Materials Chemistry and Physics 257 (2021) 123721

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Materials Chemistry and Physics

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

Effects of spheroidization heat treatment and intercritical annealing on

mechanical properties and corrosion resistance of medium carbon dual
phase steel
Maryam Soleimani, Hamed Mirzadeh *, Changiz Dehghanian
School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, P.O. Box 11155-4563, Tehran, Iran

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• Spheroidization and intercritical

annealing of CK45 medium-C steel were
studied.
• Spheroidization improved ductility and
corrosion resistance but decreased
strength.
• Appropriate DP steel by short inter­
critical anneal after spheroidizing was
obtained.
• Low martensite content in medium-C
steel in the DP microstructure was
realized.

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

Keywords: Spheroidization heat treatment and intercritical annealing and their effects on the mechanical properties and
Medium carbon steel corrosion behavior of CK45 medium carbon steel were studied. Increasing the spheroidization time resulted in
Spheroidizing the decline of strength and hardness of the initial martensitic steel but improved the tensile ductility and
Intercritical annealing
corrosion resistance. Intercritical annealing of the spheroidized steels resulted in the formation of austenite at the
Mechanical properties
Corrosion current density
expense of cementite particles at short intercritical annealing times, which resulted in the development of dual
phase (DP) steels after water quenching. Increasing the holding time at the intercritical annealing temperature
led to a remarkable increase in the volume fraction of martensite in the microstructure, leading to poor ductility
and corrosion resistance. This processing route, however, made it possible to obtain low martensite contents via
short intercritical annealing of spheroidized steels, which resulted in the enhancement of strength-ductility
balance while maintaining appropriate corrosion resistance.

1. Introduction applications especially in the automotive industry [1–5]. On the other

hand, the corrosion resistance of DP steels is an important factor
Dual phase (DP) steels have a microstructure comprised of a ferritic affecting their durability and reliability [6–11].
matrix and a hard phase (normally martensite). Based on their excellent These properties can be tailored by altering the microstructure of DP
strength-ductility balance, they are suitable materials for industrial steels, which can be simply achieved by heat treatment [12–17]. The

* Corresponding author.
E-mail address: hmirzadeh@ut.ac.ir (H. Mirzadeh).

https://doi.org/10.1016/j.matchemphys.2020.123721
Received 15 May 2020; Accepted 16 August 2020
Available online 8 September 2020
0254-0584/© 2020 Elsevier B.V. All rights reserved.
M. Soleimani et al.
spheroidization treatment is one of the heat treatment methods to alter
the microstructure of steels. Different spheroidization routes [18–22],
the effect of spheroidization time [23,24], the effect of initial micro­
structure [24–26], and the effect of deformation [22,27–29] have been
studied in detail.
The spheroidization annealed low carbon steels have been recently
considered for intercritical annealing and processing of DP steels
[30–33]. During intercritical annealing of the spheroidized microstruc­
ture, the tendency to obtain martensite phase as discrete islands was
observed, which resulted in inferior strength-ductility balance compared
to the DP steel obtained from the intercritical annealing of martensitic
microstructure. These observations negated the usefulness of the
spheroidized microstructures as the initial ones for the processing of low
carbon DP steels [30]. However, in the case of medium- and high-carbon
steels, intercritical annealing usually leads to the high volume fraction of
hard martensite phase in the form of interconnected network, which
results in high wear resistance [34] but low ductility of the resultant
steels [12,35–39]. Therefore, the ductility issue limits their applications
compared to the low carbon DP steels. As a result, the spheroidization
annealing by producing the favorable sites for the formation of austenite
(and martensite after quenching) followed by controlled intercritical
annealing to adjust the volume fraction of martensite might be an
appropriate solution for these issues. Accordingly, the present work aims
to deal with this subject to develop DP steels with high strength,
ductility, and corrosion resistance from a commercial medium carbon
steel (CK45 steel).
It should be noted that the effect of spheroidization annealing on the
corrosion resistance of ferritic-pearlitic steels has been investigated
[40–42]. The galvanic effect between the anodic ferrite and the cathodic
cementite caused the corrosion of the ferritic-pearlitic microstructures
with lamellar cementite, which as a result led to high corrosion rates.
After spheroidization annealing and formation of discrete spherical
cementite particles, the corrosion rate decreased [41,42]. However,
intercritical annealing effects on the corrosion resistance of a spheroi­
dized microstructure have not been reported so far, which will be
treated in this work for the first time.
2. Experimental details
2.1. Processing
A commercial CK45 steel with chemical composition (wt%) of Fe-
0.476C-0.543Mn-0.274Si-0.094Cr-0.044Ni-0.019P-0.007S was used in
this work. Based on the Kasatkin equations [43,44], the critical Ac1 and
Ac3 temperatures were estimated as ~ 729 ◦ C and ~784 ◦ C, respec­
tively. The initial martensitic sheet was obtained by annealing at the
austenitization temperature of 900 ◦ C for 10 min followed by water
quenching. The spheroidization annealing was performed at the
subcritical temperature of 700 ◦ C [29,30] for different holding times up
to 24 h followed by water quenching. A code was assigned to each
spheroidization annealed sample as “SAx”, where x denotes the spher­
oidization annealing time in hours. The dual phase samples were pro­
cessed by intercritical annealing of spheroidization annealed samples at
775 ◦ C for different holding times up to 600 s, which was followed by
water quenching. A code was assigned to each intercritically annealed
sample as “SAx-IAy”, where y denotes the intercritical annealing time in
seconds.
2.2. Microstructural characterization
Microstructural features were revealed by pre-etching in the LePera’s
reagent (1 g Na2S2O5 in 100 ml H2O + 4 g C6H3N3O7 in 100 ml ethanol)
followed by etching in the 2% Nital solution for DP samples and by
etching in the 2% Nital solution for other samples. Afterwards, an
Olympus Vanox optical microscope and a FEI Nova FE-SEM were used
for microstructural characterization. A Bruker EDS detector integrated
2
Materials Chemistry and Physics 257 (2021) 123721
with a true standardless P/B ZAF correction was used for elemental
analysis. A Philips X-ray diffractometer (XRD) with Cu-Kα radiation was
also used for phase analysis.
2.3. Evaluation of mechanical properties
Vickers hardness test with a load of 5 kg was used for studying the
effects of spheroidization annealing time (decrease of hardness due to
the high temperature tempering of martensite [17,45]) and intercritical
annealing time (increase of hardness due to austenitization and trans­
formation of austenite to martensite during quenching). The average of
5 indentations was considered for each sample. Tensile test specimens
with the gauge length of 25 mm were prepared according to the subsize
ASTM E8 standard for room temperature tensile testing with the con­
stant cross-head speed of 1 mm/min. These tests were repeated once to
insure the reproducibility of the results.
2.4. Evaluating the corrosion resistance
A Solartron potentiostat (Model SI 1287) operating at the scanning
speed of 2 mV/s was used for corrosion tests in a 3.5 wt% NaCl solution
at room temperature. It was based on the three electrode configuration:
Saturated calomel and platinum as reference and counter electrodes,
respectively. The specimen surface was ground and polished and an area
of 1 cm2 was examined for each sample. These tests were repeated once
and it was found that the reproducibility of the results was in the valid
range. Moreover, using a Solartron impedance analyzer (Model SI
1260), the electrochemical impedance spectroscopy (EIS) measurements
under frequency ranged from 105 kHz to 10− 2 Hz at open circuit po­
tential with amplitude of 10 mV were also performed in a 3.5 wt% NaCl
solution at room temperature.
3. Results and discussion
3.1. Evolutions of microstructure and hardness
Fig. 1a depicts the evolutions of hardness and microstructure during
spheroidization annealing. It can be seen that the hardness of the as-
quenched martensitic sample (SA0 sample) decreases rapidly with
increasing the spheroidization annealing time, and reaches a plateau at
~ 16 h. The decline of hardness during spheroidization annealing is a
high temperature tempering of martesnitic steel [30,45], where the re­
covery processes and decreasing tetragonality due to carbon loss in the
form of carbide particles are dominant microscopic processes [17,45].
The change in the martesnitic microstructure can be clearly seen by
comparing the microstructures of SA0 and SA4 samples in Fig. 1a, where
a typical tempered martensitic microstructure [45] can be seen in the
latter. The formation of spheroidized carbides can be clearly seen in the
microstructure of SA12 sample. Increasing the spheroidization anneal­
ing time up to 24 h resulted in the coarsening of the spheroidized car­
bides as can be seen in the microstructure of the SA24 sample in Fig. 1a.
Fig. 1b illustrates the evolutions of hardness and microstructure
during intercritical annealing of spheroidization annealed samples. It
can be seen that the hardness of intercritically annealed samples origi­
nated from the SA4 sample are higher than those of the samples origi­
nated from the SA12 and SA24 samples. This is related to the lower
degree of tempering in the SA4 sample, which resulted in the DP steels
with higher hardness [17]. For the SA24 sample, it can be seen that by
increasing the intercritical annealing time, the hardness increased
sharply and then reached a plateau at ~300 s. The rise of hardness is
related to austenitization and then transformation of austenite to
martensite during quenching [6]. Hence, the amount of austenite
increased with increasing the holding time. The latter can be seen in the
microstructures shown in Fig. 1b. It can be seen that the volume fraction
of martensite increased from ~20% for SA24-IA60 sample to ~70% for
SA24-IA300 sample. The microstructures reveal that it is possible to
M. Soleimani et al.
Fig. 1. Evolutions of hardness and microstructure during (a) spheroidization annealing and (b) intercritical annealing of the spheroidization annealed samples.
adjust the amount of martensite by controlling the intercritical anneal­
ing time in this steel with much higher carbon content compared to the
usual low carbon DP steels. The microstructure of the SA24-IA60 sample
implies that the carbide particles of the SA24 sample are the main ori­
gins of the austenite phase during intercritical annealing.
Fig. 2a shows the XRD patterns for the samples. In the XRD pattern of
SA4 sample, some small peaks of carbides (cementite) were observed,
which became sharper for the SA24 sample and the rest of cementite
peaks are visible. Compared to the XRD pattern of the conventional
ferritic-pearlitic sample (shown in this figure for comparison), the
cementite peaks are much sharper in the SA24 sample while the volume
fraction of cementite in these samples is the same. However, it is well-
known that for a phase with a low volume fraction, increasing the par­
ticle size of that phase results in the sharper diffraction peaks [46]. The
average size of cementite particles for the SA4 and SA24 samples can be
determined from Fig. 2b–c as 102 nm and 440 nm, respectively. Fig. 2d
shows the EDS analysis of a carbide particle, which reveals that the
atomic ratio of Fe/C is 3.42. This is near the atomic ratio of 3, which
confirms the XRD results regarding the formation of Fe3C cementite
phase from the martensitic microstructure during spheroidization
annealing. After intercritical annealing for 300 s, however, Fig. 2a re­
veals that the intensity of the diffraction peaks of cementite decreased
sharply for the SA24-IA300 sample, which reveals the formation of
austenite at the expense of cementite particles.
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Materials Chemistry and Physics 257 (2021) 123721
3.2. Tensile properties
Tensile stress-strain curves of samples are shown in Fig. 3a. It can be
seen that the SA0 sample with martensitic microstructure shows very
high strength but low ductility. As can be deduced from the stress-strain
curve of SA4 sample, spheroidization annealing significantly enhanced
the ductility but led to a remarkable decline of strength, which can be
related to the tempering effects and formation of carbides as can be seen
in Fig. 2b. By increasing the spheroidization annealing time, the total
elongation (%EL) values increased but the values of ultimate tensile
strength (UTS) decreased as can be realized from the stress-strain curves
of SA12 and SA24 samples. For instance, the UTS and %EL of the SA0
sample is 1513 MPa and 2%, respectively; while the UTS and %EL of the
SA24 sample is 496 MPa and 40%, respectively.
Based on Fig. 3a, comparing SA4-IA60 with SA4, SA12-IA60 with
SA12, and SA24-IA60 with SA24 reveal that the intercritical annealing
treatment resulted in an increase in UTS but a decrease in %EL, which
can be related to the presence of martensite in the resulting ferritic-
martensitic microstructures [47–51] as shown in Fig. 1b. Based on the
stress-strain curves of SA24-IA60, SA24-IA90, and SA24-IA300,
increasing the intercritical annealing time resulted in an increase in
strength and a decline in ductility, which is related to an increase in the
amount of martensite as shown in Fig. 1b. It can be seen that the
SA24-IA300 sample with the equilibrium amount of martensite at
775 ◦ C (~70 vol%) shows high strength but very low ductility, which is
the main reason that developing DP steels from CK45 steel is not a
common practice. However, spheroidization annealing followed by
M. Soleimani et al. Materials Chemistry and Physics 257 (2021) 123721

Fig. 2. XRD patterns, SEM micrographs, and EDS analysis of samples.

intercritical annealing for optimum time (~90 s) resulted in the devel­ results indicate the good work-hardening capacity of this steel with DP
opment of a DP700/300 steel with UTS of 694 MPa, yield stress (YS) of microstructure.
312 MPa, and total elongation of 23%. The yield ratio (YS/UTS) of this Fig. 3b summarizes the tensile results. The strength-ductility dia­
sample is ~0.45, which is lower than 0.5 [52–54], and hence, these gram shows the typical banana-type diagram [55,56], where by

4
M. Soleimani et al. Materials Chemistry and Physics 257 (2021) 123721

Fig. 3. (a) Tensile stress-strain curves of spheroidization annealed and intercritically annealed samples and (b) A summary of tensile results.

decreasing UTS, the total elongation increased and the DP samples fol­ in corrosion rate [59,60]. Therefore, the EIS results confirm the polari­
lowed the trend seen for the spheroidization annealed samples. How­ zation results regarding the increased corrosion resistance.
ever, if the yield ratio is considered, the yield ratio of DP samples is Fig. 4b reveals that intercritical annealing of spheroidization
generally lower than 0.5 but that of spheroidization annealed samples is annealed samples resulted in an increase in icorr, which is related to
higher than 0.5. This actually shows the properties that the combined reappearance of the martensite phase in these DP samples [6–11]. In
spheroidization annealing and controlled intercritical annealing can fact, an increase in the intercritical annealing time led to an increase in
offer. icorr, which is due to an increase in volume fraction of martensite. The
Nyquist plots of Fig. 4c revealed that the diameter of the semicircular arc
decreased by increasing the intercritical annealing time, which indicates
3.3. Corrosion resistance
a decrease in corrosion resistance, and the Nyquist plot tends to be
similar to that of SA0 sample by increasing the volume fraction of
The corrosion resistance of samples was evaluated by polarization
martensite. This implies that controlling the amount of martensite is an
curves (Fig. 4a and b) and EIS Nyquist plots (Fig. 4c). The polarization
important issue. The value of icorr for SA24-IA90 sample is comparable to
curves of spheroidization annealed samples are shown in Fig. 4a, where
that of SA24 sample, which reveals that the corrosion resistance of this
the vales of icorr were determined based on the Tafel extrapolation
sample with appropriate amount of martensite is favorable. Moreover,
method [57,58].
the tensile test results of Fig. 3 confirmed the appropriateness of the
It can be seen that by increasing the spheroidization annealing time,
mechanical properties of this sample. Accordingly, the combined
the icorr decreases considerably. For instance, the icorr of SA0 and SA24
spheroidization annealing and intercritical annealing route is favorable
samples is 7.5 μA/cm2 and 0.8 μA/cm2, respectively. The enhanced
for obtaining a CK45 steel with appropriate mechanical and corrosion
corrosion resistance by increasing the spheroidization annealing time
properties.
can be related to the tempering effects on the martensitic microstruc­
ture, which enhances the corrosion resistance [17]. On the other hand,
4. Conclusions
the formation of cementite phase during spheroidization annealing leads
to the formation of a micro-galvanic couple between ferrite and
The mechanical properties and corrosion behavior of CK45 medium
cementite due to the difference in the electrochemical behavior of these
carbon steel as influenced by the spheroidization heat treatment and
phases [41,42]. However, the latter effect can be completely masked by
intercritical annealing were studied. The following conclusions can be
the huge tempering effects on the corrosion resistance [17]. Regarding
drawn:
the micro-galvanic couple, when the equilibrium amount of cementite
forms during spheroidization annealing, increasing the annealing time
(1) Spheroidization treatment of the initial martensitic steel resulted
results in the coarsening of cementite particles based on the ostwald
in the formation of cementite particles in a tempered martensite
ripening mechanism. Therefore, an increase in cementite particle size
microstructure. Increasing the spheroidization time led to the
means a decrease in their total surface and the formation of discrete
decline of strength and hardness but improved the tensile
spherical cementite particles, which caused a decrease in corrosion rate,
ductility and corrosion resistance. For instance, the UTS, %EL,
and hence, the sample SA24 indicated the best corrosion resistance
icorr of the initial martensitic steel were 1513 MPa,2%, and 7.5
among the considered samples. The Nyquist plots of Fig. 4c revealed that
μA/cm2, respectively; while those of the spheroidization
the diameter of the semicircular arc for the samples with longer spher­
oidization annealing time increased, which is an indication of a decrease

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M. Soleimani et al. Materials Chemistry and Physics 257 (2021) 123721

Fig. 4. (a) Polarization curves of spheroidization annealed samples, (b) Polarization curves of intercritically annealed samples, and (c) Nyquist plots of samples,
where the fitted equivalent circuit model is also shown for simulation purposes. Rs and Rp represent the solution and charge transfer resistance, respectively. CPE
corresponds to non-ideal capacitive behavior of the metal/solution interface.

annealed sample for 24 h at 700 ◦ C were 496 MPa, 40%, and 0.8
μA/cm2, respectively.
(2) Intercritical annealing of the spheroidized steels resulted in the
formation of austenite at the expense of cementite particles at
short intercritical annealing times, which resulted in the devel­
opment of dual phase (DP) steels with appropriate amount of
martensite after water quenching. This resulted in the enhance­
ment of strength-ductility balance by developing a DP700/300
steel with yield ratio of ~0.45 while maintaining appropriate
corrosion resistance (comparable to that of spheroidization
annealed counterparts).
(3) Long holding times at the intercritical annealing temperature led
to remarkable increase in the volume fraction of martensite in the
developed microstructures, which led to poor ductility and
corrosion resistance. This revealed the importance of controlling
the intercritical annealing time for tailoring the mechanical and
corrosion properties.
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.
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