Materials Science & Engineering A 830 (2022) 142314

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

The effect of cold-rolling prior to the inter-critical heat treatment on

microstructure and mechanical properties of 4340 steel with ferrite –
Martensite microstructure
F. Hosseinifar, A. Ekrami *
Department of Materials Science and Engineering, Sharif University of Technology, Tehran, Iran

A R T I C L E I N F O A B S T R A C T

Keywords: This study investigates the effect of cold rolling prior to inter-critical annealing on microstructure and me­
Dual-phase steel chanical properties of ferrite-martensite dual phase steel. Samples were heated to 850 ◦ C for 1 h followed by oil
Martensite quenching, then the steel sheet were cold rolled by 0%,10%,15% and 20% reduction in thickness. The inter-
Ferrite
critical annealing treatment (750 ◦ C, 120min) was performed to generate a ferrite-martensite microstructure.
Cold-rolling
Mechanical properties
Microstructural studies showed that increasing the applied cold rolling, leading to increase in volume fraction of
Microstructure martensite and decrease in ferrite grain size. Mechanical properties of dual phase steel were measured by tensile,
impact and hardness tests. Results showed that ultimate tensile strength, yield strength, micro-hardness and
toughness (e.g. total elongation, uniform elongation and impact energy) increased with increasing the applied
cold rolling. Improvement of mechanical properties were related to increase in martensite volume fraction and
ferrite grain refinement. Analysis of strain hardening behavior of DP steels, by Hollomon analysis, showed two
stages of strain hardening corresponding to ferrite deformation and co-deformation of ferrite and martensite,
respectively. The strain hardening exponent of first stage (nI) increased with increasing volume fraction of
martensite. The energy absorption capacity (UE × UTS) increased with increasing cold rolling deformation.

1. Introduction
Advanced high-strength steels (AHSS) have vast applications due to
their high formability and strength and low weight. In recent decades
significant efforts were made in order to develop advanced high-
strength steels for use in the automotive industry. Lower fuel con­
sumption and reduced gas emissions as a result of lower weight along
with increased passenger safety were among the reasons behind the
development of this group of steels. The AHSS family covers different
grades of steel, including dual-phase (DP), complex-phase (CP),
martensitic (MART), transformation induced plasticity (TRIP), twinning
based plasticity (TWIP), Al-added lightweight steel with induced plas­
ticity (L-IP), and shear band strengthened (SIP) [1–5]. Although AHSS
have favorable properties, yet strength, flexibility, and cost must be
balanced prior to the application in the industry. For instance, TRIP and
TWIP steels are questioned for their high prices and their low toughness,
which is the result of precipitation hardening through aluminum and
titanium. On the other hand, dual-phase steels are relatively cheap and
formable. They have high strength, making them a potential for vast
automotive industry applications for bumpers and other parts of vehi­
cles [6,7]. High tensile strength, continuous yielding, high total elon­
gation, and initial work hardening rate, as well as low yield to tensile
strength ratio, are characteristics of dual-phase steels [8]. Moreover,
dual-phase steels possess a straightforward microstructure, better weld
ability, and thermodynamic stability, which prevent microstructural
aging during service at room temperature [9]. Dual-phase steels
commonly have a strengthening phase such as martensite or bainite,
which is surrounded by a ductile ferrite matrix. This phase organization
simultaneously provides the steel with strength and ductility [10,11].
The characteristics of the final structure, including morphology, the size,
and distribution of the martensite phase and the ferrite grain size, im­
pacts the mechanical properties and the work hardening behavior of the
dual-phase steel [12,13]. The morphology of the martensite phase has a
tremendous influence on the mechanical properties of the dual-phase
steels. Dual-phase steels containing fine and fiber martensite dispersed
homogeneously in the ferrite matrix, as opposed to dual-phase steels
having blocky ferrite and martensite or martensite islands dispersed in
the grain boundary area of multi-ax ferrite, present the best combination

* Corresponding author.
E-mail address: ekrami@sharif.edu (A. Ekrami).

https://doi.org/10.1016/j.msea.2021.142314
Received 26 July 2021; Received in revised form 7 November 2021; Accepted 8 November 2021
Available online 13 November 2021
0921-5093/© 2021 Elsevier B.V. All rights reserved.
F. Hosseinifar and A. Ekrami
of strength and ductility [13]. Zhang [14] discussed the impact of
morphology and distribution of martensite on the mechanical properties
of the dual-phase steel. The results indicate that increasing the
inter-critical annealing temperature leads to homogeneous martensite
distribution in the microstructure. Moreover, the morphology of the
martensite becomes coaxial, resulting in reduced mechanical strength in
the dual-phase steels. Although the microstructural alterations affect the
mechanical properties of the dual-phase steel, yet the martensite volume
fraction is considered to be a key factor shaping the mechanical prop­
erties [3]. Two distinct models, linear and non-linear, are suggested to
theorize the relation between the mechanical strength and the
martensite volume fraction in the dual-phase steels. According to the
linear model, increasing the martensite volume fraction leads to an in­
crease in the mechanical strength of the dual-phase steel. On the con­
trary, the relation between volume fraction and strength based on the
non-linear model is of other nature [15]. Pan et al. [16] investigated
the mechanical properties of the dual-phase steel, reporting that
increasing the inter-critical annealing temperature causes a rise in the
martensite volume fraction, while the ferrite grain size drops, the
outcome of which decreases the uniform and total elongations in the
dual-phase steels. Additionally, the results implied that decreasing the
size of the martensite islands did not cause an enhancement in the yield
and tensile strengths, forasmuch as the carbon content of the martensite
phase is the key factor influencing the mechanical properties of the
dual-phase steel. Movahed et al. [17] reported that the yield strength of
the dual-phase steels containing 20–70% martensite increases linearly
with the martensite phase; however, the tensile strength and elongation
vary linearly, reaching their maximum value at 50% martensite volume
fraction. Mazaheri et al. [18] investigated the thermo-mechanically
prepared dual-phase steels containing 30–50% martensite volume
fraction, reporting that the yield strength, tensile strength, and elonga­
tion vary linearly with the martensite volume fraction. The refinement
of the grain size in the dual-phase steels leads to a significant increase in
the mechanical strength without any loss in ductility [19]. Due to the
lowered stress/strain partitioning between ferrite and martensite, the
dual-phase steel with fine microstructure presents a proper combination
of strength, ductility, and work hardening ability [20]. Saeidi et al. [20]
developed ultra-fine grained dual-phase steel through inter-critical heat
treatment after several cold work processes and, subsequently,
inter-critical annealing in a short period of time. Due to the uniform
distribution of strain in the ultra-fine grained dual-phase steel, the steel
offered more toughness compared to coarse grain dual-phase steel.
Furthermore, the resistance to the nucleation of dimples in the fine grain
dual-phase steel increases as well, whereas the dual-phase steel with
coarse grains maintained a higher density of piled up dislocation in the
ferrite – martensite grain boundary, which led to stress concentration in
the martensite and as a result, nucleation of dimples from the martensite
phase [21].
As mentioned previously, extensive studies have been performed on
dual-phase steels to improve the performance and mechanical properties
of these types of steels. The greatest effect on improving the mechanical
properties of dual-phase steels was achieved by grain refinement.
Various methods involving severe plastic deformation (SPD), increase in
heating rate, changing the soaking time and temperature in the inter-
critical region, and increased alloying elements have been performed
to achieve this purpose. But, these methods bring barriers to the in­
dustrial manufacturing of fine-grained dual phase steels. However, the
successful production of fine-grained DP steels remains a challenge. The
purpose of this study is to propose a new processing route for grain
refinement of dual-phase steels that can be industrially implemented. In
this study, notwithstanding previous investigations, fine-grained dual-
phase steels were produced in a shorter processing route by applying
and increasing cold rolling on martensitic microstructure. Grain
refinement is achieved without applying any changes on heating rate or
soaking time and temperature in the inter-critical region and neither
special heating furnaces. The results represent that increasing the
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Materials Science & Engineering A 830 (2022) 142314
applied cold-rolling on martensitic steel causes a high density of
preferred nucleation sites for austenite formation which leads to grain
refinement of the structure after finishing the inter-critical annealing.
In the present study, four groups of dual-phase AISI4340 steels with
different ferrite and martensite contents were developed through the
thermo-mechanical process. Finally, the microstructure, tensile prop­
erties, work hardening, and the fracture surfaces of dual-phase samples
were characterized and discussed.
2. Experimental methods
The AISI 4340 steel’s chemical composition, determined by atomic
emission spectroscopy analysis, is given in Table .1. To perform the
thermomechanical treatment, samples were cut into 10*50*100 mm
plates. Ac1 and Ac3 inter-critical temperatures are, using equations (1)
and (2), 728.5 ◦ C, and 795.4 ◦ C, respectively.
Ac1(oC) = 723-10.7Mn + 29.1Si-16.9Ni+16.9Cr+290As + 6.38W (1)
Ac3(oC) = 910-203C0.5+44.7Si-15.2Ni+104V + 31.5Mo+13.1 W (2)
The schematic of the thermomechanical treatment cycle is illustrated
in Fig. 1. Steel plates were heated at 850 ◦ C for 60 min in a furnace with
a heating rate of about 14 C/min, before quenching into oil. The sub­
◦
sequent martensitic samples were cold rolled up to 10%, 15%, and 20%
reduction in thickness. To develop a ferrite-martensite microstructure,
the unrolled and rolled samples were held at 750 ◦ C for 120 min, in the
inter-critical region, and then cooled in oil to room temperature. The
produced DP steels referred to 0DP, 10DP, 15DP and 20DP respectively
in this research.
The heat-treated specimens were mounted, grinded and polished
based on standard metallographic methods, followed by a chemical etch
in 2% Nital solution (98 ml C2H6O + 2 ml HNO3). Microstructure studies
were performed on section parallel to rolling direction (Fig. 2). More­
over, the “Olympus BX51 M′′ optical microscope with a “Clemex”
camera (OM) and “TE-SCAN MIRA3” field emission scanning electron
microscope was used for further investigation of microstructure. The
martensite and ferrite volume fraction and ferrite grain size were
measured by the “Image J′′ image processing Software. The volume
fraction was determined by optical image analysis processing (threshold
method). The average values were calculated from measured values on
20 micrographs.
The Vickers hardness was measured at 30 N and the average of 10
measurements were selected as hardness.
Uniaxial tension test was employed on specimens, with 25 mm gage
length and 6 mm width, at room temperature using “Santam STM150” at
a constant speed of 2 mm/min. The tension test samples were prepared
according to ASTM E8 standard [22] in the rolling direction. The
average results of 3 specimens were reported as tensile properties.
The Charpy impact test was used to determine the impact resistance
of dual-phase microstructures. Impact tests specimens (Fig. 3) were
prepared according to ASTM E23 standard [23]. The average impact
energy of 3 specimens was reported as the impact energy. The fractured
tensile specimen surfaces were studied, using field emission scanning
electron microscope (FE-SEM) and “Olympus SZH10” stereo
microscope.
3. Results
3.1. Microstructure
The microstructure of dual-phase specimens, without cold rolling
and after 10%, 15%, and 20% cold rolling in section parallel to the
rolling direction is presented in Fig. 4 Microstructure of produced DP
steels consists of fiber martensite within the ferrite matrix. As mentioned
in section 2, ferrite and martensite volume fractions are measured on
optical photographs. For example, ferrite and martensite phases are
F. Hosseinifar and A. Ekrami Materials Science & Engineering A 830 (2022) 142314

Table 1
Chemical Composition of investigated low alloy AISI4340 (wt%).
C Si Mn Al Cr Ti Mo Ni P, Co, Cu Fe

0.35 0.3 0.77 0.086 1.15 0.11 0.17 0.94 <0.1 Balance

strength increase with increasing the cold rolling. The strength of the
dual-phase steels are affected by the martensite volume fraction, the
strength of each phase and the grain size of the present phases in the
structure.
As illustrated in Fig. 7, the specimen’s yield strength increases with
the administration of cold work. Therefore, the yield strength increment
is due to the rise in the volume fraction of the martensite, as well as the
grain refinement of the ferrite phase (Table .2).
The correlation between yield strength and ferrite grain size is pre­
sented in Fig. 8, This curve indicates that the yield strength of investi­
gated dual-phase steels decrease linearly with increasing the ferrite
grain size. The results of the current study are in accordance with that of
Ashrafi et al. [26].
Fig. 1. Thermomechanical process routes for producing dual phase steel.
3.2.2. Uniform and total elongations
Fig. 9 represents variation of uniform and total strains (Table .3) with
represented in Fig. 5 for 10DP steel. Table .2 demonstrates the
volume fraction of martensite (or cold rolling %). As can be seen, uni­
martensite and ferrite volume fractions and ferrite grain size of inves­
form strain increases with increasing cold rolling, but total elongation
tigated dual phase steels. It can be seen from Table .2 that with
increases with cold rolling up to 15% and decreases then with further
increasing the percentage of rolling the martensite volume fractions
rolling reduction in thickness.
increases and the ferrite grain size decreases.

3.2. Tensile properties

The engineering stress-strain curves of 0DP, 10DP, 15DP and 20DP

are presented in Fig. 6. The stress-strain curve indicates that unlike
ferrite - pearlite steel, the yield point phenomenon does not appear in
dual-phase steels. The occurrence of the yield point phenomenon in the
ferrite-pearlite microstructure has been attributed to the dislocation
locking by the Cottrell atmosphere of interstitial atoms [24]. Volume
expansion and shear stress resulting from austenite to martensite phase
transformation leads to the formation of unlocked dislocations in the
ferrite and zones adjacent to the transformed martensite phases. The
presence of these dislocations corresponds to the lack of yield point
phenomenon in the ferrite-martensite steels [25].

3.2.1. Ultimate tensile strength and yield strength

Mechanical properties of investigated DP steels are presented in
Table .3.
Fig. 3. Specimen geometry for Charpy impact test. ND normal direction, TD
Variation of tensile and yield strengths with rolling percentage are
transverse direction, and RD rolling direction.
plotted in Fig. 7 As can be seen, both ultimate tensile strength and yield

Fig. 2. Specimen coordinate system for microstructural observation. ND normal direction, TD transverse direction, and RD rolling direction.

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F. Hosseinifar and A. Ekrami
Fig. 4. Microstructures of produced dual phase steels in section parallel to the rolling direction (a) 0DP, (b) 10DP, (c) 15DP (d) 20DP. DP steels were produced
according to processing routes illustrated in Fig. 1.
3.2.3. Hardness
The results of hardness test for investigated dual phase steels are
presented in Table .3. The hardness of dual-phase steels (HVDP) can be
determined using the rule of mixtures (Equation.3):
HVDP = VF HVF + VM HVM (3)
HVF, HVM, VF, and VM represent the ferrite phase hardness,
martensite hardness, volume fraction of ferrite, and volume fraction of
martensite, respectively. Assuming that the hardness of ferrite and
martensite are independent of the volume fraction and morphology of
ferrite and martensite, the hardness of dual-phase steels can be rewritten
into (Equation.4):
HVDP = A + B VM (4)
Equation.4 demonstrates the linear association between the
martensite volume fraction and the hardness of dual-phase steels, i.e.,
the hardness of dual-phase steel follows up as the volume fraction of
martensite increases.
Fig. 10 shows the relation between the hardness as a function of
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Materials Science & Engineering A 830 (2022) 142314
martensite volume fraction. This figure confirms the linear increase of
hardness by increasing the volume fraction of martensite. By calculating
A and B from Fig. 10, the following equation can be drawn for the
investigated DP steels (Equation.5):
HVDP = 253.4 + 3.5 Vf (5)
3.2.4. Work hardening
Hollomon’s equation [27] was applied to investigate the work
hardening behavior of produced dual phase steels (Equation.6):
σ = K εn (6)
Where k and n are the strength index and strain hardening exponent
respectively. Hollomon’s equation can be rewritten into:
Lnσ = LnK + n Lnε (7)
In which the relation between Lnσ and Lnε is linear and the value of n
is the slope of this line. In the Hollomon relation, n is a proper criterion
F. Hosseinifar and A. Ekrami Materials Science & Engineering A 830 (2022) 142314

for highlighting the work hardening ability of materials. The Lnσ vs. Lnε
curves of the analyzed 0DP and 20DP steel are presented in Fig. 11, the
10DP and 15DP showed the same behavior. The values of strain hard­
ening exponent (n) are presented in Table .4. The work hardening
exponent values at the first stage are greater than those in the second
stage for each DP steels and increases with the progress of the cold work.

3.2.5. Impact test

The impact test results of DP steels (Table .3) which plotted in Fig. 12
indicate that the impact energy increases with the progress of the cold
rolling.

3.2.6. Energy absorption capacity

Energy absorption capacity is considered a key factor in the auto­
motive industry since it remarkably defines the damage inflicted on the
vehicle upon an accident. The multiplication of uniform elongation and
ultimate tensile strength is regarded as the energy absorption capacity in
dual-phase steels. The energy absorption capacities of investigated dual
phase steels are presented in Table .5.
Fig. 5. Microstructures of 10DP steel in section parallel to the rolling direction.
White and dark phases represent ferrite and martensite phase respectively.
3.2.7. Fractography analysis
As illustrated in Fig. 13, the fracture surface consists of three zones.
The first zone includes planes with a 45◦ angle, called shear planes, and
Table 2
Microstructural parameters of investigated dual phase steels. is responsible for the plastic deformation. The second zone contains
rougher lines called radial lines, and the third zone includes flat planes
Sample Martensite volume Ferrite volume ferrite grain size
that are referred to as fiber zone. The fracture planes in the fiber zone are
fraction (%) fraction (%) (μm)
perpendicular to the applied load direction.
0DP 45.2 ± 4.1 54 ± 4 10.25 ± 3.2
Fig. 14 shows the relation between the total elongation and area
10DP 48 ± 2.4 51.9 ± 2.4 8.06 ± 1.4
15DP 59.6 ± 4.7 40.3 ± 4.7 5.28 ± 0.61 reduction of investigated dual-phase steels. According to Figs. 13 and
20DP 76.5 ± 3.8 23.4 ± 3.8 2.72 ± 0.44 14, with increasing the applied cold rolling, plastic deformation of
investigated dual phase increased that has complied with results of
impact test and variation of total elongation of investigated dual phase
steels.
The images from field emission SEM (Fig. 15) indicate that the
fracture surface of investigated dual-phase steels contains dimples and
cleavage planes that suggest mixture of ductile and brittle fractures.
According to Fig. 16, with increasing the volume fraction of
martensite, resulted from increase in cold rolling percentage prior to
inter-critical heat treatment, the mean size of dimples increases as well
and resulting in the increment of the total elongation of the investigated
dual-phase samples.

4. Discussion

4.1. The effect of cold rolling on microstructure

Plastic deformation increases the stored energy of the structure,

Fig. 6. Engineering Stress-Strain curves of investigated dual phase steels.
which increases the driving force required for the nucleation of ferrite
and austenite in the inter-critical region. The stored energy is released
by recrystallization.
During heating the structure to the inter-critical region, recrystalli­
zation of ferrite from the martensitic structure is completed at first.
According to Fig. 4, the absence of grain orientation in the rolling di­
rection proves the completion of ferrite recrystallization from the
martensitic microstructure in the inter-critical region. Austenite is then
formed at the recrystallized ferrite grain boundaries due to the low

Table 3
Summary of mechanical properties of studied DP steels.
Sample Yield Strength Ultimate Tensile Total elongation Uniform Vickers hardness Impact energy Reduction of Area (R/ Yield
(MPa) Strength (MPa) (%) elongation (%) (HV) (J) A) (%) ratio

0DP 908.7 ± 9.2 1481.1 ± 11.6 7.1 2.9 400.1 9.6 15.4 0.6
10DP 1065.9 ± 11.1 1617.7 ± 8.5 7.9 3.1 430 10.1 34.9 0.6
15DP 1090.6 ± 3.6 1630.2 ± 3.4 13.4 3.5 470.7 11.8 41.3 0.5
20DP 1171.8 ± 4.1 1691.9 ± 5.7 8.8 3.8 517.3 13 47.5 0.7

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F. Hosseinifar and A. Ekrami Materials Science & Engineering A 830 (2022) 142314

Fig. 7. Ultimate tensile strength, yield strength and volume fraction of martensite as a function of applied cold work.

Fig. 8. Variation of yield strength with ferrite grain size.

heating rate. The distribution of austenite phase is also affected by the
ferrite recrystallization process [28]. Formation of austenite in
inter-critical region can be separated into two stages: (1) nucleation of
austenite from recrystallized ferrite grain boundaries (2) dissolution of
ferrite in newly formed austenite [28].
Cold-rolling of the martensitic microstructure leads to an increase in
the dislocations density. Heating of this structure to the inter-critical
temperature causes the deterioration of crystal lattice resistance and
motion of dislocations. The possibility of diffusion authorizes the
dislocation climb process. Thereupon, similar dislocations establish sub-
grain boundaries that ultimately result in a fine-grain structure.
The austenite transformation behavior is also affected by grain size
of steel so a finer-grained material is rising to faster transformation [29].
Increasing the density of recrystallized ferrite grain boundaries due
to increasing the applied cold rolling causes increasing nucleation sites
for austenite formation and raising the volume fraction of martensite
after quenching the structure. In other words, variation of ferrite and
martensite volume fractions is a fruit of different nucleation kinetics of
austenite and ferrite in the inter-critical region [16]. According to
Table 2, with increasing the applied cold-rolling the ferrite grain size
decreases and volume fraction of martensite increases.
4.2. The effect of cold rolling on mechanical properties
4.2.1. Ultimate tensile strength and yield strength
As discussed previously, with increasing the percentage of applied
cold work the nucleation rate of austenite phase increases and leads to
increase in volume fraction of martensite during the inter-critical

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F. Hosseinifar and A. Ekrami
Fig. 9. Percentage of uniform and total elongation of dual phase specimens as a
function of Volume Fraction of Martensite and applied cold roll.
Fig. 10. Hardness as a function of martensite volume fraction or applied
cold rolling.
annealing. Therefore, both yield and tensile strengths increase which is
in line with the results presented by Maleque et al. [30]. Reducing the
grain size is considered to be one of the main approaches for strength­
ening of steels. Part of the strength increment is due to the grain
refinement. As shown in Table .2, decrease in ferrite grain size was
observed with increase in reduction in thickness because of the cold
rolling.
The grain boundary density increases with grain refinement. The
grain boundaries are counted as a barrier against the motion of glissile
dislocations. The grain boundary strength is greater than the grain
strength at temperatures lower than 0.5 Tm. Thus, raising the grain
boundary density yields to an increasing the structure’s strength [18].
Volume fraction of martensite also affects on ferrite strength. During
the austenite to martensite transformation, the increased volume
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Materials Science & Engineering A 830 (2022) 142314
fraction of martensite in dual-phase steels results in a higher density of
dislocations in the adjacent ferrite phase. Therefore, the hard-worked
ferrite causes the enhancement of the strength of the dual-phase steel.
According to the Hall-Petch theory (equation.8), grain refinement
leads to the enhancement of the yield strength. The theory imparts that
the applied stress must reach a certain value so that the piled-up dislo­
cations at a grain boundary could propagate through it; hence the in­
crease of grain boundaries density incites the increase in the yield stress.
The Hall-Petch equation is as follows:
σy = σ0+kD− 0.5
(8)
The σy represents the yield strength, D is the average grain diameter,
K is the strengthening coefficient, and σ0 is the lattice resistance to
dislocation motion.
4.2.2. Uniform and total elongations
Structure refinement reduces the stress concentration in the ferrite
and martensite interface and improves the stress transfer among these
phases. Based on misorientation analysis within the deformed micro­
structure, it has been shown that lattice deformation was mainly higher
at the ferrite–martensite interfaces than at the center of the ferrite grains
[31]. It means that there is a positive deformation gradient from the
center of the ferrite grain towards its boundaries; so, the lower this
distance, the lower the deformation gradient. Therefore, it was expected
that in a fine grained DP microstructure, owing to smaller constituent
grains, deformation gradient within the microstructure would be lower,
i.e. better strain distribution existed in the microstructure [32]. The
uniform distribution of fine martensite within the microstructure of
dual-phase steels reduces the stress concentration, levels the distribution
of strain in the structure, and postpones the necking and heterogeneous
deformation to higher strains [33]. Fig. 9 indicates that the total elon­
gation of 15% cold-rolled specimen is higher than other samples. The
case behind the increase of ductility in this specific sample can be
associated with the fact that by further increment in the volume fraction
of martensite, along with a reduction in the grain size of the ferrite
phase, the density of glissile dislocations in the ferrite phase increases,
and locking of the dislocations at the early stages of deformation reduces
the ductility of steel with a higher volume fraction of martensite. The
results of the current study are in accordance with the results of Saeidi
et al. [34].
4.2.3. Hardness
The increase in hardness can be attributed to the simultaneous effect
of increasing the volume fraction of martensite, grain size reduction and
uniform distribution of the hard phase in the structure. Martensite vol­
ume fraction increment leads to the generation of residual stresses and a
higher density of dislocation within the adjacent ferrite phase, thus
increasing the hardness of the dual-phase structure. It has been reported
that with increasing the applied cold rolling, the martensite developed
by the rapid cooling from the inter-critical zone contains more internal
twins, which also increases the hardness of the martensite [35].
4.2.4. Work hardening
The strain hardening exponent was attributed to the maximum
uniform plastic deformation [17]. Therefore, increasing the strain
hardening exponent value, n, suggests that the material is more capable
of plastic deformation before reaching instability and necking. From
Fig. 11, which shows variation of ln σ with ln ε, it can be seen two lines
with different slope values (nI and nII in Table .4) for a given steel.
Therefore, it can be deduced that the investigated DP steels showed two
stages of work hardening. The stages of work hardening are categorized
as:
• Stage 1: Deformation of ferrite
• Stage 2: Simultaneous deformation of ferrite and martensite
F. Hosseinifar and A. Ekrami Materials Science & Engineering A 830 (2022) 142314

Fig. 11. Plot of log true stress - log true strain for investigated dual phase steel with (a) 0DP, (b) 20DP.

Therefore, plastic deformation has dwindled at the second stage of work

Table 4 hardening. In both stages, the strain hardening exponent increases with
Summary of the strain hardening results for the DP steels.
the progress of the cold work.
Steel nI nII εtr With increase in the volume fraction of martensite due to the further
0DP 0.83 0.43 0.033 progress of the cold roll, the density of dislocations generated in the
10DP 0.88 0.46 0.037 ferrite phase increases and causing increase in the work hardening rate
15DP 0.89 0.54 0.039 and the strain hardening exponent. The work hardening rate increases,
20DP 0.92 0.59 0.043
which in part, postpones necking to higher stresses and increases the
uniform and total elongations of the sample. The transition strain be­
tween the deformation stages (εtr), also increase with the progress of the
cold work.

4.2.5. Impact test

Due to the austenite to martensite transformation stresses, the ferrite
undergoes plastic deformation, therefore enhancing the toughness of the
structure, since the ferrite reduces the stress concentration in the zones
adjacent to the martensite - ferrite interface. In other words, the volume
expansion caused by the transformation of austenite to martensite
generates compressive stress in the ferrite. Moreover, during the
nucleation and growth of cracks in the martensite, this stored elastic
energy in ferrite is discharged and prevents crack propagation [36]. As
mentioned previously, the volume fraction of martensite increases with
increasing the cold work, the density of the dislocations developed in the
ferrite increases and ultimately giving a raise to the impact energy of the
specimens.
Further increase in the applied cold work leads to the reduction of
ferrite grain size. Reduced grain size is also one of the factors affecting
the increase in the impact energy of investigated DP steels.

Fig. 12. Impact energy of investigated dual phase steels. 4.2.6. Energy absorption capacity
According to Table .5, cold work increment increases the energy
absorption capacity of the dual-phase steels, which is in conflict with the
Table 5 results of Ashrafi et al. [26] reporting that increasing the volume frac­
Energy absorption capacity of the investigated dual phase steel. tion of martensite yields to a lower energy absorption capacity. The role
Sample Uniform elongation Ultimate Tensile Strength UTS × UE (% of grain refinement on increasing the uniform elongation and strength of
(%) (MPa) MPa) () the dual-phase steels in the current study is regarded as the cause behind
0DP 2.98 1481.08 4413.62 the energy absorption capacity improvement resulted from the cold
10DP 3.11 1617.78 5031.30 work.
15DP 3.58 1630.23 5836.22
20DP 3.83 1691.93 6480.10
4.2.7. Fractography analysis
According to Figs. 13 and 14, the increase in the shear zone of the
However, the 3rd stage has been suggested [17]. In this stage, fracture surface notwithstanding the increase in the volume fraction of
deformation of martensite may takes place due to the change in the the martensite in the dual-phase steel due to the cold working, can be
morphology or strength reduction. But, in this research the 3rd stage was attributed to the grain refinement.
not seen. When the martensite islands are scattered in the ferrite matrix, micro
According to Table .4, the work hardening exponent values at the dimples begin to nucleate in the ferrite – martensite interface. Moreover,
first stage are greater than those in the second stage for each DP steels. the images of the fracture surface of the specimen without cold roll show

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F. Hosseinifar and A. Ekrami Materials Science & Engineering A 830 (2022) 142314

Fig. 13. Stereo graph taken from fracture surface of tensile specimens (a) 0DP, (b)20DP. (I) Shear zone, (II) Radial line (III) Fiber zone.

more cleavage planes, hence more brittle fracture. However, with

further progress of the cold roll process, i.e. increase in the volume
fraction of martensite as well as the reduction in the grain size, the
nucleation sites for dimples dwindle and their range increases, conse­
quently the growth and connection of dimples shift to higher strains,
which leads to the increase in the total elongation and impact energy.
Ductile fracture happens in 3 stages: Nucleation of dimples, growth
of dimples, and coalescence of the dimples. The nucleation of the dimple
in dual-phase steels occurs for three reasons [10]:

⋅ Formation of cracks in the martensite

⋅ Loss of coherency at the ferrite – martensite interface
⋅ Loss of coherency at the ferrite – ferrite interface

The number of dimples in the fracture surface depends on the

number of available nucleation sites. Since there’s a direct link between
the total elongation and the dimple’s size, enlargement of the dimples
leads to an increase in the total elongation [37].
According to Fig. 16 and Table .3, The larger average size of dimples
in the fracture surface of the 15% cold work dual-phase steel sample
validates the higher elongation of this specimen.
Fig. 14. Total elongation and area reduction of investigated dual phase steels.

Fig. 15. FE-SEM micrographs taken from fracture surfaces of tensile tested specimens. (a)0DP, (b)20DP.

9
F. Hosseinifar and A. Ekrami
Fig. 16. Average dimple size as a function of Martensite volume fraction and
Total elongation as a function of average dimple size.
5. Conclusion
The effect of cold rolling, prior to the inter-critical heat treatment, on
microstructure and mechanical properties of ferrite – martensite dual-
phase steels were evaluated. Results indicate that:
• With increasing the cold rolling before inter-critical annealing heat
treatment, the ferrite grain size decreased and volume fraction of
martensite increased.
• The ultimate tensile strength, the yield stress, the uniform and total
elongation increased with further progress of applied cold work. But
total elongation decreased with rolling reduction more than 15%.
• The strain hardening exponent of stage 1 (nI) and stage 2 (nII) of work
hardening increased with increasing the applied cold rolling.
• The impact energy and energy absorption capacity increased with
increasing the cold rolling.
10
Materials Science & Engineering A 830 (2022) 142314
• The fracture surface of the investigated dual-phase specimens
included cleavage planes and dimples, indicating mixture of ductile
and brittle fracture in these steels.
CRediT authorship contribution statement
F. Hosseinifar: Conceived and designed the experiments, performed
experiments, analyzed data, Writing – original draft. A. Ekrami:
conceptualized the main idea, reviewed and edited the manuscript.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgment
Financial support by the Sharif University of Technology, Iran is
gratefully acknowledged.
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