the heating temperature on the growth rate of the austenite grains, which clearly
increases after 950 °C. The increase of the growth rate with increasing temperature is
palpable from equation 2.
According to the phase diagram of our study steel determined by the JMatPro computer
software, which is presented in figure 4, we notice the presence of precipitates, mainly M23C6
between 900 and 1000 °C. These carbides slow down the growth of the austenite grains.
Increasing the heating temperature will result in the progressive dissolution of the carbides,
therefore the austenite grains grow faster [12,15].

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Figure 3: Evolution of average austenite grain size with different heating temperatures at
different holding times.

Figure 4: Phase diagram of AISI 302 steel as received.

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3.3.Influence of precipitated particles on austenite grain size
Figure 5 shows the microstructure of AISI 302 steel observed by optical microscope for a
heating temperature of 900 °C and a holding time of 1 and 10 minutes. From figure 5a no
intergranular precipitation was detected, since the requirement for M23C6 precipitation is not
satisfied at this very short holding time. By prolonging the holding time we observe the
segregation of carbides in the form of a discontinuous film at the grain boundaries due to their
high interfacial energy, as shown in figure 5b.
Zener and Smith [16] concluded that the presence of precipitates in steels causes a decrease in
the growth of austenite grains at high temperature, the undissolved precipitates trap the
austenite grains which limits their growth.
The relationship between the precipitate pinning force and the displacement of the grain
boundaries is defined as follows [12,17,18] :

(3)

Where is the drag force, and are the volume and radius of the precipitated particles,
respectively, and is the interface energy.
According to equation 3, the pinning force is proportional to the volume fraction of the
precipitated particles and inversely proportional to their size. This means that a decrease in
the fraction of precipitated particles with the increase of their size implies the decrease of the
pinning force, and consequently the size of the austenite grains increases.

Figure 5: Optical micrograph of the microstructure of AISI 302 steel after treatment at 900 °C
for: (a) 1 min, (b) 10 min.

Figure 6 shows a scanning electron microscope image of AISI 302 steel at a heating
temperature of 900 °C and a holding time of 20 minutes. The results obtained confirm those
found in the phase-temperature diagram calculated by JMatPro, the intergranular carbides are
of the M23C6 type, composed essentially of chromium and carbon (see figure 4).

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In conclusion, the developed carbides exert pinning forces on the grain boundaries which
limits the growth of austenite grains, this blockage decreases with increasing temperature due
to the progressive dissolution of precipitates, as shown in the phase diagram.

Figure 6: SEM micrograph of the microstructure of AISI 302 steel after treatment at 900 °C
during 20 min.

4. Modeling and discussion


4.1.Modeling of the growth of austenite grains
According to the above study the growth of austenite grains is influenced essentially by two
parameters: the heating temperature and the holding time.
In the literature there are two types of models that are widely used for the prediction of
austenite grain growth, the Arrhenius type equations [8,19] which are based on the heating
temperature and the holding time in their prediction, in this model is constant, the second
model is the Sellars type equations [7,9,12] which add in their prediction the effect of the
initial size of the austenite grains, so that is constant and is equal to 1.
In this study we will take into consideration the influence of the initial austenite grain size
while considering constant, therefore a combination of the two models will be used for
modeling the growth of austenite grains. The equation of our model is expressed as follows:

(4)

Where and are the average and initial austenite grain size (µm), respectively, is the
austenite grain growth index, is the austenite grain growth time index, these indices are
determined experimentally, is a constant, is the holding time (min), is the activation
energy of grain growth (J/mol), is the gas constant (8.314 J/mol. K) and is the heating
temperature (K).
Taking the natural logarithm of equation 4 while rearranging it we obtain the following
equation 5:
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(5)

Using the experimental data while fixing , the parameters and are obtained by partial
derivation from Equation 5, respectively, with respect to at a specified heating
temperature, and with respect to ⁄ at a fixed holding time. Their expressions are expressed
as follows:

(6)


(7)

The linear fit of equations 6 and 7 allows us to determine the values of and for different
values of , so by replacing them in equation 5 the values of are deduced for each n.
This allows us to obtain several austenite grain growth functions according to each value of .
Thus the most optimum grain growth index „ ‟ is determined through the error function, f
error is expressed according to equation 8:

∑ (8)

Where the austenite grain size calculated by the mathematical model and is the
austenite grain size measured from experiments.
Figure 7 visualizes the variation of as a function of . The optimal value of n
corresponds to the minimum of the curve where the first derivative of cancels.
After polynomial fitting of the data, the function is determined according to equation 9.
The ideal grain growth index that corresponds to the point where the derivative of the
function cancels is equal to 2.4867 from figure 7.

(900 – 1000 °C) (9)

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Figure 7: Variation of the sum of squared errors ‘ ’ as a function of n.

In order to determine the grain growth time index „ ‟ and the activation energy of grain
growth „ ‟ at the optimal value of already defined, linear fit of the calculated data of the
variation of as a function of ln(t) related by equation 6, as well as the variation
of as a function of 1000/T correlated by equation 7, depicted in figures. 8 and 9,
is used.
From the linear fit lines the values of and are 0.895733 and 187786.9323 J/mol
respectively at this heating temperature stage (900 °C - 1000 °C). Subsequently the value of
„ ‟ is calculated from equation 5, which is 2.3953×1010 at the same temperature level.
At this level the elements of equation 5, , , and are determined, and then our
mathematical model to describe the austenite grain growth of AISI 302 steel is presented as
follows:

( ) – (10)

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Figure 8: Relationship between and ln(t) at different heating temperatures.

Figure 9: Relationship between and 1000/T at different heating temperatures.

4.2.Verification of the deployed mathematical model


Figure 10 represents the variation of the grain diameter predicted by our mathematical model,
as well as the experimental grain diameter as a function of holding time at different
temperatures. This figure allows us to validate our mathematical model by comparing the

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predicted and experimental results. From this comparison we notice a good agreement
between the predicted and experimental results, which means that our model can predict the
austenite grain growth at this temperature stage.
In addition, in order to verify the accuracy of our mathematical model, we use statistical
parameters. In our study we chose the coefficient of determination (R²) which allows to
measure the quality of the prediction of the model. When R² tends towards 1 it means that our
mathematical model has a strong predictive power. The second parameter used in this study is
the average absolute relative error (AARE) which is the average of the relative errors of the
model, it indicates the accuracy of the model. When the value of the AARE is small the
model is reliable. And the last parameter used is the root mean square error (RMSE), which is
a measure that groups all the prediction errors of the different data points, allowing to predict
with rigor the accuracy of the model. When its value is smaller it indicates a better accuracy.
R², AARE and RMSE are calculated according to the following equations [17,20] :

√∑ √∑

√ ∑

Where and are the experimental and mathematically predicted grain size, respectively,

and are the mean values of and , respectively, and is the total number of
experimental data.

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Figure 10: Comparison between predicted and measured austenite grain sizes for different
conditions.

The values of statistical parameters R² „coefficient of determination‟, AARE „average


absolute relative error‟ and RMSE „root mean square error‟ of the data presented in figure 11
are 0.993228, 6.90%, 3.89µm respectively. From these values it can be concluded that our
model can accurately predict the austenite grain growth of AISI 302 steel at this heating
temperature stage.

Figure 11: Comparison of average grain size data between experimental and predicted from the
grain growth model.

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5. Conclusions

In this study, the growth of austenite grains in AISI 302 steel was treated, at heating
temperatures between 900 and 1000 °C and holding times up to 360 minutes. From this
study the following conclusions were drawn:
- The austenite grain growth process is influenced by the heating temperature as well as the
holding time, however the effect of the heating temperature is more evident.
- The growth of austenite grains occurs in two stages, a rapid growth stage related to a short
holding time, and a more stable growth stage related to a longer holding time.
- The presence of carbides at the austenite grain boundaries blocks their growth, the
increase in temperature implies the dissolution of carbides, and consequently a faster
growth.
- The mathematical model developed in this study takes into consideration the effect of
heating temperature, holding time and initial austenite grain size. This model is verified
by statistical parameters, which proved its ability to accurately predict the growth of
austenite grains.

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