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1 s2.0 S0264127516303902 Main PDF
1 s2.0 S0264127516303902 Main PDF
a r t i c l e
i n f o
Article history:
Received 10 December 2015
Received in revised form 10 January 2016
Accepted 19 March 2016
Available online 24 March 2016
Keywords:
Interstitial free steel
Thermomechanical simulation
Critical temperatures
Multiaxial forging
Mechanical properties
Transmission electron microscopy (TEM)
a b s t r a c t
In the present study, evolution of microstructure during multiaxial forging (MAF) of a NbTi stabilized IF steel
and its mechanical properties have been investigated. The forging schedule was designed on the basis of critical
temperatures Ar3, Ar1 (evaluated from dilatometric curve through thermomechanical simulator) and recrystallization stop temperature, Tnr (determined from Boratto equation). MAF was performed for 5 cycles in 3 different
phase regimes; in pure -region (1050 C), transformation zone (800 C) and pure -region (650 C). The
deformed samples were cooled by normal air cooling. EBSD and optical microscopy investigation conrmed the
formation of ne ferrite grains (~5 m) due to strain induced transformation of unstable at 800 C and ultrane
ferrites (~1 m) through subgrains formation at pure -ferritic region at 650 C. The specimen forged in pure region showed a 4-fold improvement of yield strength (YS) compared to that of the starting material (141 MPa)
without much interfering its ductility (25%). This is ascertained to the development of bimodal grain structures
and formation of ultrane carbide precipitates which were conrmed by EBSD and TEM analysis. The theoretical
YS was estimated through analysis of different strengthening mechanisms and found to be highly corroborated
with the experimentally obtained result.
2016 Elsevier Ltd. All rights reserved.
1. Introduction
Interstitial free (IF) steels are widely used in applications starting
from automotive body parts to electronic components as well as enamel
wares to house hold appliances and structural industries due to their
wide range of mechanical properties and high formability [1,2]. The
major drawback of these steels is the low level of yield strength.
Capdevila et al. [3] explained that IF steels have interstitial-free bcc ferrite matrix which results low yield strength and high strain rate sensitivity. Various research groups throughout the world are trying to
improve the mechanical strength without much affecting their formability and/or ductility. Various mechanisms are proposed for the occurrence of grain renement during thermomechanical deformation
depending on the material and processing methods and temperatures
employed. Lim et al. [4] performed multiaxial compression studies on
-FeC alloy at room temperature. The grain renement was explained
on the basis of intersection of micro-bands formed due to strain localization leading to formation of subgrains. These subgrains subsequently
rotated to form ultra ne crystallites. The formation of substructures
due to multiaxial forging (MAF) of a HSLA steel was reported to be generally of equiaxed bounded by high angle boundaries [5]. Deep
Corresponding author.
E-mail address: sumit.rkvm@gmail.com (S. Ghosh).
1
1st and 2nd authors have equal contribution.
http://dx.doi.org/10.1016/j.matdes.2016.03.107
0264-1275/ 2016 Elsevier Ltd. All rights reserved.
48
that case the total elongation is reported to be very poor, e.g., only
7.5% [1]. To the best of our knowledge, hardly any literature is available on the effect of different critical temperatures on the thermomechanical behavior (i.e. on MAF) of IF steel. Therefore, aim of the
present work is to investigate the inuence of MAF processing parameters on the microstructures and mechanical properties of a
NbTi stabilized IF steel deformed in pure -region, transition
region and pure -phase regime. And also examine the possibilities
of achieving high YS with signicance ductility, moderate YS with
good ductility etc. by simple MAF which is industrially reliable. In
the current investigation, the microstructural evolution due to MAF
at different critical regions and quantitative results were studied in
detail by light microscopy, EBSD and TEM. The accumulated dislocation densities were calculated using X-ray diffraction line prole
analysis (XRDLPA) to explain the strengthening mechanisms. The effect of temperature and strain hardening exponent on deformation
behavior were also investigated to correlate the YS and uniform
elongation. The YS obtained through analysis of strengthening
mechanisms is discussed in detail and the same was correlated
with that of the experimentally obtained results. A quantitative
fractography analysis was also carried out to correlate % elongation
of the respective samples.
p
p
Tnr 887 464C 6445Nb644 Nb 732V230 V 890Ti
363Al357Si
The samples were rst homogenized at temperature of 1200 C for
1 h and then cooled down to the forging temperature within the furnace. The MAF were performed in a Birson friction screw press at
~ 1050, ~ 800 and ~ 650 C. Graphite powder mixed with acetone was
used for the lubrication during the forging to cause relatively better homogeneous deformation. The samples were held in the furnace at the
particular temperature at least for 10 min to achieve the forging temperature after the each pass. The MAF was performed at a strain rate
of about 10 s1 and an equivalent total true strain of 6 (0.4 15; 15
passes for 5 cycles) was maintained for each sample. After completion
of the forging operation (5 cycles = 15 passes) each forged sample
was air cooled to room temperature. The microstructural analysis was
performed using optical microscopy (Leica DMI 5000M), FE-SEM,
EBSD and transmission electron microscopy (TEM). EBSD analysis was
performed using FEI-Quanta 200FE-SEM equipped with the TSL data acquisition system. For EBSD analysis, specimens were mechanically
polished up to ne cloth using colloidal silica followed by electro
polished in an electrolyte of 20% perchloric acid in methanol at
40 C using 21 V for 50 s. The EBSD scans were performed on electrochemically polished samples with a step size of 0.5 m and subsequent
analysis was performed using TSL-OIM software. To study the dislocation density in MAFed specimens, X-ray diffraction (XRD) study was
carried out at scan rate of 0.5/min using Cu K radiation (1.5409 A)
in a Bruker AXS D8 Advance instrument. The transmission electron microscope (FEI Technai 20 G2S-Twin) was operated at 200 kV. The samples for TEM analysis were prepared by thinning down the thickness to
~ 100 m through grinding on silicon carbide coated emery papers of
Table 1
Chemical composition (wt.%) of the IF steel obtained by optical emission spectroscopy analysis.
Element
Mn
Si
Al
Cu
Ni
Nb
Ti
Fe
wt.%
0.005
0.52
0.005
0.02
0.009
0.048
0.013
0.01
0.016
0.05
0.006
99.3
Fig. 2. Dilatometry curve for TiNb microalloyed steel obtained through Gleeble-3800.
800, 1200, 1500 grit size. The samples of 3 mm diameter disc were
punched out from this thin foil. The disc samples were electropolished using a FEI twin jet electro polisher in a solution of 90% methanol + 10% perchloric acid kept at 20 C temperature. The electropolishing was carried out at 40 V.
The hardness measurements were performed using a Vickers hardness tester (FIEVM50 PC) with an applied load of 10 kg for a dwell
time of 30 s. The tensile tests were conducted on ASTM E8 sub-size specimens (10 mm gauge length, 3 mm width and 2 mm thickness). The
tests were carried out at a constant strain rate of 5 104 s1 using a
H25 K-S Tinius Olsen machine. In each case, at least 3 samples were tested to verify the reproducibility of the results. The fractured surface of
the tensile specimens was analyzed using a scanning electron microscope (ZEISS, 51-ADD0048) at an operating voltage of 15 kV to determine the mode of failure under uniaxial tensile loading.
3. Results and discussion
3.1. Microstructural investigation
The optical microstructure of as-cast specimen is shown in Fig. 3a.
The cast inhomogeneous microstructure consists of different size ferrite
grains; proeutectoid smaller size ferrites as the main micro-constituents
along with larger size ferrites. No pearlite is present in the microstructure as the C content is very less (0.005%). The annealing treatment
was carried out at 1200 C for 1 h to obtain uniform initial grains. The
optical microstructure of the homogenizing annealed steel (hence onwards called as starting material) is shown in Fig. 3b. The annealing
treatment led to the formation of coarse grained ferrites as compared
49
to the cast structure. The average grain size is measured by line intercept method and the average grain size of the as-cast and starting material samples are 210 and 260 m, respectively. During the homogenizing
annealing, all alloying elements are dissolved in austenite grains and
new austenite grains are developed. During cooling, pro-eutectoid ferrite nucleated at the austenite grain boundaries at Ar3 temperature
and grew further to reach room temperature. Alloying elements are
likely to precipitate out in the form of carbides during cooling.
Earlier in the Experimental section, we have already mentioned that
the recrystallization stop temperature of the present steel was estimated to be ~ 1000 C, and critical temperatures Ar1 (701 C) and Ar3
(860 C) were obtained from dilatometric analysis. On the basis of the
above critical temperatures, the starting material samples were deformed by multi-axial forging for 5 cycles at 3 different temperatures:
at 1050 C (recrystallization region, ), 800 C ( transition region)
and 650 C (pure region). In each case the deformed specimen was
cooled down to room temperature by normal air cooling. Initially, the
samples were homogenized for 1 h at 1200 C, and then, multi-axial
forging (MAF) were carried out maintaining a constant temperature of
1050 C. After rst cycle of forging, the sample was kept in the furnace
to attain a temperature of 1050 C before proceeding to next cycle of
forging. Thus, grain renement is promoted in each pass by repeated deformation of recrystallized austenite grains. Finally, a recrystallized
small size austenite grains structure is produced by MAF at 1050 C
( region) from the deformed austenite grains. After deformation
when normal air cooling was employed, the pro-eutectoid ferrites
were nucleated along recrystallized austenite grain boundaries at
around Ar3, and complete ferritic transformation took place at room
temperature (C = 0.005%). Thus, the room temperature microstructure
of the specimen deformed in -region consists of equi-axed ferrites
(Fig. 4a) with an average grain size of ~ 35 m (as shown in Fig. 4b).
Cuddy et al. [15] also found uniform equi-axed ferritepearlite microstructure in low carbon Nb microalloyed steel after hot rolling at
above recrystallization temperature followed by air cooling. The grain
growth of the pro-eutectoid ferrites are expected to take place during
the cooling process after forging. As stated by Yang et al. [16], coarsening
of the austenite grains is expected to be hindered during the period of
intermittent heating because of the presence of ne carbide and/or nitrides precipitates. Arribas et al. [17] showed that the presence of ne
TiN particles inhibits grain growth of austenites during inter-pass
delay times and maintained a ne recrystallized austenite grains structure. Hu et al. [18] demonstrated that the inhibiting the grain growth
may also be attributed to the solute drag effect promoted by Nb in
solid solution. Gong et al. [19] recently investigated the dissolution kinetics of NbC and (Ti, Nb)C in HSLA steels during holding period at
1200 C of the hot rolled steel (850 C). They reported that rate of austenite grain coarsening was less for the NbTi steel than that of the Nb
steel because of the high temperature stability of (Ti, Nb)C. By
thermomechanical control processing, Zhang et al. [20] reported to develop a high strength re resistant steel having high Nb and low Mo. The
Fig. 3. Optical microstructure of IF steel: (a) as cast sample (b) annealed at 1200 C.
50
cell walls are regions of high free energy and become sites for ferrite nucleation, and thus lead to strain-induced transformation of the unstable
austenite. Analogous to the microstructural evolution observed by Junior et al. [21], it is suggested that the transformation occurs
with the ferrite nucleation sites in the remaining austenite grains.
Thus, the application of large deformation tends to: (i) enhance
transformation; and (ii) activate dynamic phenomena such as dynamic
recrystallization and strain-induced dynamic phase transformation. As a
result, MAF of IF steel in this region followed by air cooling formed a ne
equiaxed ferrite grains (~5 m).
The maximum grain renement was obtained when the thermomechanical treatment was carried out in the pure ferritic region at 650 C
(below Ar1). Room temperature microstructure is composed of two
kinds of ferrite grains: approximately 70% of the grains having an average size ~2527 m and 30% of the grains (subgrains) with an average
size of ~ 13 m (as shown in Fig. 4g). When the coarse ferrite grains
are repeatedly deformed, they get strain hardened and nally recovered
Fig. 4. Optical microstructure after (a) ve cycle MAF at 1050 C. (b) Corresponding average grin size distribution. (c) Optical microstructure after ve cycle MAF at 800 C.
(d) Corresponding EBSD image with average grain size distribution. (e) and (f) Grain boundary misorientation prole. (g) Optical microstructure after ve cycle MAF at 650 C. (hi)
Corresponding EBSD image with average grain size distribution. (j) and (k) Grain boundary misorientation prole. (UFF ultrane ferrites; FF ne ferrites).
51
Fig. 4 (continued).
microstructure. In addition, due to the presence of micro-alloying elements, such as Nb and Ti in the present steel, high density dislocations
produced during the MAF are favorable for nucleation sites of Nb/Ticarbonitride precipitates [25]. These precipitates also play an important
role in the microstructural renement during thermomechanical [26].
At high temperature, the dislocations produced during MAF undergo a
recovery process associated with dislocation movement and absorption.
This leads to the formation of low density dislocations in the microstructure and form larger size recrystallized grains.
EBSD analysis has been carried out for the two selected samples;
MAFed at transition zone and pure -region, which showed signicantly rened microstructures after 5 cycles of forging. The EBSD inverse pole gure map and superimposed grain boundary map of both
the specimens revealed a severely deformed equiaxed ne grain structure, as shown in Fig. 4d and h, respectively. Fine ferrite grains embedded within the larger size ferrites regions can be visible from the EBSD
image (Fig. 4d and h). The grain colors are determined by the orientation of each grain as shown in the inset unit triangle of the gures.
The orientation image microstructure in the specimen deformed in
52
identied from the TEM micrographs, as one is shown in Fig. 5d. The formation of micro-shear bands in various directions is due to the change
in the strain paths during MAF in -ferritic region.
3.2. Mechanical properties
The mechanical properties of the MAFed samples were evaluated by
Vickers hardness measurements and tensile tests, and these are compared with those of the as-cast and starting material (annealed) specimens. Vickers hardness measurements of the samples processed at
different conditions (Fig. 6) were carried out to correlate YS of the
MAFed samples, and the comparative results are shown in Table 2.
The average hardness value of the annealed sample is only 0.68 GPa.
And the hardness values increased rapidly due to straining during
MAF at different critical temperature zones. There is 2 fold increases in
the hardness value (1.39 GPa) when MAF was carried at 1050 C. The
hardness value further enhanced when MAF was done at lower temperatures i.e. below Ar3 (at 800 C) and pure ferritic region (650 C). The
maximum hardness was measured to be 1.91 GPa for the samples
forged at 650 C. This is an ~ 2.8 times higher when compared to that
of the starting material sample. Increase in the hardness is mainly due
to the renement of the ferrite grains continuously with decreasing
the processing temperature. It is well-known that the hardness is proportional to the YS of an engineering structural material [28]. Analysis
of the improvement of the YS is discussed in the relevant section (in
the stress-strain plot).
The engineering stress-strain curves of the as-cast, annealed starting
material and MAFed specimens are shown in Fig. 7. Compared to the mechanical strength of the as-cast sample (YS = 165 MPa, UTS = 280 MPa),
Fig. 5. (a) TEM bright eld image of dislocation structure of MAFed specimens at 650 C, (b) SADP spot pattern of NbC from [111] zone axis and ring pattern from the background ne ferrite
matrix, (c) TEM dark eld image, recorded from the diffracted beam from the spot as encircled (sky colour) in Fig. 4b, (d) micro-shear bands formation in various directions.
53
the annealed sample showed slight less YS and UTS (YS = 141 MPa,
UTS = 256 MPa) with a corresponding increase (~12%) in the ductility.
The tensile ductility of the annealed sample was estimated to be ~46%,
while the ductility of the as-cast specimen was 34%. The reduced YS
and improved elongation % of the starting material are attributed to the
formation of comparatively larger size grains (~260 m; Fig. 3b) than
that of the as-cast structure (210 m; Fig. 3a).
The YS and UTS (Fig. 7) of the specimen forged at -recrystallized region found to increase to 435 and 473 MPa, respectively, as compared to
that of the homogenized annealed specimen (YS = 141 MPa, UTS =
256 MPa). The corresponding YS and UTS further improved to 466 and
496 MPa, respectively, after MAFed at austenite-ferrite ( ) transition region (just below Ar3 region) followed by cooling under same conditions. The specimen MAFed in pure ferritic region showed the
maximum enhancement of the YS and UTS, and the corresponding
values are 601 and 628 MPa, respectively. It can be observed that the enhanced YS, 601 MPa, is N4 times than that of the starting annealed material (141 MPa). It can also be noticed (from Fig. 7) that the YS and UTS
of the MAFed specimens in 3 specic phase regions increased with
slight expense of the ductility. The ductility of the recrystallized controlled MAFed specimen decreased to ~ 31%, which corresponds to an
average grain size of ~35 m (Fig. 4a). The specimen forged in transition
region showed a ductility ~28%, which corresponds to ferrite grain size
of ~5 m embedded with larger size ferrites of ~32 (Fig. 4c-d). The specimen rolled in pure ferritic region showed a total elongation of ~ 25%.
We have already described earlier that the microstructure of the specimens deformed at the pure ferritic region comprised of 2 types of grains
(Fig. 4g-h); ultrane ferrite grains (30%, ~13 m size), large size ferrites (70%, ~ 2527 m). Therefore, it can be observed that the YS of
the air cooled specimens is signicantly improved without much affecting the ductility, especially when forged in pure ferritic phase regime.
This is mainly due to 2 reasons: (i) extensive grain renement and (ii)
dual size grain distribution obtained by MAF in this region. It is known
that the grain renement is a fundamental strategy to enhance YS of
metallic materials without much sacricing their ductility [26]. Therefore, improvement of the YS is due to the formation of ner ferrite grains
and the large size grains are responsible for retaining the ductility. Bodin
et al. [29] also observed the formation bimodal distribution of ferrite
grains in CMn steel (0.1C, 0.5Mn, 0.0045N) after intercritical rolling
within (825775) C. They also found an improvement of the YS while
retaining the ductility almost same. Gao et al. [30] reported an improvement of YS and formability of 17% Cr ferritic stainless steel due to the
Table 2
The mechanical properties of the homogenized annealed and multi-axially forged IF steel specimens in different critical zones.
Forging temperature (C)
YS (MPa)
UTS (MPa)
Elongation (%)
1050
800
650
Annealed sample
As cast sample
435 5
466 4
601 6
141 3
165 4
473 3
496 7
627 8
256 5
281 3
30.44 1.5
27.55 1
25 1.5
46 1.7
34 1.5
0.126
0.11
0.086
0.254
0.207
54
r
2obs 2i
where, obs and i, respectively, are the integral breadth of the corresponding hkl reection at the full width at half intensity maxima
(FWHM) of the forged specimen and standard Al2O3.
Therefore, r is the total broadening due to the crystallite size and
lattice microstrain. The crystallite size and lattice microstrain have
been estimated from the analysis of 3 peaks of each specimen by
using the plot between Brcos vs. sin as per WilliamsonHall technique
[35]. The dislocation density (d) can be estimated from the following
equation [36] using the average crystallite size (D) and lattice
microstrain () as follows:
1
p
2 2
d 2 3
Db
p .
3
where a = 0.28664 nm [28]. Table 3 shows the detailed values of crystallite size, lattice microstrain and dislocation density, theoretical and
experimentally obtained YS of the forged samples.
It can be noticed that the average lattice microstrain increased from
2.71 103 for the specimen forged -region (1050 C) to 4.33 103
corresponding to the specimen forged at 650 C in single phase region. Correspondingly, the dislocation density, d, found to increase
from 3.97 1014 m2 to 8.15 1014 m2. Using the same technique,
Sarkar et al. [37] also calculated the dislocation density of a single and
4 passes ECAPed specimens (at room temperature) of an IF steel and
Taylor 0 MGbhi1=2
Fig. 8. (a) X-ray diffraction pattern of the MAFed IF steel specimen in different processing conditions showing peak broadening. (b) Magnifying view of peak broadening for 110 reection.
55
Table 3
Crystallite size, microstrain and dislocation density values, theoretical and experimentally obtained yield strength for IF steel MAFed at different conditions.
Processing conditions
Dislocation (m2)
Taylor (MPa)
y (MPa)
82.03
69.05
46.22
2.71
3.67
4.33
3.97 1014
4.72 1014
8.15 1014
439
471
609
435
466
601
which is equivalent to grain size for ultrane structure. As we have earlier mentioned that the improvement of the YS is due to the grain size
renement, dislocation strengthening and precipitation hardening.
While, the Taylor's equation does not consider the contribution of the
YS from the precipitation strengthening. Therefore, the theoretical YS
practically would have been much higher if all the strengthening contributions were considered. Also for the theoretical calculations, the material is always assumed to be isotropic with respect to all strengthening
mechanisms. But in the practical material, always some defects are
present and it is anisotropic in nature in that sense. Therefore, experimental YS always should be lower than that of the theoretical YS if all
the strengthening components are included in the strength estimation.
So, it can be concluded that the theoretical YS of the present material
would have been much higher than that of the experimentally obtained
values after considering the contribution from the precipitation
strengthening.
Fig. 9. Variation of YS and Uniform elongation (UE) with strain hardening exponent.
56
Fig. 10. SEM fractographs of tensile test specimen: (a) as-cast, (b) annealed, (ce) ve cycles MAF at 1050, 800 and 650 C, respectively.
obtained in the annealed specimen. The average dimple size has been
compared to the % elongation of the respective sample processed
under different conditions (Fig. 11). Initially, both the dimple size and
4. Conclusions
Fig. 11. The average dimple size vs. % elongation of the respective sample processed under
different conditions.
cooling. On the basis of the results and their analysis, the following conclusions can be ascertained:
(1) The grain renement mechanisms are found to be inuenced by
the deformation temperatures in the 3 different phase regimes.
Grain renement during MAF at -region (1050 C) is promoted
by continuous dynamic recrystallization of deformed austenite
grains and formed ne equiaxed ferrite grains (~35 m) on normal cooling. On the other hand, formation of ne ferrite grains
(~5 m) is attributed to the strain induced transformation of unstable during MAF in transformation zone (800 C). The
ultrane ferrite grains formation (~1 m) in pure ferritic region
(650 C) occurs through subgrains formation by deformation induced ferrite transformation (DIFT).
(2) The maximum renement of grains was achieved when the specimen forged in pure ferritic region. This is attributed to the development of micro-shear bands in multiple directions, repeated
change in the accumulated strain paths to promote dislocation
activity, increase in the misorientation angles of grain boundaries
and DIFT. This has been conrmed by detailed EBSD study and
TEM investigation.
(3) Multiaxially forged sample at pure ferritic state (650 C) shows
highest value of mechanical properties (YS-601 MPa and UTS628 MPa) without much interfering the total elongation (25%)
compared to the other two cases. The improvement of the YS simultaneously with retaining high ductility is accomplished to the
fact of bimodal grain structure obtained by MAF in this region.
The ne size ferrites (average size ~ 13 m) is accountable for
the high YS, while the comparatively larger size ferrite grains
(average size ~2527 m) liable for the retained ductility.
(4) The improvement in the mechanical properties along with high
ductility can be enlightened to the presence of special features
in the microstructure such as ultrane precipitates of TiC and/
or NbC in ferrite matrix, which has been conrmed by TEM study.
Acknowledgement
The authors are highly acknowledged the TATA Steel, Jamshedpur
for providing the steel for the research purposes and Indian Institute
of Technology Roorkee for providing the research facilities to carry out
the work.
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