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Article history: The hot deformation behavior and static microstructure evolution of a 21Cr stabilized ferritic stainless
Received 5 December 2012 steel was studied using axisymmetric hot compression tests on a Gleeble 1500 thermomechanical
Received in revised form simulator. The deformation was carried out at 950–1050 1C to strains of 0.2 to 0.6 using strain rates of
24 January 2013
0.01, 0.1 and 1 s 1. The compression was followed by a holding period of 0 to 180 s in order to study
Accepted 25 January 2013
Available online 9 February 2013
the static recrystallization kinetics. The electron backscatter diffraction (EBSD) technique was used in
analyzing the resultant microstructures. A constitutive equation that well describes the flow stress as a
Keywords: function of strain, strain rate and temperature was developed. The active dynamic restoration
Ferritic stainless steel mechanism was found to depend on the Zener–Hollomon parameter, such that continuous dynamic
Flow stress
recrystallization was observed under low Zener–Hollomon parameter conditions but under high
Constitutive analysis
Zener–Hollomon parameter microstructures were dynamically recovered, and no dynamic formation
Restoration mechanisms
Recrystallization of new grains occurred. Static recrystallization resulted in little or no grain refinement, and further,
EBSD strain did not have an accelerating effect on the static recrystallization kinetics beyond the strain of 0.4.
& 2013 Elsevier B.V. All rights reserved.
0921-5093/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2013.01.077
2 S.V. Mehtonen et al. / Materials Science & Engineering A 571 (2013) 1–12
the post hot rolling annealing. The amount of stored energy of a were machined from the hot-rolled bands. The size of the speci-
bulk material can be measured quantitatively by thermal analysis mens was chosen so that the height to diameter ratio is within the
methods, such as differential scanning calorimetry (DSC) e.g. acceptable limits of 1–2 [24]. Axisymmetric compression tests
[14–16]. Electron backscatter diffraction (EBSD) and transmission were performed employing a Gleeble 1500 thermomechanical
electron microscopy (TEM) [16,17], microhardness e.g. [16,18] and simulator. The specimens were reheated at the rate of 20 1C/s to
the line broadening of X-ray diffraction (XRD) [19] are methods for 1100 1C for solution annealing, held for 2 min and then cooled to
qualitatively analyzing the dislocation density and thereby the the deformation temperature (950, 1000 or 1050 1C) at the cool-
local stored energy. Further, the amount of stored energy can be ing rate of 10 1C/s. The specimens were compressed in a single hit
estimated qualitatively from the amount of work hardening in the to a true strain of 0.2–0.6 at a constant true strain rate of 0.01,
flow stress curves [20]. The dynamic restoration processes greatly 0.1 or 1 s 1. After the compression, the specimens were either
affect the amount of stored energy and hence the static restoration water quenched to room temperature immediately after the
mechanisms and kinetics. The flow behavior and the microstruc- deformation or held at the deformation temperature for 10 to
ture evolution of austenite in static recrystallization process during 180 s, and subsequently air cooled to room temperature. The
hot deformation are extensively studied subjects. Also the defor- deformed and annealed microstructures were characterized using
mation of ferrite in interstitial free and low-carbon steels has been a field emission scanning electron microscope FEG-SEM (Carl
investigated by many authors in warm working temperature range, Zeiss Ultra Plus) with an electron backscatter diffraction detector
e.g. [21,22], but in these studies, the deformation took place below (EBSD) (HKL Nordlys). The recrystallized fractions were deter-
the austenite–ferrite phase transformation temperature A1. There- mined metallographically from the deformed and annealed speci-
fore, the restoration mechanisms may differ from those experi- mens using the SEM-EBSD. For metallographic examinations,
enced in the hot deformation temperature range of 950–1050 1C. cross-sections of the cylindrical compression specimens halved
Zhang et al. [23] investigated the effect of shear bands formed parallel to the cylinder axis were used. One specimen was
during hot rolling on static recrystallization rate in a 21%Cr ferritic quenched immediately after the 2 min of solution annealing at
stainless steel, however they did not pay attention to the flow 1100 1C in order to measure the initial grain size. This was found
behavior of the steel. to be 157 mm using the mean linear intercept method.
In this study, the hot deformation behavior of stabilized high-
Cr ferritic stainless steel was investigated by hot compression
tests with the final aim of clarifying the hot rolling schedules, 3. Results and discussion
which might improve the final product quality. The purpose was
to identify the dynamic restoration processes taking place during 3.1. Flow behavior during hot deformation
hot deformation and to develop constitutive equations to predict
the flow stress under various Zener–Hollomon parameter condi- The measured flow stress curves during compression tests are
tions. Also, the effect of Zener–Hollomon parameter on the static presented in Fig. 1. The shape of flow curves is similar to those
restoration kinetics was studied in order to explore ways to previously measured for high-Cr ferritic stainless steel [12]. (Note
promote recrystallization after the hot rolling stage. that the drop in the flow stress curves at the higher strain rates at
the strain of about 0.06 is caused by a machine effect and has no
2. Experimental
Table 1
The experimental steel used in the study was laboratory cast Chemical composition of the investigated
ingot of 70 kg hot rolled at 1100 1C from 48 mm down to the steel (in wt%).
thickness of 15 mm with 3 passes. The chemical composition (in
weight percent) of the steel is listed in Table 1. Cylindrical C N Cr Ti Nb
Fig. 1. Flow stress curves at strain rates of 0.01–1 s 1 at (a) 950 1C, (b) 1000 1C and (c) 1050 1C.
metallurgical origin.) The flow stress increases with decreasing 3.2. Constitutive equations
deformation temperature and increasing strain rate. However, it
is seen that at 1000 and 1050 1C at low strain rates of 0.01 and Constitutive equations describing flow stress in terms of
0.1 s 1 there is hardly any work hardening, except at very small deformation temperature and strain rate can be expressed by
strains, indicating the occurrence of pronounced dynamic recov- the Zener–Hollomon parameter (Z), which is a temperature
ery (DRV). However, a real steady-state flow condition where the modified strain rate, defined by the equation [26]:
flow stress is constant is only reached at 1050 1C at the strain rate
of 0.01 s 1, i.e. a low Zener–Hollomon parameter (Z) condition Q def
Z ¼ e_ exp ð1Þ
(see Eq. 1 below). At the higher strain rate of 1 s 1, the flow stress RT
increases with strain indicating dislocation storage in the micro-
where e_ is the strain rate, Q def the activation energy for deforma-
structure, particularly at 950 1C. This indicates that the deforma-
tion, R the gas constant (8.3145 kJ/mol), and T the deformation
tion mechanisms operating are different under low and high Z
temperature (K). Constitutive equations based on Z can be applied
conditions. The high Z condition is not sufficient for DRV to
not only on homogeneous materials but also on multi-phase
overcome the hardening produced by dislocation storage in the
materials such as functionally graded materials [27].
microstructure, which is observed as work hardening and conse-
The relationship between Z and the flow stress can be
quently as higher flow stress. Since the stored energy of deforma-
expressed by different experimental equations, such as 2–4; i.e.
tion consists of the energy of dislocations and point defects, such
the power function, the exponential function and the hyperbolic
as vacancies, created during the deformation [3], higher amount
sine function, respectively.
of work hardening leads to higher amount of stored energy. The
low Z condition is favorable for DRV, and therefore the flow stress
Q def 0
curves can reach a steady state. Z ¼ e_ exp ¼ A0 snc ð2Þ
RT
In the instance of dynamic recrystallization (DRX), the flow
stress curves typically exhibit a single maximum, which is
Q def
followed by a softening stage until eventually, a steady stage in Z ¼ e_ exp ¼ A00 expðbsÞ ð3Þ
RT
the flow stress is reached. This is also typical of continuous
dynamic recrystallization (CDRX) [25]. However, it can be seen
from Fig. 1 that there are no such signs of DRX in the flow stress Q def
Z ¼ e_ exp ¼ A½sinhðasÞnc ð4Þ
curves. RT
4 S.V. Mehtonen et al. / Materials Science & Engineering A 571 (2013) 1–12
where A0 , A00 , A, nc, n0c, b and a are material constants. a is a stress Table 2
multiplier and an adjustable constant which brings as into the The calculated values for n0c, b, a, and nc at strains of 0.1–0.35.
right range, and can be described as
True strain Power law Exponential law Hyperbolic sine law
b
a ð5Þ nc0 b a nc
n0c
The power function (Eq. 2) is used for lower stress values than 0.1 5.504 0.122 0.022 3.959
0.15 5.070 0.115 0.023 3.770
the exponential function (Eq. 3), whereas the hyperbolic sine
0.2 4.934 0.109 0.022 3.673
function (Eq. 4) can be applied through the whole stress range [28]. 0.25 4.899 0.105 0.021 3.637
The peak stress sp , e.g. [29] or sometimes the steady state 0.3 4.828 0.101 0.021 3.587
stress sss , e.g. [30] is used in defining the constitutive equations 0.35 4.835 0.101 0.021 3.585
and for calculating the deformation activation energy, especially Average 5.012 0.109 0.022 3.702
shows that the values for n0c, b and nc can be obtained by plotting ln e_
vs. ln se , lne_ vs. se , and lne_ vs. ln sinhðase Þ , respectively. We have:
@lne_
n0c ¼ ð9Þ
@lnse T
Fig. 3. The plot used for calculating Qdef at 0.2 strain using the hyperbolic sine law.
@lne_
b¼ ð10Þ
@se T
Table 3
@lne_ The calculated Qdef as a function of strain.
nc ¼ ð11Þ
@ln½sinhðase Þ T
Power law Qdef Exponential law Qdef Hyperbolic sine law Qdef
The plot used for determining nc at the strain of 0.2 are shown in Strain
[kJ/mol] [kJ/mol] [kJ/mol]
Fig. 2. s0:2 represents the measured true stress at the true strain of
0.2. An average value for a was calculated to be 0.022 using Eq. 5. The 0.1 417.956 390.824 392.076
0.15 387.461 382.116 385.750
values for n0c, b and nc at different strains are presented in Table 2.
0.2 393.318 387.564 390.687
The activation energy for deformation can be calculated using 0.25 405.465 392.333 399.982
plots (in Fig. 3 for hyperbolic sine equation) together with the 0.3 407.447 390.628 400.826
Eqs. 12–13 for the power equation, exponential equation, and the 0.35 418.931 404.959 412.287
Average 405 391 397
Fig. 4. The plot of lnZ vs. ln s (power law). During hot deformation, the strain rate is maintained constant
while the stress value needed to achieve this is being measured.
At each value of strain, flow curves are in different stages of
deformation and may feel different deformation or softening
mechanisms. The variation of flow stress as a function of strain
was incorporated into the constitutive equations by Slooff et al.
[36] by adding a strain-dependent parameter. The method has
been later used successfully by many authors, e.g. [37–40]. Fig. 7
shows the parameters of the constitutive equations as a function
of strain and some variation can be seen. In the current study a
linear fit (Eq. 15) was imposed on the parameters of the
constitutive equation (Fig. 7).
a ¼ 0:02330:0073e
nc ¼ 4:12261:4414e
Q def ¼ 376:93 þ 88:903e
ln A ¼ 32:823 þ 8:0137e ð15Þ
Fig. 6. Plot of lnZ vs. ln½sinhðasÞ (hyperbolic sine law with a ¼0.022).
the best fit, i.e. the highest value for the correlation coefficient R2
(Fig. 6).
The values for Qdef for ferrite given in the literature are quite
scattered. The present value of 397 kJ/mol is in line with the Fig. 7. Variation of Qdef, ln A, nc and a as a function of strain.
6 S.V. Mehtonen et al. / Materials Science & Engineering A 571 (2013) 1–12
Fig. 8. Comparison between the measured and predicted flow stress considering the strain compensation in the constitutive equation at (a) 950 1C, (b) 1000 1C and
(c) 1050 1C.
Fig. 10. Dynamic microstructure evolution at 950–1050 1C at strain rates of 0.01–1 s 1 (0.4 strain). The white and yellow lines represent small angle grain boundaries with
misorientation of 21–51 and 51–151, respectively. The black colored boundaries have the misorientation greater than 151. New dynamically formed grains at 1000 1C are
pointed out by yellow arrows. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)
Fig. 12. Dynamic microstructure evolution at 950 1C at (a) 1 s 1 and (b) 0.01 s 1 (0.4 strain). The white and yellow lines represent low-angle grain boundaries with
misorientation of 21–51 and 51–151, respectively. The black colored boundaries have the misorientation greater than 151. (For interpretation of the references to color in
this figure legend, the reader is referred to the web version of this article.)
Table 4. The Avrami exponent provides information about the stainless steel, in which n depended on the fraction recrystallized:
nucleation mechanism in the recrystallization event. It is gener- when the recrystallized fraction was below 70%, n was 2.85,
ally independent of temperature, but here some variation of n is whereas for recrystallized fraction exceeding 70%, n was 1.03. The
seen in the Table 4, presumably reflecting the contribution of limit of 70%, where the recrystallization rate slowed down, is
recovery in softening by reducing the driving force for recrystal- substantially lower than the 95% observed here and e.g. by
lization. Particularly at 950 1C, n is smaller than at higher Sinclair et al. [46]. However, it was concluded that the banded
temperatures, although values as low as 0.9 have been reported austenite present in the structure of the AISI430 was a reason to
[45] for dynamically recovered a-iron. However, a typical value retard the SRX kinetics [32].
for n in dynamically recovered material would be 2 [45]. Complex recrystallization kinetics of ferrite in an IF steel was
The dependence of t 0:5 on the deformation temperature is also observed by Akbari et al. [47]. In fact, in their study, SRX
presented in Fig. 17. The value for the apparent activation energy ceased after reaching a certain recrystallized fraction. The critical
for recrystallization Qapp determined from this data is 221 kJ/mol, fraction was found to be dependent on the deformation tempera-
which is slightly lower than the 280 kJ/mol reported for a-iron [33]. ture, varying between 500 and 800 1C after 50% of deformation:
The last 5% fraction of the grains seemed to recrystallize more the lower the deformation temperature the higher the recrystal-
slowly than expected from the Avrami fits (see Fig. 16). This lized fraction achieved. The authors concluded that this behavior
‘‘sluggish’’ recrystallization in ferritic stainless steels has also was caused by precipitation interacting with the recrystallization.
been noticed by Sinclair et al. [46], who concluded that it was Precipitation might have retarded the recrystallization kinetics
caused by heterogeneity in the microstructure and texture, which also in the present study, since the investigated steel is highly
was ultimately a result of two different types of recovered grains. alloyed with precipitate forming elements. Because of the stabi-
Also small precipitates were found to play a major role by lization, at least TiN and NbC precipitates are present in the
affecting the movement of grain boundaries through Zener drag microstructure. Further, other precipitates, such as chromium
and ultimately cause the ‘‘sluggish’’ recrystallization behavior carbides, might have formed during the deformation and holding
towards the end of the recrystallization. The first type of recov- periods and thereby affected the recrystallization kinetics.
ered grain had a heterogeneous subgrain structure, but the grain The recrystallization rate is generally strongly dependent on
type was prone to abnormal subgrain growth. The abnormally the degree of deformation. Here, the effect of strain is shown in
large subgrains were able to act as nuclei for static recrystalliza- Fig. 18 revealing that the recrystallization rate is faster (t 0:5 ¼ 34 s)
tion (SRX). The second grain type had generally a larger subgrain at 0.4 strain compared to that at 0.2 strain (t 0:5 ¼ 109 s). However,
size and lower misorientation spread within the grain but the there is no accelerating effect between strains 0.4 and 0.6,
substructure was not able to form large subgrains suitable for indicating that no more deformation is stored beyond 0.4 strain
recrystallization nuclei. This type of mechanisms could explain at 1000 1C, which is in line with the observation of Akbari et al.
the slowing down of the recrystallization rate also observed here, [47] that in the ferrite region of an IF steel the strain had an
since the heterogeneity of substructure between grains was accelerating effect on the SRX kinetics but only to a certain point.
present in the current study as well (see Fig. 12). The amount of Glover and Sellars noted [45] that in a-iron, the SRX rate is
substructure and the size and location of subgrains varied independent of strain in the ‘‘steady-state’’ region of the flow
between the grains, which could be due to the different orienta- curve. However, at low strains, where work hardening occurs, the
tion of the grains regarding the direction of deformation. Because accelerating effect is very strong. Further, it has been proposed
the test specimens used in the present work were axisymmetric that the strain exponent is constant at low strain values, but
and hence no rolling direction existed in the deformation, the decreases when the strain approaches the critical strain for the
effect of grain orientation and texture on the deformation and initiation of DRX [48]. The lack of an accelerating effect of strain
restoration mechanisms could not be verified. However, it is likely could be because strong DRV prevents dislocation storage in the
that grain orientations play a significant role in explaining the microstructure such that increasing strain in the ‘‘steady-state’’
different substructures observed. Also it is known that the region does not increase the driving force for recrystallization.
CDRX kinetics is strongly dependent on the crystallographic The power of strain, p in Eq. (18), on t 0:5 between the strains of
orientation [4]. Hinton and Beynon [32] proposed the possibility 0.2 and 0.4 was calculated to be 1.7, which is significantly
of two different recrystallization kinetics for AISI 430 ferritic smaller than values previously proposed for austenitic steels;
3.81 to 3.55 [49], 4 [48] and 2.2 [50].
Fig. 18. The effect of strain on the SRX rate at 1 s 1 at 1000 1C, and the corresponding SEM-EBSD maps of the partly recrystallized microstructures: (a) 0.6 strain, 10 s
holding, (b) 0.6 strain, 30 s holding, (c) 0.4 strain, 30 s holding, (d) 0.4 strain, 180 s holding and (e) 0.2 strain, 120 s holding.
The recrystallized grains appeared first at the original grain in flow stress curves because of extensive dynamic recovery
boundaries, which is the site where the dynamically formed new and continuous dynamic recrystallization. At high Zener–
grains were mainly detected (Figs. 10 and 13). Further, in order Hollomon parameter, work hardening continued up to max-
for the nucleus to be able to grow, it must have a high-angle grain imum strains of 0.4–0.6 used.
boundary, which in many cases was formed dynamically during 2. Under low Zener–Hollomon parameter deformation condi-
the deformation. Hence, it is likely that the dynamically formed tions, the formation of new grains by continuous dynamic
small grains grew statically during the holding period. recrystallization was detected but without a drop in the flow
Increasing the degree of deformation beyond the strain of stress level, presumably due to the small fraction of dynami-
0.4 is not likely to promote SRX kinetics because of the intense cally formed grains in the microstructure.
DRV as shown above. In order to promote SRX after hot deforma- 3. Under high Zener–Hollomon parameter deformation condi-
tion, the amount of stored energy in the microstructure should be tions, microstructures were dynamically recovered, but no
increased so that the driving force for SRX would be as high as dynamic formation of new grains occurred.
possible. This can be achieved by using deformation conditions 4. The parameters of the constitutive equation for deformation
not favorable for DRV, i.e. low deformation temperature and high varied as a function of strain and therefore the effect of strain
strain rate followed by annealing at a higher temperature. was incorporated in the constitutive equation. The strain
Increasing the degree of deformation would, however, result in modified constitutive equation was successfully used for pre-
smaller recrystallized grain size as was the case after 0.6 strain: dicting the flow stress.
the SRX rate was not accelerated from that of after 0.4 strain but 5. The average activation energy for deformation, Qdef, was
the higher strain resulted in smaller recrystallized grain size. determined to be 397 kJ/mol and the apparent activation
energy for static recrystallization, Qapp, 221 kJ/mol.
6. The rate of static recrystallization was increased by increasing
4. Summary strain up to 0.4, but beyond this value the rate of recrystalliza-
tion remained unchanged. Increasing the strain to 0.6 did,
The hot deformation behavior at different temperatures (950– however, lead to finer recrystallized grain size when hardly
1050 1C) and strain rates (0.01–1 s 1) of a stabilized 21Cr ferritic any refinement of grain size was to be achieved after straining
stainless steel has been studied. Because of the composition, the to 0.2 or 0.4.
investigated steel is in ferritic state in the hot working tempera- 7. In order to promote static recrystallization after hot deforma-
ture range. The results can be summarized as follows: tion, the stored energy in the microstructure, i.e. the driving
force for static recrystallization, should be increased. This can
be achieved by using deformation conditions, which are
1. Under low Zener–Hollomon parameter deformation condi- unfavorable for dynamic recovery, i.e. low deformation
tions, no work hardening was seen above the strain of 0.05 temperature and high strain rate. Carrying out the subsequent
12 S.V. Mehtonen et al. / Materials Science & Engineering A 571 (2013) 1–12
annealing at a higher temperature than the deformation would [19] P. Gay, P.B. Hirsch, A. Kelly, Acta Metall. 1 (1953) 315–319.
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The financial support from the Finnish Funding Agency for
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by the Academy of Finland through the Graduate School on
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