Materials Science & Engineering A 633 (2015) 1–8

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Materials Science & Engineering A

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

Development of high strength hot rolled low carbon copper-bearing

steel containing nanometer sized carbides
M.P. Phaniraj a,1, Young-Min Shin a,b,1, Joonho Lee b, Nam Hoon Goo c, Dong-Ik Kim a,
Jin-Yoo Suh a, Woo-Sang Jung a, Jae-Hyeok Shim a,n, In-Suk Choi a,n
a
High Temperature Energy Materials Research Center, Korea Institute of Science and Technology, Seoul 136-791, Republic of Korea
b
Department of Materials Science and Engineering, Korea University, Seoul 136-701, Republic of Korea
c
Sheet Product Design Group, Hyundai Steel Co., North Industrial Street 1400, 343-823, DangJin 343-823, Republic of Korea

art ic l e i nf o a b s t r a c t

Article history: A low carbon ferritic steel was alloyed with Ti, Mo and Cu with the intention of achieving greater
Received 18 December 2014 increment in strength by multiple precipitate strengthening. The steel is hot rolled and subjected to
Received in revised form interrupted cooling to enable precipitation of Ti–Mo carbides and copper. Thermodynamic calculations
24 February 2015
were carried out to determine equilibrium phase fractions at different temperatures. Microstructure
Accepted 24 February 2015
Available online 10 March 2015
characterization using transmission electron microscopy and composition analysis revealed that the
steel contains
5 nm size precipitates of (Ti,Mo)C. Precipitation kinetics calculations using MatCalc
Keywords: software showed that mainly body centered cubic copper precipitates of size o 5nm form under the
HSLA steel cooling conditions in the present study. The steel has the high tensile strength of 853 MPa and good
Copper
ductility. The yield strength increases by 420 MPa, which is more than that achieved in hot rolled low
Nano-sized carbides
carbon ferritic steels with only copper precipitates or only carbide precipitates. The precipitation and
Interrupted cooling
Numerical simulation strengthening contribution of copper and (Ti,Mo)C precipitates and their effect on the work hardening
behavior is discussed.
& 2015 Elsevier B.V. All rights reserved.

1. Introduction
The long-standing goal in research on high strength steels has
been to increase the strength while maintaining the ductility,
toughness, weldability and cost effectiveness. In low carbon
ferritic steels the strength–ductility combination is achieved by
microalloying with elements such as Nb, V or Ti in the mill
processed condition without the requirement of an additional
heat treatment. The microalloying elements form nanocrystalline
carbides/carbonitrides which strengthen the ferrite matrix by
grain size refinement and precipitation strengthening. The con-
ventional microalloyed steels typically possess yield strengths in
the range 450–550 MPa [1,2], however significant improvements
in strength can be achieved by a combination of alloy design and
thermo mechanical processing followed by controlled cooling.
Recently, Funakawa et al. [3] reported an increase in yield
strength of 300 MPa in the hot rolled low carbon steel micro-
alloyed with Ti and Mo in equiatomic concentration. The hot rolled
n
Corresponding authors.
E-mail addresses: jhshim@kist.re.kr (J.-H. Shim),
insukchoi@kist.re.kr (I.-S. Choi).
1
The authors contributed equally to this work.
sheet was air cooled to 620 1C where phase transformation (γ-α)
was accompanied by precipitation of alloy carbides. The high
strength of the steel was due to ferrite grain size refinement
(
3 μm) and precipitation of nanometer size (Ti,Mo)C carbides
(
3 nm). Chen et al. [4] compared carbide size and hardness of
three continuously cooled ferritic steels containing the microalloy-
ing elements Ti, Ti–Mo and Ti–Nb respectively. They reported that
the Ti–Mo steel had the finest carbide size and highest hardness.
The relatively lower change in carbide size and hardness measure-
ments after different cooling rates lead them to conclude that the
carbide formed in the Ti–Mo steel was relatively thermally stable.
Copper addition in amounts of 1–2 wt% has also been used for
precipitation strengthening in low carbon structural steels [5–9].
Commercially available copper containing low carbon steels such as
ASTM A710 or HSLA80, also contain microalloying elements such as
Nb and have yield strength between 450 and 520 MPa [10,11] in the
as-rolled and air-cooled condition. The higher strength of these steels
is because of the formation of nanosized copper precipitates in ferrite
and grain refinement brought out by microalloy carbides in prior
austenite. Misra et al. [12] studied the effect of copper addition on the
mechanical properties of hot rolled V–Nb microalloyed steels. They
reported that increasing the copper content from 0.22 to 0.63 wt%
increased the yield strength by
25 MPa in the as rolled condition. In

http://dx.doi.org/10.1016/j.msea.2015.02.067
0921-5093/& 2015 Elsevier B.V. All rights reserved.
2 M.P. Phaniraj et al. / Materials Science & Engineering A 633 (2015) 1–8
order to increase the strength further they microalloyed the Cu–Nb–V
steel with Ti and Mo. The yield and tensile strength improved to
554 MPa and 658 MPa, respectively after aging the as-rolled speci-
men. The improvement in strength was due to ferrite grain refine-
ment (2–10 μm), and nano sized precipitates of copper and the
carbides: NbC, VC, Mo2C, Ti(Nb)C. The % elongation decreased with
increase in strength. Their results show that multiple carbide pre-
cipitates may not guarantee the yield strength superior to that
obtained in steels with fewer type of carbide precipitates [3,13].
In the present study the low carbon steel is alloyed with both
copper, and titanium and molybdenum with the intention of
synergizing their beneficial effect on mechanical properties. The
structure and properties of Ti–Mo and Cu–Ti–Mo microalloyed
steels were investigated to determine the contributions to
strength by Ti–Mo carbides individually and together with copper
precipitates. The thermo-kinetic software MatCalc has been used
to calculate evolution of copper precipitates in Fe–1.4% Cu alloy
[14] and in austenitic heat resistant steels by this paper's co-
authors [15]. In the present study MatCalc was used to calculate
the phase evolution and size distribution of copper precipitates.
2. Experimental and computational details
The compositions of steels designated as CMn, TiMo and CuTiMo
are given in Table 1. CMn is the base low carbon steel without any
precipitate forming elements. TiMo and CuTiMo are the CMn steel
microalloyed with titanium and molybdenum, and microalloyed with
copper, titanium and molybdenum respectively. The alloys were
prepared using vacuum induction melting into 5.7 kg ingots. The
ingots were forged and rolled at 1100 1C into 15 mm thick slabs. The
slabs were then heated to 1250 1C and held for 30 min to dissolve any
precipitates and then rolled to 75% reduction at 900 1C. After rolling
the specimens were first air cooled to 650 1C and held for 5 min,
followed by air cooling to 500 1C where it was held for 60 min and
then furnace cooled to room temperature. The precipitates viz. (Ti,
Mo)C carbide and Cu rich phase are expected to form at 650 1C
[3,4,16] and 500 1C [17,18] respectively.
The specimens for the tension test were prepared from the rolled
plates along the rolling direction according to ASTM standard E08-M
with gage length of 25 mm, gage width of 6 mm and thickness of
2 mm. The tests were carried out at the constant crosshead speed of
1 mm/min. The tension test experiments were conducted on two
specimens for each composition. The microstructure was character-
ized using scanning electron microscope (SEM), the 200 kV Tecnai
20 transmission electron microscope (TEM) and energy dispersive
spectroscopy (EDS). Focused Ion Beam (FIB) technique was used to
make thin foil specimens for characterization of precipitates in TEM-
EDS. The precipitates were also extracted by dissolution in the
electrolyte solution consisting of 4% tetramethylammonium chlor-
ide, 10% acetone and 86% methyl alcohol. The grain size was
determined from SEM micrographs with help of an image analyzer
using the linear intercept method. The precipitate size and distribu-
tion were determined from measurements in TEM micrographs on
up to 400 extracted particles.
The equilibrium phase fractions at different temperatures were
calculated using Thermo-Calc [19,20]. The data set of parameters
Table 1
Chemical composition (wt%).
Steel C Mn Si Mo Ti Cu Al
CMn 0.07 1.47 0.32 – – – 0.04
TiMo 0.07 1.34 0.32 0.20 0.09 – 0.04
CuTiMo 0.07 1.53 0.34 0.21 0.09 1.17 0.04
for the thermodynamic models describing the Fe–C–Mn–Si–Mo–
Ti–Cu system used in Themo-Calc was from the TCFE database
incorporated in the software. The phases included in the calcula-
tions were austenite, ferrite, cementite, fcc-copper, and MC (M ¼Ti,
Mo) carbide. A thermo-kinetic software MatCalc (version 5.30)
[21–23] was used to determine the precipitation kinetics and size
distribution of Cu precipitates and MC carbides. In MatCalc the
microstructure evolution is calculated based on the classical
nucleation theory. The evolution equations for the radius and
composition of each precipitate are derived from the thermody-
namic extremum principle. The thermodynamic and kinetic data
required for the simulation are calculated from the MatCalc
database ‘mc_steel’, version 1.18, and the MatCalc mobility data-
base ‘mc_sample_fe’, version 1.007. The following assumptions
were made for the simulation: (i) average grain size and disloca-
tion density of austenite is 50 μm and 1012 m  2, (ii) average grain
size and dislocation density of ferrite is 15 μm and 1013 m  2, (iii)
nucleation of bcc Cu and MC precipitates occurs on grain bound-
aries and dislocations, (iv) the austenite–ferrite transformation
occurs at 650 1C and (v) the bcc Cu precipitates transform into fcc
Cu precipitates when they grow in a range between 3–5 nm.
3. Results
3.1. Phase equilibria
The equilibrium phase fractions calculated using ThermoCalc
are plotted as a function of temperature in Fig. 1. In all the steels
cementite precipitates below
700 1C and precipitation of face
centered cubic (fcc) copper begins at around 750 1C. In steels
containing Ti and Mo MC carbide (NaCl structure) precipitates,
consisting mainly of TiC, start to form around 1150 1C. In these
steels the volume fraction of cementite is relatively lower than
that in CMn steel. The lower cementite content is expected
because some carbon is used up in the formation of MC type
precipitates.
3.2. Microstructure
The microstructure in all the steels consists mainly of polygonal
ferrite (Fig. 2). In the CMn steel cementite exists in pearlite form
whereas in TiMo and CuTiMo steels pearlite colonies are less
common. The latter is consistent with the calculations of equili-
brium phase fractions (Fig. 1) where it was noted that the lower
fraction of cementite was because some carbon was used in the
formation of MC carbides. The ferrite grain size of CMn steel is
16 μm whereas both TiMo and CuTiMo steels have relatively finer
grain size of 12 μm.
Fig. 3a is a TEM micrograph of the extracted nanometer size
carbide particles from TiMo steel. The electron diffraction pattern
from the precipitates shows that they have a typical face centered
cubic structure (Fig. 3b). The lattice parameter calculated based on the
diffraction ring diameter is 0.430 nm which is similar to that of TiC
(0.433 nm). The EDS spectrum shows that MC precipitates contains Ti
and Mo as main components (Fig. 3c). The copper peak (at
8 eV) in
the EDS spectrum is from the Cu grid that supports the carbon
extraction replica. The composition analyses showed that MC pre-
cipitates contain molybdenum and titanium in the atomic concentra-
tion ratio between 0.2 and 0.4. This indicates that the precipitates are
indeed (Ti,Mo)C precipitates. The precipitates have size in the range
Fe from 2 nm to 7 nm (Fig. 3d).
Fig. 4 shows the diffraction pattern and bright field and dark field
Bal. images from the foil specimen of the CuTiMo steel. The diffraction rings
Bal.
Bal.
for (110)-αFe and for (111) and (200) from TiC are overlaid on the
diffraction pattern. The diffraction pattern has been inverted i.e. the
 M.P. Phaniraj et al. / Materials Science & Engineering A 633 (2015) 1–8
Fig. 1. Calculated equilibrium phase fractions plotted as a function of temperature in (a) CMn steel, (b) TiMo steel and (c) CuTiMo steel.
diffraction spots are now black and the background is white-grey to
enable clearer identification of spots from carbide. The dark field image
for the spot marked A in the diffraction pattern shows the size of the
carbide particles. The particle size of the carbides in the present study
was measured, like in the TiMo steel, from transmission electron
micrographs of extracted precipitates and found to be in the range
from 2 nm to 8 nm (Fig. 4d). Composition analysis showed that the
Mo/Ti atomic concentration ratio, like in the TiMo steel, was in the
range 0.2–0.4.
In the CuTiMo steels the copper precipitates could not be identified
in the electron microscope. However, simulations using MatCalc for the
processing temperature–time conditions employed in the present
study showed that bcc-copper precipitation initiated in the ferrite
matrix and reached saturation (Fig. 5a) and fcc-copper precipitates
have begun to form. The precipitates are mainly body centered cubic
and their size is largely between 2.4 nm and 3 nm (Fig. 5b). A small
fraction of precipitates having size larger than 3 nm have transformed
to the face centered cubic structure. The
3 nm precipitates are fully
coherent with the matrix and cannot be observed in the TEM because
of poor diffraction contrast [24,25]. However, in a parallel unpublished
work, by the present authors, on a 1.7 wt% Cu steel under similar
processing conditions fcc-copper precipitates of size 6–13 nm formed
and could be easily identified.
3.3. Mechanical properties
The strength of the CMn steel increases with microalloying
additions significantly (Fig. 6a). The yield stress, σy, of the TiMo
steel (642 MPa) is more than 2.4 times that of CMn steel (Table 2).
The CuTiMo steel has the highest yield (732 MPa) and tensile
3
strength (853 MPa). The % elongation of both TiMo and CuTiMo
steels is similar (16%) but lower than that of the CMn steel (33%).
In order to compare the effect of alloying additions on the work
hardening rates, the engineering stress–strain curves were first
transformed into true stress–true strain curves. The data between
the yield stress and the maximum stress were then fitted to a
polynomial and this polynomial was then differentiated with
respect to strain. Fig. 6b shows the work hardening rate, dσ/dε
plotted as a function of the reduced flow stress, σ  σy, for the
three steels. Typically there is a high initial work hardening rate
followed by a decrease as deformation proceeds. The initial work
hardening rate increases from
3100 MPa in the CMn steel to

4100 MPa in the TiMo steel. The CuTiMo steel has an initial work
hardening rate marginally higher than the TiMo steel, however,
the slope of the work hardening rate curve is initially lower and in
the later stages of deformation is similar to the TiMo steel.
4. Discussion
4.1. Microstructure
The solubility of titanium in ferrite is low thereby cooling the
steels after hot rolling to 650 1C supersaturates ferrite and results
in the precipitation of alloy carbides during subsequent cooling.
The alloy carbide precipitates contained molybdenum and tita-
nium in the Mo/Ti atomic concentration ratio of 0.2–0.4 indicating
that they could have formed over range of temperatures. A
thermodynamic equilibrium calculation was carried out to deter-
mine the Mo/Ti atomic ratio as a function of temperature. The Mo/
Ti atomic concentration ratio decreased with increasing
4 M.P. Phaniraj et al. / Materials Science & Engineering A 633 (2015) 1–8
Fig. 2. SEM micrographs of the steels after hot rolling and cooling: (a) CMn steel, (b) TiMo steel and (C) CuTiMo steel.
temperature and reached 0.2 at
600 1C (Fig. 7). Therefore the
precipitates observed in the present study have most likely formed
below 600 1C. Chen et al. [4] have reported similar precipitation
from supersaturated ferrite when they cooled (Ti,Mo)C forming
steels at different cooling rates.
The Fe-base copper alloys [5,24,26] on aging, usually in the
temperature range 400–650 1C, initially form metastable bcc
copper precipitates. As these precipitates grow they transform to
the 9R structure [27] and then at relatively larger size to the stable
fcc structure. The metastable bcc structure is maintained up to a
size of 2.4–3 nm [18,28]. The peak hardness during aging is
achieved when the precipitates have the bcc structure. The size
of copper precipitates in the CuTiMo steel is largely between
2.4 and 3 nm. Thereby, the strengthening due to copper precipi-
tates in the CuTiMo steel should be analogous to that of the steel in
the peak aged condition. Indeed the significant improvement in
yield strength after adding copper to the TiMo steel, calculated in
the next section, is mainly due to the bcc copper precipitates.
4.2. Estimating precipitation strengthening contributions
The base composition of the steels is similar to CMn steel and
the microstructure consists mainly of ferrite with some pearlite.
Thereby the contribution to yield strength after alloying can be
estimated by deducting the yield strength of CMn steel. The
contribution to yield strength from precipitates can be determined
after accounting for solid solution strengthening and grain size
strengthening using Eq. (1).
σ ppt ¼ σ YS  σ CMn
YS  Δσ g  σ Cu ð1Þ
where Δσg is the increment in the contribution because of the
slightly finer grain size of TiMo and CuTiMo steels, when com-
pared with CMn steel, calculated using 17.402 d  1/2 [3,29] and σCu
is the contribution from solid solution strengthening by copper
(38 MPa per wt% Cu [1]). The amount of copper remaining in
solution after precipitation was calculated to be 0.7 wt%; this
amount was used to calculate σCu in Eq. (1). The solubility of
titanium and molybdenum in ferrite is low and is assumed to have
negligible solid solution strengthening effect. The precipitation
strengthening contributions calculated using Eq. (1) are given in
Table 2. The increment in yield strength due to precipitation in
TiMo steel is 347 MPa. This is comparable to the 340 MPa
improvement in yield strength reported on low carbon steels
alloyed with Ti and Mo and processed under different conditions
[3]. The precipitation strengthening contribution in the CuTiMo
steel is 420 MPa which is more than one and half times the yield
strength of the CMn steel.
 M.P. Phaniraj et al. / Materials Science & Engineering A 633 (2015) 1–8 5

Fig. 3. (a) TEM micrograph showing precipitates extracted from TiMo steel, the corresponding, (b) fcc diffraction pattern, (c) EDS Spectrum from the precipitates, and
(d) distribution of carbide size.

4.3. Work hardening
In a matrix with non-shearable precipitates the moving dis-
locations bypass the particle forming a loop around the particle
rather than cut it. Thereby, the effective spacing between particles
is effectively reduced and the stress required to move another
dislocation past the particle increases according to the Ashby–
Orowan mechanism [30]. The dislocation loop exerts a back stress
which must be overcome for additional slip to take place. Conse-
quently the matrix strain hardens rapidly as more dislocation
loops form around the particle. The (Ti,Mo)C precipitates, formed
in the present study, are hard and the dislocations should by pass
6 M.P. Phaniraj et al. / Materials Science & Engineering A 633 (2015) 1–8

Fig. 4. (a) Bright field and (b) dark field image corresponding to the spot marked A in the diffraction pattern (c) from the CuTiMo steel and (d) size distribution of extracted
precipitates.

Fig. 5. Kinetics of copper precipitation in CuTiMo (a) and precipitate size distribution (b).

the particles, form loops around them, and thereby give rise to the Copper precipitates are elastically soft and can be sheared by
significantly higher work hardening rate (Fig. 6). Indeed dislocation the moving dislocations [26]. Nakashima et al. [32] have reported
loops have been observed in deformed (Ti,Mo)C forming steels [31]. that in Fe–Cu alloys moving dislocations cut and pass through
 M.P. Phaniraj et al. / Materials Science & Engineering A 633 (2015) 1–8 7

Fig. 6. Engineering stress-elongation (a) and work hardening rate-reduced stress (σ  σy) curves (b) for CMn, TiMo and CuTiMo steels.

Table 2 deformation (Fig. 6b). Similar arguments have been posed by

Measured yield strength (YS), tensile strength(TS), % elongation and calculated Militzer et al. [35] in their study where Fe–Cu alloys exhibited
precipitation strengthening contribution and increment in YS due to finer grain size higher work hardening rate when the size of copper precipitates
(Δσg). was close to the size at which transformation occurs. However,
Steel YS (MPa) TS (MPa) % Elongation σppta (MPa) Δσg (MPa)
further study is needed to validate the hypothesis of the dynamic
transformation and the associated change in the hardening rate.
CMn 267 401 33 – –
TiMo 642 770 16 354 21
4.4. Ductility
CuTiMo 732 853 16.6 417 21

a
σppt is the increment in yield strength due to precipitates. Ductile failure is initiated by nucleation of voids at hard second
phase particles such as carbides and nitrides in steels. At large
strains the dislocation structure around the particle imposes high
local stress that upon reaching a critical value will cause decohe-
sion of the particle/matrix interface thereby nucleating a void.
Particles as small as 5 nm have been found to nucleate voids [36].
The relatively lower ductility of the TiMo steel when compared
with the CMn steel is thereby likely due to void nucleation at the
carbide/matrix interface. Typically, increasing the volume fraction
of hard second phase decreases the ductility [37,38]. However,
there is no decrease in the ductility of the CuTiMo steel where the
matrix has copper precipitates in addition to carbide particles. This
is because, as noted above, the moving dislocations cut and pass
through the relatively soft copper particles resulting in only a
marginal increase in work hardening rate. Consequently the
increase in the local stress is lower than that required for
particle–matrix decohesion and the ductility remains unaffected.

Fig. 7. The atomic concentration ratio Mo/Ti in MC carbide precipitates in TiMo
steel, obtained from thermodynamic equilibrium calculations, plotted as a function
of temperature.
copper particles of size up to 70 nm. Once the particles are sheared
the resistance to further dislocation motion decreases which
should result in the lowering of the macroscopic strain hardening
rate [33,34]. The increase in strength on copper addition and
marginal increase in the initial work hardening rate (Fig. 6), when
compared with the TiMo steel, are in accordance with the
hypothesis noted above. However, the macroscopic work hard-
ening rate becomes similar to the TiMo steel in the later stages of
deformation. This could be explained as follows. The copper
precipitates in the present study have a size close to the size at
which transformation to the 9R structure [27] occurs. It is possible
that during deformation bcc copper particles with size around
3 nm transformed to the stronger 9R structure which increased
the hardening rate such that the slope of the work hardening rate
curve becomes similar to the TiMo steel in the later stages of
5. Summary and conclusions
Three low carbon steels: a plain low carbon steel, microalloyed
with Ti and Mo, and microalloyed with Cu, Ti and Mo were
prepared and subjected to hot rolling followed by interrupted
cooling. ThermoCalc was used to determine equilibrium phase
fractions at different temperatures. MatCalc was used to simulate
the precipitation kinetics and determine size distribution of
copper precipitate. The microstructure was characterized using
SEM, TEM and EDS. The specimens were tested in tension to
determine mechanical properties.
1. Alloying with Cu, Ti and Mo increases the yield strength of the
low carbon ferritic steel from 267 MPa to 732 MPa and tensile
strength from 401 MPa to 853 MPa.
2. Fcc (Ti,Mo)C carbides of
5 nm diameter and bcc Cu-rich
precipitates of o5 nm diameter form in the ferrite matrix.
3. The increment in yield strength due to the precipitation
strengthening effect of carbides in the TiMo steel is 347 MPa.
8 M.P. Phaniraj et al. / Materials Science & Engineering A 633 (2015) 1–8
The alloy carbides are hard and moving dislocations by-pass,
form loops around them giving rise to the significantly higher
work hardening rate.
4. The precipitation strengthening contribution of copper and
carbide precipitates jointly, in the CuTiMo steel, is 420 MPa.
This is more than the increments in yield strength that would
be achieved with only copper precipitates or only carbide
precipitates. Though the total fraction of precipitates in the
CuTiMo steel has increased the ductility is not adversely
affected because of the shearable copper precipitates.
Acknowledgments
The authors gratefully acknowledge the financial support
provided by the Korea Institute of Science and Technology (Grant
nos. 2E25322 and 2Z04520).
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