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Effect of critical temperatures on microstructures and mechanical properties of

Nb–Ti stabilized IF steel processed by multiaxial forging

Article  in  Materials & Design · June 2016

DOI: 10.1016/j.matdes.2016.03.107

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Effect of critical temperatures on microstructures and mechanical properties
of Nb–Ti stabilized IF steel processed by multiaxial forging

Sumit Ghosh, Ajay Kumar Singh, Suhrit Mula

PII: S0264-1275(16)30390-2
DOI: doi: 10.1016/j.matdes.2016.03.107
Reference: JMADE 1585

To appear in:

Received date: 10 December 2015

Revised date: 10 January 2016
Accepted date: 19 March 2016

Please cite this article as: Sumit Ghosh, Ajay Kumar Singh, Suhrit Mula, Effect of
critical temperatures on microstructures and mechanical properties of Nb–Ti stabilized
IF steel processed by multiaxial forging, (2016), doi: 10.1016/j.matdes.2016.03.107

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 ACCEPTED MANUSCRIPT

Effect of critical temperatures on microstructures and mechanical properties of Nb-Ti

stabilized IF steel processed by multiaxial forging

Sumit Ghosha*, Ajay Kumar Singha, Suhrit Mulaa

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a
Department of Metallurgical and Materials Engineering, Indian Institute of Technology Rookee, Roorkee-247667,
Uttarakhand, India.
* Corresponding Author: Email: sumit.rkvm@gmail.com;

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Phone: +91-1332-285763; Fax: +91-1332-285243

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Abstract

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In the present study, evolution of microstructure during multiaxial forging (MAF) of a Nb-Ti
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
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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 γ-
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region (1050°C), γ→α transformation zone (800°C) and pure α-region (650°C). The deformed
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samples were cooled by normal air cooling. EBSD and optical microscopy investigation
confirmed the formation of fine ferrite grains (~5μm) due to strain induced transformation of
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unstable γ at 800°C and ultrafine ferrites (~1μm) through subgrains formation at pure α-ferritic
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region at 650°C. The specimen forged in pure α-region showed a 4-fold improvement of yield
strength (YS) compared to that of the starting material (141MPa) without much interfering its
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ductility (25%). This is ascertained to the development of bimodal grain structures and formation
of ultrafine carbide precipitates which were confirmed 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.

Keywords: Interstitial free steel; Thermomechanical simulation; Critical temperatures;

Multiaxial forging; Mechanical properties; Transmission electron microscopy (TEM).

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

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1st and 2nd authors have equal contribution.

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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

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without much affecting their formability and/or ductility. Various mechanisms are proposed for
the occurrence of grain refinement during thermomechanical deformation depending on the

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material and processing methods and temperatures employed. Lim et al. [4] performed multiaxial

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compression studies on α-Fe–C alloy at room temperature. The grain refinement was explained
on the basis of intersection of micro-bands formed due to strain localization leading to formation

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of subgrains. These subgrains subsequently rotated to form ultra fine crystallites. The formation
of substructures due to multiaxial forging (MAF) of a HSLA steel was reported to be generally
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of equiaxed bounded by high angle boundaries [5]. Deep drawability of P-added ferritic IF steel
was reported to improve as the finish rolling temperature decreased from 620 to 560°C [6].
Bhowmik et al. [1] stated that generation of submicron grains during MAF of IF steel lead to
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tremendous increase in the tensile strength with some loss of ductility. The formation of micro-
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voids in cryogenically rolled IF steel found to reduce YS in comparison to that obtained for the
sample rolled at ambient temperature [7]. The microstructural refinement of IF steel occurred
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monotonously with increasing the number of ECAP passes [8]. Both yield and ultimate strength
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increased with the number of passes, while the ductility lost after 1 pass was partially regained at
higher number of passes. From the above studies, it can be concluded that the grain size
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strengthening is one of the vital methods where one can expect an improvement in the
mechanical strength without much affecting its ductility.
Now a days, MAF is known to be a unique processing technique to obtain ultrafine grained
(UFG) microstructure [9]. Alexander [10] proposed that MAF exhibits certain advantages over
other processes such as ECAP or rolling, e.g. it is a simple process based on the free forging
operation. But, Kundu et al. [11] stated that the extent of work hardening is very less in the
MAF-processed materials. This is attributed to the increase in strain rate sensitivity with strain in
high strength materials. So, enhancement of the mechanical strength without much affecting the
formability is a challenging job. It can be noticed from the literature that, in most cases, the
improvement of the YS is also limited to less than 500 MPa for the thermomechanically
processed IF steels. Rarely, the YS is reported to be over 600 MPa; and in that case the total

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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 thermo-
mechanical behavior (i.e. on MAF) of IF steel. Therefore, aim of the present work is to
investigate the influence of MAF processing parameters on the microstructures and mechanical

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properties of a Nb-Ti stabilized IF steel deformed in pure γ-region, γ→α transition region and
pure α-phase regime. And also examine the possibilities of achieving high YS with significance

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ductility, moderate YS with good ductility etc. by simple MAF which is industrially reliable. In

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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

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accumulated dislocation densities were calculated using X-ray diffraction line profile analysis
(XRDLPA) to explain the strengthening mechanisms. The effect of temperature and strain
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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
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quantitative fractography analysis was also carried out to correlate % elongation of the respective
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samples.
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2 Material and experimental procedure

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The material, i.e. interstitial free (IF) steel used for the present study was supplied by TATA
Steel, Jamshedpur, India. The chemical composition obtained by optical emission spectroscopy
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(Spectrolab, Germany) analysis is given in Table1. The dimensions of the specimen used for the
multiaxial forging were in the ratio of 1.5:1.22:1.0 [12]. The samples were machined to obtain
the required size of 30mm×24.5mm×20mm. In the multiaxial forging (MAF) process, the
specimen was rotated by 90° after each pass and a uniaxial compressive true strain of ɛ ~ 0.4 was
applied to the longest side at each MAF pass. The schematic diagram shown in Fig.1 represents
to one complete cycle of MAF process.
Table 1: Chemical composition (wt.%) of the IF steel obtained by optical emission spectroscopy
analysis.
Element C Mn S P Si Al Cu Ni Nb Ti N 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

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Assuming the conservation of volume and material isotropy, this procedure enables to maintain
the initial dimensional ratio at the end of each pass [12]. In this work, the MAF performed in the
three different phase regimes, i.e. in pure γ-region (at 1050°C), γ→α transformation zone (at
800°C) and pure α-region (at 650°C). The dilatometry test was performed in the Gleeble-3800

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thermomechanical simulator to obtain the useful critical temperatures such as austenite to ferrite
start transformation temperature (Ar3) and austenite to ferrite finish transformation temperature

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(Ar1).

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Fig. 1: Schematic design of multi-axial forging for 1 cycle.

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A cylindrical shaped sample was heated up to the temperature of 1200°C at a heating rate of
5°C/sec and then the sample was cooled down to room temperature maintaining the same
cooling rate (i.e. 5°C/sec). The changes in the slope of the dilatometry curve can be observed
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during the phase transformation due to expansion/contraction of the specific volume of different
phases [13]. At the atmospheric pressure, the pure iron exists in BCC ferrite (α) crystal structure
up to <912°C and beyond this temperature, it transforms to FCC austenitic (γ) structure. During
the transformation of ferrite to austenite, the atomic volume changes by 1% [13]. The critical
temperatures, Ar3 and Ar1 obtained from the cooling curve (as shown in Fig. 2), respectively, are
860 and 701°C. Boratto et al. [14] postulated a standard equation for the calculation of Tnr
(recrystallization stop temperature). Using the Boratto equation (as shown below), the Tnr was
estimated to be ~970°C for the present steel.
Tnr = 887 + 464C + (6445Nb - 644 Nb) + (732V - 230 V) + 890Ti + 363Al - 357Si

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Fig. 2: Dilatometry curve for Ti-Nb microalloyed steel obtained through Gleeble-3800.

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The samples were first 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
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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
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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 about10 sec-1 and an
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equivalent total true strain of 6 (0.4×15; 15 passes for 5 cycles) was maintained for each sample.
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After completion of the forging operation (5 cycles = 15 passes) each forged sample was air
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cooled to room temperature. The microstructural analysis was performed using optical
microscopy (Leica DMI 5000M), FE-SEM, EBSD and transmission electron microscopy (TEM).
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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 fine 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 μm 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 Kα 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 μm through grinding on silicon carbide coated emery papers of 800, 1200,
1500 grit size. The samples of 3 mm diameter disc were punched out from this thin foil. The disc
samples were electro-polished using a FEI twin jet electro polisher in a solution of 90%
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methanol+10% perchloric acid kept at -20oC temperature. The electro-polishing was carried out
at 40V.
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

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ASTM E8 sub-size specimens (10 mm gauge length, 3 mm width and 2 mm thickness). The
testes were carried out at a constant strain rate of 5×10-4 s-1 using a H25 K-S Tinius Olsen

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machine. In each case, at least 3 samples were tested to verify the reproducibility of the results.

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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

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failure under uniaxial tensile loading.

3 Results and Discussion

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3.1 Microstructural investigation
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Fig. 3: Optical microstructure of IF steel: (a) as cast sample (b) annealed at 1200°C.

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 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 µm, respectively. During the homogenizing

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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.

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Earlier in the Experimental section, we have already mentioned that the recrystallization stop

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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

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critical temperatures, the starting material samples were deformed by multi-axial forging for 5
cycles at 3 different temperatures: at 1050°C (recrystallization region, γ), 800°C (γ→α transition

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region) and 650°C (pure α 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
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1200°C, and then, multi-axial forging (MAF) were carried out maintaining a constant
temperature of 1050°C. After first 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 refinement is
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promoted in each pass by repeated deformation of recrystallized austenite grains. Finally, a

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recrystallized small size austenite grains structure is produced by MAF at 1050°C (γ region)
from the deformed austenite grains. After deformation when normal air cooling was employed,
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the pro-eutectoid ferrites were nucleated along recrystallized austenite grain boundaries at
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around Ar3, and complete ferritic transformation took place at room temperature (C=0.005%).
Thus, the room temperature microstructure of the specimen deformed in γ-region consists of
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equi-axed ferrites (Fig. 4a) with an average grain size of ~35 μm (as shown in Fig. 4b). Cuddy et
al. [15] also found uniform equi-axed ferrite-pearlite 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 fine
carbide and/or nitrides precipitates. Arribas et al. [17] showed that the presence of fine TiN
particles inhibits grain growth of austenites during inter-pass delay times and maintained a fine
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

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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 Nb–Ti 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 fire resistant steel having high Nb and low Mo. The high

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YS at 600°C was ascertained to the formation of cementites and precipitation of complex
carbides (Nb,Mo,V)C of <10 nm size in ferritic matrix.

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During deformation in γ→α transition region (just below Ar3) at 800°C, complete

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recrystallization does not occur between the deformations passes, and the deformation strain is
retained from one pass to the next pass. The retained strain thus increases number of nucleation

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sites for γ→α transformation. Therefore, a fine ferritic grains (FF) structure is likely to form,
which is also observed in the present study as shown in Fig. 4c. The microstructure is consisted
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of FF (av. grain size of ~5 μm) embedded with larger size ferrites (av. size ~32 μm, estimated
from 300 grains by line intercept method). At the beginning of the deformation, the
microstructure is composed of mainly smaller size nucleated ferrites (just started to nucleate
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from γ→α) and retained austenites. Taking into account that austenite is a low stacking fault
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energy material, a typical dislocations substructure is formed inside the remaining austenitic
grains during deformation in this region. The dislocations cell walls are regions of high free
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energy and become sites for ferrite nucleation, and thus lead to strain-induced transformation of
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the unstable austenite. Analogous to the microstructural evolution observed by Junior et al. [21],
it is suggested that the γ→α transformation occurs with the ferrite nucleation sites in the
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remaining austenite grains. Thus, the application of large deformation tends to: (i) enhance γ→α
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 fine equiaxed ferrite grains (~5μm).
The maximum grain refinement 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
~25-27 μm and 30% of the grains (subgrains) with an average size of ~1-3 μm (as shown in Fig.
4g). When the coarse ferrite grains are repeatedly deformed, they get strain hardened and finally
recovered and recrystallized to generate new equiaxed grains. Multidirectional forging for a large
number of cycles leads to the accumulation of a large strain, which results in the formation of

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high density dislocation substructures both at the ferrite boundaries and inside the grains. These
substructures finally yield fine grained ferrites [18]. It is generally agreed that lowering the
deformation temperature can promote deformation induced ferrite transformation (DIFT) and
decrease the ferrite grain size [22]. The strain accumulation and then change in the strain path in

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all the 3 directions during MAF can introduce a large amount of micro-shear bands in various
directions. This promotes dislocations activation, accumulation and rearrangement between

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them, increase in the misorientation of grain boundaries, conversion of the low angles grain

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boundaries to high angles boundaries, and finally leads to the formation of ultra fine ferrites [23].
Development of a trimodal grains structure (large pancaked austenite, ultra-fine austenite and

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submicron ferrite grains) was achieved during deformation of a duplex low-density Fe–18Mn–
8Al–0.8C steel at 1000°C [24]. Formation of micro-shear bands followed by dynamic
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recrystallization of austenites and the DIFT reported to be the dominant mechanisms for the
formation of the trimodal 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
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MAF are favorable for nucleation sites of Nb/Ti-carbonitride precipitates [25]. These precipitates
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also play an important role in the microstructural refinement during thermomechanical [26]. At
high temperature, the dislocations produced during MAF undergo a recovery process associated
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with dislocation movement and absorption. This leads to the formation of low density
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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
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and pure -region, which showed significantly refined microstructures after 5 cycles of forging.
The EBSD inverse pole figure map and superimposed grain boundary map of both the specimens
revealed a severely deformed equiaxed fine grain structure, as shown in Figs. 4d and h,
respectively. Fine ferrite grains embedded within the larger size ferrites regions can be visible
from the EBSD image (Figs. 4d and h). The grain colors are determined by the orientation of
each grain as shown in the inset unit triangle of the figures. The orientation image microstructure
in the specimen deformed in α→γ transition region resulted in partially finer grains (~5 m)
along with larger sized grains (~32m) structure (Fig. 4d). The distribution of average grain size
is shown in Fig. 4e. It exhibited that the grains are mostly with low angle grain boundaries (Fig.
4f). Large amount of low angle boundaries can be attributed to the presence of comparatively
large sized grains. Fig. 4h reveals the deformed structure of the sample forged at α-region and

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the average grain size distribution is presented in Fig. 4j. This shows the formation of ultrafine
grains with a size of 1-3 μm (~30%) along with larger sized grains of ~25-27 μm (70%). A large
number of ultrafine grains can clearly be observed in the magnifying EBSD image shown in Fig.
4i. It can be identified that the new grains were developed along the grain boundaries of the pre-

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existing ferrite grains. From the analysis of the microstructures, it can also be noticed that the
misorientation angle of the grain boundaries (Fig. 4k) is comparatively higher than that of the

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transition region's forged sample. This is due to the fact of the dynamic recrystallization of ferrite

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grains during MAF at pure -ferritic region [27].

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Fig. 4: Optical microstructure after (a) Five cycle MAF at 1050°C (b) Corresponding average
grin size distribution (c) Optical microstructure after Five cycle MAF at 800°C (d)
Corresponding EBSD image with average grain size distribution (e) and (f) grain
boundary misorientation profile (g) Optical microstructure after Five cycle MAF at
650°C (h-i) Corresponding EBSD image with average grain size distribution (j) and (k)
grain boundary misorientation profile. (UFF→ultrafine ferrites; FF→fine ferites).
TEM images of the specimens MAFed at 650°C followed by air cooling are shown in Figs. 5a-d.
Fig. 5a shows high density dislocations produced during the MAF. The presence of fcc Niobium
carbide (NbC) along with its SADP is presented in Fig. 5b. Apart from the spot pattern
(appearing as regular hexagon) of the NbC from [111] zone axis, the SADP also reveals ring
pattern as well originated from the background consisting of fine ferrite grains. Distribution and
size of NbC precipitates can be ascertained from the TEM image shown in Fig. 5c. The image

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was recorded from the diffracted beam from the spot as encircled in Fig. 5b. It can be noticed
(from Fig. 5c) that the ultrafine precipitates of ~9-10 nm size are distributed randomly in the
matrix of fine ferrites. A large number of micro-shear bands in various directions can clearly be
identified from the TEM micrographs, as one is shown in Fig. 5d. The formation of micro-shear

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bands in various directions is due to the change in the strain paths during MAF in -ferritic
region.

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Fig. 5: (a) TEM bright field 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
fine ferrite matrix,(c) TEM dark field image, recorded from the diffracted beam from the
spot as encircled (sky colour) in Fig. 4b (d) micro-shear bands formation in various
directions.

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

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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

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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

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lower temperatures i.e. below Ar3 (at 800°C) and pure ferritic region (650°C). The maximum

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hardness was measured to be 1.91 GPa for the samples forged at 650°C. This is a ~2.8 times
higher when compared to that of the starting material sample. Increase in the hardness is mainly

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due to the refinement 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
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structural material [28]. Analysis of the improvement of the YS is discussed in the relevant
section (in the stress-strain plot).
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Fig. 6: Vickers hardness of as received annealed and MAFed specimens.

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Fig. 7: Engineering stress vs. Engineering strain curve.

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), the annealed sample showed slight less YS and UTS (YS=141

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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 μm; Fig. 3b) than that of the as-cast

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structure (210 μm; Fig. 3a).

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Table 2: The Mechanical properties of the homogenized annealed and multi-axially forged IF
steel specimens in different critical zones.

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Forging YS UTS Elongation Strain hardening
temperature (°C) (MPa) (MPa) (%) exponent (n)

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1050 435±5 473±3 30.44±1.5 0.126
800 466±4 MA 496±7 27.55±1 0.11
650 601±6 627±8 25±1.5 0.086
Annealed sample 141±3 256±5 46±1.7 0.254
As cast sample 165±4 281±3 34±1.5 0.207
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The YS and UTS (Fig. 7) of the specimen forged at 𝛾-recrystallized region found to increase to
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435 and 473 MPa, respectively, as compared to that of the homogenized annealed specimen
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(YS=141 MPa, UTS=256 MPa). The corresponding YS and UTS further improved to 466 and
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496 MPa, respectively, after MAFed at austenite-ferrite (γ→α) transition region (just below Ar3
region) followed by cooling under same conditions. The specimen MAFed in pure ferritic region
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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 more than 4
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 specific 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 μm (Fig. 4a). The
specimen forged in transition region showed a ductility ~28%, which corresponds to ferrite grain
size of ~5 μm embedded with larger size ferrites of ~32 (Figs. 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 (Figs. 4g-h); ultrafine ferrite grains (30%, ~1-3 μm size), large size ferrites (70%, ~25-27
μm). Therefore, it can be observed that the YS of the air cooled specimens is significantly
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improved without much affecting the ductility, especially when forged in pure ferritic phase
regime. This is mainly due to 2 reasons: (i) extensive grain refinement and (ii) dual size grain
distribution obtained by MAF in this region. It is known that the grain refinement is a
fundamental strategy to enhance YS of metallic materials without much sacrificing their ductility

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[26]. Therefore, improvement of the YS is due to the formation of finer ferrite grains and the
large size grains are responsible for retaining the ductility. Bodin et al. [29] also observed the

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formation bimodal distribution of ferrite grains in C-Mn steel (0.1C, 0.5Mn, 0.0045N) after

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intercritical rolling within (825-775)°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

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formability of 17% Cr ferritic stainless steel due to the formation of in-grain shear bands and
{111} recrystallized textures when hot rolling was carried out at low finishing temperature at
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700°C. Cizek et al. [31] studied the strengthening behavior of an IF steel after the HPT at room
temperature and demonstrated that the improvement of the YS occurred mainly due to the
dislocation strengthening and grain size refinement. The dislocation strengthening reported to be
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effective up to an equivalent strain of 3; whereas grain size refinement is saturated at an

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equivalent strain of 15. Further deformation lead to an additional moderate strengthening by the
formation of high angles grain boundaries (HAGBs) leading to a higher Hall-Petch coefficient.
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Enhancement of the YS and UTS of the samples forged at recrystallized γ-region is mainly due
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to the formation of smaller size ferrites (transformed from the fine recrystallized austenite
grains). Thus, the grain boundary area of austenites increases which provides a large number of
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nucleation sites for ferrites during cooling. Hence, the room temperature microstructure consists
of mainly small size equiaxed ferrite grains (~35 μm). On the other hand, the YS of the MAFed
samples in γ→α transition region found to further increase than that of the recrystallized
controlled MAFed samples due to the additional refinement of ferrite grains. The microstructure
found to consist of equiaxed fine ferrites of ~5 μm size embedded with larger size ferrites of ~32
μm. The formations of fine ferritic grains are due to the (also discussed earlier in the section of
microstructural investigation): (i) enhancement of γ→α transformation; and (ii) dynamic
recrystallization and strain-induced dynamic phase transformation. The strain induced dynamic
ferrite transformation was also reported to enhance mechanical properties in a TRIP steel
deformed just below Ac3 temperature [32]. Intercritical deformation followed by quenching and
partitioning of a HSLA steel resulted an ultrahigh YS with a significant ductility due to the

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formation of fine grained ferritic structure by deformation induced ferrite transformation [33].
Overall, it can be concluded that the improvement of the YS of the thermo-mechanically treated
samples is well-corroborated with the hardness values of the corresponding samples.
The dislocation density of the MAFed samples was calculated from the X-ray diffraction (XRD)

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data to analyze the strengthening effect due to strain hardening. The XRD patterns of the
controlled multi-axial forged specimens are shown in Fig. 8a. All these patterns have revealed

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the presence of only bcc -ferrite phase. However, width of the peaks is found to be broadened

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(a magnifying view of peak broadening for 110 reflection is shown separately in Fig. 8b) as the
deformation temperature decreased. The broadening of the peaks occurs mainly due to the

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refinement of crystallite size and increase in the dislocation lattice strain [34]. The instrumental
peak broadening has been eliminated from the total broadening using the standard broadening
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data of polycrystalline Al2O3 as per the Gaussian profile fit [35]:

βr = (β2 - β2 ) (1)
obs i
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where, obs and i, respectively, are the integral breadth of the corresponding hkl reflection at the
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full width at half intensity maxima (FWHM) of the forged specimen and standard Al2O3.
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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
reflection.

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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 BrCosθ vs. Sinθ as per Williamson-Hall technique [35]. The
dislocation density (ρd) can be estimated from the following equation [36] using the average

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crystallite size (D) and lattice microstrain (ε) as follows:

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1

ρ =
 
2 3 ε2 2
(2)

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d Db

where, b is the Burgers vector of the α-iron. For BCC α-ferrite, b = a 3 , where a=0.28664 nm
2

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[28]. Table 3 shows the detailed values of crystallite size, lattice microstrain and dislocation
density, theoretical and experimentally obtained YS of the forged samples.
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Table 3: Crystallite size, microstrain and dislocation density values, theoretical and
experimentally obtained yield strength for IF steel MAFed at different conditions.
Processing Crystallite size Lattice microstrain Dislocation σTaylor σy
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conditions (nm) (×10-3) (m-2) (MPa) (MPa)

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MAF in γ-region 82.03 2.71 3.97×10 439 435
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at 1050°C
MAF in γ-α
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transition zone 69.05 3.67 4.72×1014 471 466

at 800°C
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MAF at 650°C 46.22 4.33 8.15×1014 609 601

It can be noticed that the average lattice microstrain increased from 2.71x10-3 for the specimen
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forged γ-region (1050°C) to 4.33x10-3 corresponding to the specimen forged at 650°C in single
phase α-region. Correspondingly, the dislocation density, ρd, found to increase from 3.97×1014
m−2 to 8.15×1014 m−2. 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 the
reported values, respectively, were 3.6×1014 m−2 (i.e. at a strain of 1.15) and 6.88×1014 m−2 (at a
strain of 4.6). In the present study also, almost the same level of dislocation density has been
obtained for the multiaxially forged samples in γ-region (3.97×1014 m−2 and α-region (8.15×1014
m−2), although both deformations were carried out at higher temperatures. In case of the
specimen deformed at transition region, the dislocation density found to be 4.72×1014. Therefore,
it can be noticed that the accumulated dislocation density reached the maximum value for the
specimen forged in α-region compared to that of the other 2 forged samples. This is

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accomplished to the accumulation of high amount of lattice microstrain in α-region compared to

other 2 forged samples. The accumulated lattice strain results in the formation of high density
dislocation substructures at the ferrite boundaries as well as inside the grains [12]. These
substructures finally developed ultrafine ferrite grains by recovery during cooling.

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It should be remembered that usually the mean crystallite size estimated by X-ray diffraction line
profile analysis (XRDLPA) is lower than the actual grain size of the material [37,38]. Because

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of severe plastic deformation, the grains are usually divided into subgrains or dislocation

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substructures, and these dislocation cells are separated from each other by low-angle grain
boundaries [39]. The estimated crystallite size is generally comparable to the average domains

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size which diffracts X-rays coherently to produce broadened peaks [37,38]. To correlate the YS
obtained by experimental measurement, the theoretical YS due to dislocation strengthening has
been estimated using Taylor’s equation [28] and tabulated in Table 3;
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σ = σ0 + αMGbρ1 2 (3)
Taylor
where, σ0 is the friction stress (= 30 MPa), α a constant (α is taken as 0.33), G is the shear
D
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modulus (= 82 GPa), b is the Burgers vector (= 0.25 nm) and M is the Taylor factor = 3 for
untextured polycrystalline materials [37].
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It can be noticed that for all the specimens (Table 3), the experimentally obtained YS is very
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close to the theoretical YS as estimated using Taylor's equation (Eq. 3). It can be remembered
that the theoretical value of the YS was estimated only due to dislocation density, which includes
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the grain size effect. It should be remembered that the dislocation density increases with decrease
in the crystallite size (Eq. 2), which is equivalent to grain size for ultrafine structure. As we have
earlier mentioned that the improvement of the YS is due to the grain size refinement, 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

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been much higher than that of the experimentally obtained values after considering the
contribution from the precipitation strengthening.

3.3 Strain hardening behavior

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It is well-known that the strain-hardening exponent (n) is the basic deformation performance
parameter of metallic materials and it determines the flow behavior of a material when it is being

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deformed [28]. Material having higher n has better formability than that of the material having

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less value of n. The slope of the logarithmic plot of the equation σ = Kεn (log σ = log K + n logε)
is equal to the strain hardening exponent (n) [28]. In the present study, n was calculated from the

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true stress-true strain curves to analyze the effect of the deformation temperatures on the tensile
behavior of the IF steel. Fig. 9 shows the variation of the YS and uniform elongation as a
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function of the strain hardening exponent (n) for the thermomechanically treated samples
compared to that of the as-cast and annealed specimens. The values of n are also summarized in
Table 2 along with the other mechanical properties.
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Fig. 9: Variation of YS and Uniform elongation (UE) with strain hardening exponent.

In the cast specimen, the value of n was estimated to be 0.207. After homogenizing annealing
treatment, it increases to 0.254 due to softening of the material. The value of n is gradually
decreased with increase in the YS. The minimum value of n reaches to 0.086 corresponding to
the YS of 601 MPa, which is correspond to the specimen deformed in pure ferritic region. The
uniform elongation is found to be more for the sample having high value of n. This can be
clearly evident from Fig. 9 that the annealed specimen, which shows a large uniform elongation
of 30% has the highest value of n (0.254). Generally, the material exhibiting a low YS and large

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uniform elongation demonstrates a large amount of formability [40]. Because, the materials
having low YS and large uniform elongation are usually associated with large work-hardening
capacity. The value of uniform elongation can also been related with the inverse of the YS [40].
It can clearly be observed from Fig. 9 that the maximum YS of 601 MPa, which corresponds to

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the specimen deformed in pure ferritic region, shows a uniform elongation of only ~6.4%
(n=0.086); whereas, the maximum value of uniform elongation reaches to ~30% (n=0.254)

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corresponding to the YS of 141 MPa for the annealed sample. It can be noticed that the MAF

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among the 3 regions, the value of n is higher (0.126) for the specimen MAFed in pure austenitic
phase region compared that of the specimens deformed at other 2 regions, i.e. γ→α transition

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region (0.11) and at pure α region (0.086). The presence of ferrites during deformation leads to
high rate of strain hardening followed by formation of very fine ferrite grains. Therefore, it can
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be concluded that the specimen having high %elongation and low YS shows high value of strain
hardening exponent (n), which is essential for better formability. It can be noticed that total
elongation lies within a narrow range between 30 to 25% after MAF at 3 different phase regimes,
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while YS and UTS improve significantly. The MAFed specimen deformed in the ferritic region
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showed a remarkable improvement of YS (601 MPa as compared to 141 MPa of starting

materials) with a total elongation of ~25%; but its uniform elongation is limited to ~6.4% only
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corresponding to a poor value of n (0.086). This indicates that the formability is poor when
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deformed in the ferritic region. The extent of work hardening generally is very less in the MAF-
processed materials [11]. This can be attributed to the increase in strain rate sensitivity with
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strain especially for the materials of high strain rate sensitivity like IF steel [1,3] reported almost
same level improvement in the YS (600 MPa) after MAF of the IF steel; but the total elongation
was reported to be much inferior (only 7.5%) compared to that of the present study (25%).
Therefore, as compared to the previously reported works, better combination of mechanical
strength and ductility has been achieved in the present study. The multi axial forging is
associated with heterogeneities in microstructure. We are working out to overcome the
limitations associated with the process by optimizing temperatures, number of cycles, strain rate
per pass etc. in order to obtain desired microstructure and formability. The proper optimization
of the parameters may led to the increase in the uniform elongation and formability without
losing much of the strength. After achieving the goal, we will communicate our findings to the
same reputed Journal as early as possible.

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3.4 Fractography analysis

The fractured surface of the tensile specimens was examined under scanning electron microscope
to analyze the mode of failure and the fractographs are shown in Figs. 10a-e. Presence of dimple

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marks in the as-cast and annealed specimens indicates a ductile mode of failure. Larger size and
deeper dimple ruptures (av. size ~13 μm) can clearly be observed (in Fig. 10b) on the fractured

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surface of the annealed sample as compared to that of the as-cast sample (~9 μm) (Fig. 10a). This
observation correlates well with the high amount of tensile elongation obtained in the annealed

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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 ductility

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increased compare to that of the as-cast sample because of the increase in the grain size due to
annealing. Thereafter, (from Fig. 11) the average dimple size found to gradually decrease with
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decrease in the %elongation corresponding to decrease in the processing temperature (Fig.11).
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Fig. 10: SEM fractographs of tensile test specimen: (a) as-cast, (b) annealed, (c-e) five cycles
MAF at 1050, 800 and 650°C, respectively.

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This is because of the increase in the strength (equivalent to brittleness) of the material (Figs.
10c-e) due to the grain size refinement and strain hardening associated with the plastic
deformation [18,28]. It can be remembered that the %elongation of the samples forged in the γ
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and γ→α critical phase regions varies marginally from 31 to 28% only. This can be also be
correlated with the fractographs of the corresponding samples (Figs. 10c,d). The specimen
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MAFed at pure ferritic region showed relatively smaller size shallow dimple marks (Fig. 10e)
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indicating comparatively brittle appearance ductile failure.

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Fig. 11: The average dimple size vs. %elongation of the respective sample processed under
different conditions.

4 Conclusions
In the present study, we have investigated the microstructure and mechanical properties of Nb-Ti
stabilized IF steel multiaxially forged for 5 cycles in 3 critical temperature regions followed by
normal air cooling. On the basis of the results and their analysis, the following conclusions can
be ascertained:

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(1) The grain refinement mechanisms are found to be influenced by the deformation
temperatures in the 3 different phase regimes. Grain refinement during MAF at γ-region
(1050°C) is promoted by continuous dynamic recrystallization of deformed austenite grains and
formed fine equiaxed ferrite grains (∼35 μm) on normal cooling. On the other hand, formation of

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fine ferrite grains (~5μm) is attributed to the strain induced transformation of unstable γ during
MAF in γ→α transformation zone (800°C). The ultrafine ferrite grains formation (~1μm) in

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pure ferritic region (650°C) occurs through subgrains formation by deformation induced ferrite

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transformation (DIFT).

(2) The maximum refinement of grains was achieved when the specimen forged in pure ferritic

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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
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misorientation angles of grain boundaries and DIFT. This has been confirmed by detailed EBSD
study and TEM investigation.
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(3) Multiaxially forged sample at pure ferritic state (650°C) shows highest value of mechanical
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properties (YS-601 MPa and UTS-628 MPa) without much interfering the total elongation (25%)
compared to the other two cases. The improvement of the YS simultaneously with retaining high
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ductility is accomplished to the fact of bimodal grain structure obtained by MAF in this region.
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The fine size ferrites (average size ~1-3μm) is accountable for the high YS, while the
comparatively larger size ferrite grains (average size ~25-27μm) liable for the retained ductility.
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(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 ultrafine precipitates of TiC
and/or NbC in ferrite matrix, which has been confirmed 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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References
[1] Bhowmik A, Biswas S, Dhinwal SS, Sarkar A, Ray RK, Bhattacharjee D, Suwas S. Mi-
crostructure and texture evolution in interstitial-free (IF) steel processed by multi-axial forging.
Mater. Sci. Forum 2012;702-703:774-777.

PT
[2] Rana R, Bleck W, Singh SB, Mohanty ON. Development of high strength interstitial free steel by
copper precipitation hardening. Mater. Lett. 2007;61:2919–2922.

RI
[3] Capdevila C, Amigo V, Caballero FG, Andres CG, Salvador MD. Influence of micro- alloying
elements on recrystallization texture of warm-rolled interstitial free steels. Mater. Trans.

SC
2010;51:625-634.
[4] Lim SM, Wahabi ME, Desrayaud C, Montheillet F. Microstructural refinement of an Fe–C alloy

NU
within the ferritic range via two different strain paths. Mater. Sci. Eng. A 2007;532:460–461.
[5] Padap AK, Chaudhari GP, Pancholi V, Nath SK. Microstructural evolution
MA and mechanical
behavior of warm multi-axially forged HSLA steel. J. Mater. Sci. 2012;47:7894–7900.
[6] Guo WM, Wang ZC, Sheng L, Wang XB. Effect of finish rolling temperature on microstructure
and mechanical properties of ferritic rolled P-added high strength interstitial free steel sheet. J. Iron
D

Steel Res. Int. 2011;18:42-46.

TE

[7] Anand G, Sinha A, Chattopadhyay PP. Variation of tensile behaviour of interstitial free steel rolled
at cryogenic and room temperature. J. Inst. Eng. India Ser. D 2013;93:97–103.
P

[8] Mathis K, Krajnak T, Kuzel R, Gubicza J. Structure and mechanical behaviour of interstitial-free
steel processed by equal-channel angular pressing. J. Alloys Compd. 2011;509:3522-3525.
CE

[9] Halfa H. Recent trends in producing ultrafine grained steels. J. Minerals Mater. Charact. Eng. 2014;
2:428-469.
AC

[10] Alexander DJ. New methods for severe plastic deformation processing. J. Mater. Eng. Perform.
2007;16:360-374.
[11] Kundu A, Kapoor R, Tewari R, Chakravartty JK. Severe plastic deformation of copper using
multiple compression in a channel die. Scr. Mater. 2008;58:235–238.
[12] Salishchev GA, Valiakhmetov OR, Galeyev RM. Formation of submicrocrystalline structure in the
titanium alloy VT8 and its influence on mechanical properties. J. Mater. Sci. 1993;28:2898–2902.
[13] Andres CG, Caballero FG, Capdevila C, Alvarez LF. Application of dilatometric analysis to the
study of solid–solid phase transformations in steels. Mater. Charact. 2002; 48:101–111.
[14] Boratto F, Barbosa R, Yue S, Jonas JJ, 1988. Effect of chemical composition on the critical
temperature of microalloyed steels. Proceeding on Int. Conf. THERMEC1988;1: 383-390.
[15] Cuddy LJ. Grain refinement of Nb steels by control of recrystallization during hot rolling. Metall.
Mater. Trans. A 1984;15:87-98.

24
 ACCEPTED MANUSCRIPT

[16] Yang JH, Liu QY, Sun DB, Li XY. Recrystallization behavior of deformed austenite in high
strength microalloyed pipeline steel. J. Iron Steel Res. Int. 2009;16:75-80.
[17] Arribas M, Lopez B, Rodriguez-Ibabe JM. Additional grain refinement in recrystallization
controlled rolling of Ti-microalloyed steels processed by near-net-shape casting technology. Mater.

PT
Sci. Eng. A 2008;485:383–394.
[18] Hu J, Du LX, Xie H, Gao XH, Misra RDK. Microstructure and mechanical properties of TMCP

RI
heavy plate microalloyed steel. Mater. Sci. Eng. A 2014;607:122–131.
[19] Gong P, Palmiere EJ, Rainforth WM. Dissolution and precipitation behaviour in steels micro-

SC
alloyed with niobium during thermo-mechanical processing. Acta Materialia 2015;97;392–403.
[20] Zhang ZY, Yong QL, Sun XJ, Li ZD, Kang JY, Wang GD. Microstructure and mechanical

NU
properties of precipitation strengthened fire resistant steel containing high Nb and low Mo. J. Iron
Steel Res., Int. 2015;22:337-343. MA
[21] Junior AMJ, Guedes LH, Oscar B. Ultrafine grain refinement during the simulated the-
rmomechanical processing of low carbon steel. J. Mater. Res. Technol. 2012:1:141-147.
[22] Sun ZQ, Yang WY, Qi JJ, Hu AM. Deformation enhanced transformation and dynamic
D

recrystallization of ferrite in a low carbon steel during multipass deformation. Mater. Sci. Eng. A
TE

2002;334:201-206.
[23] Zhao B, Liu F, Li G, Xu R, Yang J. Effect of temperature and strain on microstructure refinement
in low carbon microalloyed steel during multi-axis deformation process. Met. Mater. Int.
P

2013;19:549-553.
CE

[24] Mohamadizadeh A, Hanzaki AZ, Kisko A, Porter D. Ultra-fine grained structure formation through
deformation-induced ferrite formation in duplex low-density steel. Mater. Des. 2016;92:322–329.
AC

[25] Priestler R, Li PH, Zhou C, Ibraheem AK. Microally precipitation in HSLA steel austenite.
Microstruct. Sci. 1998;26:447-454.
[26] Gladman T. The Physical Metallurgy of Microalloyed Steels. The Institute of Material, London:
1997, p. 280–288.
[27] Ghosh S, Mula S. Thermomechanical processing of low carbon Nb–Ti stabilized microalloyed
steel: Microstructure and mechanical properties. Mater. Sci. Eng. A 2015;646:218–233.
[28] Dieter GE. Mechanical Metallurgy, second ed. Mc Graw-Hill Book Co., New York: 1976, p. 325-
337.
[29] Bodin A, Sietsma J, Van der Zwaag S. On the nature of the bimodal grain size distribution after
intercritical deformation of a carbon-manganese steel. Mater. Charact. 2001;47:187-193.

25
 ACCEPTED MANUSCRIPT

[30] Gao F, Yu FX, Liu FT, Liu ZY. Hot deformation behavior and flow stress prediction of ultra
purified 17% Cr ferritc stainless steel stabilized with Nb and Ti. J. Iron Steel Res. Int. 2015;22:827–
836.
[31] Cízek J, Janecek M, Krajnak T, Straska J, Hruska P, Gubicza J, Kim HS. Structural characterization

PT
of ultrafine-grained interstitial-free steel prepared by severe plastic deformation. Acta Mater.
2016;105:258-272.

RI
[32] Mohamadizadeh A, Hanzaki AZ, Manesh SH, Imandoust A. The effect of strain induced ferrite
transformation on the microstructural evolutions and mechanical properties of a TRIP-assisted

SC
steel. Mater. Sci. Eng. A 2014;607:621–629.
[33] Liu H, Sun H, Liu B, Li D, Sun F, Jin X. An ultrahigh strength steel with ultrafine-grained

NU
microstructure produced through intercritical deformation and partitioning process. Mater. Des.
2015;83:760–767. MA
[34] Ungar T, Ott S, Sanders PG, Borbely A, Weertman JR. Dislocations, grain size and planar faults in
nanostructured copper determined by high resolution X-ray diffraction and a new procedure of peak
profile analysis. Acta. Mater. 1998;46:3693-3699.
D

[35] Mote VD, Purushotham Y, Dole BN. Williamson-Hall analysis in estimation of lattice strain in
TE

nanometer-sized ZnO particles. J. Theo. Appl. Phys. 2012;6:1–8.

[36] Zhao YH, Horita Z, Langdon TG, Zhu YT. Evolution of defect structures during cold rolling of
P

ultrafine-grained Cu and Cu–Zn alloys: Influence of stacking fault energy. Mater. Sci. Eng. A
2008;474:342–347.
CE

[37] Sarkar A, Bhowmik A, Suwas S. Microstructural characterization of ultrafine-grain interstitial-free

steel by X-ray diffraction line profile analysis. Appl. Phys. A 2009;94:943–948.
AC

[38] Cullity BD. Elements of X-Ray Diffraction, Edison Wesley, London:1978, p. 259-270.
[39] Dasharath SM, Koch CC, Mula S, Effect of stacking fault energy on mechanical properties and
strengthening mechanisms of brasses processed by cryorolling. Mater. Charact. 2015;110:14-24.
[40] Kang DH, Kim DW, Kim S, Bae GT, Kim KH, Kim NJ. Relationship between stretch formability
and work-hardening capacity of twin-roll cast Mg alloys at room temperature. Scr. Mater.
2009;61:768–771.

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Graphical abstract

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Research Highlights

 Evolution of ultrafine grained interstitial free steel by multiaxial forging.

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 Experimental parameters were designed through dilatometric study using Gleeble-3800

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simulator.

 The specimen forged at pure ferritic region shows best combination of YS and ductility.

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 EBSD study confirms the formation ultrafine grains with high angle of misorientation.

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 Nanosize Ti-Nb carbides and dislocation strengthening play vital roles to produce

ultrafine grained steel through multiaxial forging.

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