Materials and Design 63 (2014) 42–49

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Materials and Design

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Copper precipitation and its impact on mechanical properties in a low

carbon microalloyed steel processed by a three-step heat treatment
W.H. Zhou a,b, H. Guo a, Z.J. Xie a, C.J. Shang a,⇑, R.D.K. Misra b
a
School of Materials Science and Engineering, University of Science and Technology, Beijing, China
b
Laboratory for Excellence in Advanced Steel Research, Center for Structural and Functional Materials, Institute for Material Research and Innovation, University of Louisiana
at Lafayette, P.O. Box 44130, Lafayette, LA 70503, USA

a r t i c l e i n f o a b s t r a c t

Article history: The structure–mechanical property relationship, with particular focus on effect of tempering process on
Received 1 April 2014 the microstructural evolution and mechanical properties was investigated in a low carbon Cu-bearing
Accepted 27 May 2014 steel that was processed in three-steps, namely, intercritical annealing, intercritical tempering, and tem-
Available online 11 June 2014
pering heat treatment. The objective of adopting three steps was to elucidate the nature and evolution of
microstructural constituents that contributed to high strength–ductility combination in the studied steel.
Keywords: The three-step processing led to a microstructure primarily comprising of ferrite, retained austenite, and
Microalloyed steel
small amount of bainite/martensite. The mechanical properties obtained were: yield strength > 720 MPa,
High strength
Ductility
tensile strength > 920 MPa, uniform elongation > 20%, total elongation > 30%, and low yield ratio of 0.78.
Retained austenite The tempering step led to a significant increase in both yield and tensile strength and decrease in yield
Mechanical properties ratio, without reducing ductility, a behavior attributed to the precipitation of copper in retained austenite
Copper precipitation and ferrite. The precipitation of copper enhanced the stability of retained austenite and work hardening
rate, leading to a high volume fraction of retained austenite (29%), with consequent increase in elonga-
tion and significant increase in yield and tensile strength during tempering.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction to obtain high strength in steels [4–6]. By introducing precipitation

Restrictions on energy consumption and safety concern in
structures have motivated the development of new advanced high
strength steels (AHSSs). They are characterized by excellent combi-
nation of strength and ductility at a reasonable cost. In response to
this demand, retained austenite-containing steels have attracted
significant attention and are considered promising futuristic mate-
rials because of transformation-induced plasticity (TRIP) effect. The
TRIP effect provides high strength–ductility combination. In TRIP
process, C–Mn–Si TRIP-aided steel with tensile strength grade of
780–1470 MPa was obtained. In these steels, the microstructure
consisted of fine bainitic lath and considerable volume fraction of
retained austenite [1]. The yield strength was further enhanced
to GPa range by replacing the bainitic matrix with martensite
through the Q–P process [2,3]. In this regard, potentially innovative
heat treatments for processing of AHSS are TRIP and quenching and
partitioning (Q&P).
It is now widely recognized that precipitation strengthening is
an effective method to improve strength and has been employed
⇑ Corresponding author. Tel.: +86 010 62322428; fax: +86 10 62332428.
E-mail address: cjshang@ustb.edu.cn (C.J. Shang).
in TRIP-based systems, a good combination of strength and ductil-
ity can be achieved [7]. The disadvantage of conventional TRIP and
Q&P steels is that they generally exclude precipitation strengthen-
ing. The strength of TRIP and Q&P steels can be enhanced through
precipitation strengthening. Compared with the C–Mn–Si tradi-
tional TRIP steels, the addition of Nb, Mo, V led to significant
increase in both yield and tensile strength. The precipitation in
both ferrite and austenite led to 800–1000 MPa tensile strength
in TRIP steels [8,9]. The Nb-bearing Q–P steels exhibited high
strength-high ductility combination after tempering. This
improvement was attributed to the precipitation of niobium [10].
Based on this theory, microalloyed TRIP-aided and quenched, par-
titioned, and tempered (Q–P–T) steels are being explored.
The precipitation of copper occurs during aging because of low
solubility of copper in ferrite. The addition of copper in steel
enhances yield strength via precipitation strengthening, and can
be further encouraged to precipitate during aging in the tempera-
ture range of 500–550 °C [11,12]. Moreover, copper as an austenite
stabilizing element, is expected to stabilize austenite. However,
studies dealing with the stabilization of austenite via copper are
limited. Furthermore, multi-step intercritical heat treatment has
been proposed to be beneficial in stabilizing retained austenite

http://dx.doi.org/10.1016/j.matdes.2014.05.059
0261-3069/Ó 2014 Elsevier Ltd. All rights reserved.
 W.H. Zhou et al. / Materials and Design 63 (2014) 42–49 43

[13,14]. In the low Ni-content steel, it is difficult to obtain high Ni

containing laths that will form retained austenite during one-step
tempering, thus a two-step successive treatment is required. In the
first step conducted at high temperature, laths of intermediate Ni-
content were obtained and the second step was performed at
lower temperature to obtain high-Ni laths, and consequently,
retained austenite was obtained [13]. A similar approach was used
in the design of 5Mn steel [14]. Thus, it is appropriate to combine
these factors via a multi-step heat treatment process and obtain
excellent strength–ductility combination in Cu-bearing steels.
It was recently demonstrated that a good combination of
strength and ductility can be obtained through a two-step inter-
critical heat treatment in a low carbon microalloyed steel [15].
The combination of retained austenite and nano-scale precipitation
provided superior mechanical properties. However, the application
of high intercritical tempering temperature of 660 °C was respon- Fig. 1. Schematic diagram of three-step heat treatment. Cooling method in each
step is air cooling.
sible for inadequate precipitation. Also, copper precipitation was
delayed in Nb-microalloyed steels [16]. Thus, the precipitation
strengthening effect was incomplete in the two-step heat treat-
ment. It is therefore important to introduce a tempering process
to take advantage of copper in terms of precipitation strengthening
and stabilization of austenite.
Based on the above discussion, the objective of the study
described here is to explore microstructure–mechanical property
relationship, with focus on the effect of tempering, on mechanical
properties in a low carbon Cu-bearing steel. The steel was pro-
cessed through a three-step intercritical annealing, intercritical
tempering, and tempering heat treatment process.

2. Experimental procedures

The nominal chemical composition of the alloy in weight% was

Fe–0.11C–2.01Mn–0.78 Si–0.78Al–0.076–Nb–1.04Cu–1.00Ni–
0.26Mo. Niobium was added for grain refinement and precipitation
strengthening, while Cu and Mo were added for precipitation
strengthening. The phase transformation temperature, Ac1 and
Ac3, were measured to be 658 °C and 929 °C, respectively.
The steel was melted in a vacuum induction furnace and cast as
a 40 kg ingot and forged in the shape of a block prior to hot rolling.
The forged blocks were first homogenized by reheating to 1200 °C
for 2 h. Next, they were hot rolled to 8 mm thickness via six passes
and air-cooled to room temperature. The microstructure of as-hot
rolled steel comprised of bainite and martensite constituents. The
optimal annealing and tempering temperatures selected were
780 °C and 660 °C, respectively, for two-step intercritical heat
treatment, based on our previous study [15]. The third step of tem-
pering was carried out at 500 °C to obtain fine-scale precipitation
of copper.
Tensile specimens were machined to gauge length of 25 mm
and diameter of 5 mm according to ASTM: E8 specification. Stan-
dard tensile tests were conducted at room temperature using com-
puterized tensile testing system.
Fig. 1 is a schematic of the heat treatment process. Samples Fig. 2. Engineering stress–strain (a) and true stress–strain (b) plots of experimental
steel heat treated using different steps. Sample A-intercritical annealed, sample
were intercritical annealed at 780 °C for 30 min and then air-
B-intercritical annealed and intercritical tempered, sample C-intercritical anneald,
cooled to room temperature (sample A). Another sample desig- intercritical tempered, and tempered.
nated as sample B, was subjected to a subsequent intercritical tem-
pering process at 660 °C for 30 min. After this two-step heat
treatment, sample C was tempered at 500 °C for 30 min and air electron microscope operated at 20 kV. The EBSD scans were car-
cooled to room temperature. ried out in step size of 100 nm. The volume fraction of retained
Heat treated samples were mechanically polished using stan- austenite was determined by X-ray diffraction (XRD), using peak
dard metallographic procedure and etched with 2% nital for the intensity of (2 0 0)a, (2 1 1)a, (2 0 0)c, (2 1 1)c and (3 1 1)c.
examination of microstructure. Microstructural characterization Transmission electron microscopy (TEM) studies were carried
was carried out using scanning electron microscopy (SEM) in con- out to characterize reversed austenite and nano-scale precipita-
junction with electron back scatter diffraction (EBSD). SEM was tion. 3 mm TEM disks were punched from the foils and twin-jet
performed using a ZEISS ULTRA-55 field emission scanning polished using an electrolyte consisting of 5% perchloric acid and
44 W.H. Zhou et al. / Materials and Design 63 (2014) 42–49
95% ethanol. TEM was carried out using JEOL JEM-2100 FS TEM
operated at 200 kV.
3. Results and discussion
3.1. Mechanical properties
Engineering and true tensile stress–strain plots of heat treated
samples A, B, and C are presented in Fig. 2. Two types of stress–
strain plots were obtained. They were characterized by continuous
and discontinuous yielding. The one-step as-annealed steel (sam-
ple A) had lower yield strength and indicated continuous yielding.
While the two-step processed steel (sample B) exhibited discontin-
uous yielding with a defined yield plateau similar to the three-step
processed steel (sample C). It is known that the discontinuous
yielding is related to interaction between dislocations and intersti-
tial solute element (carbon). In dual-phase steels, when the dislo-
cation density in ferrite is low, discontinuous yielding occurs
[17], which has been observed in TRIP steels [18,19]. Thus, it is
envisaged that discontinuous yielding is related to reduction in
dislocation density caused by tempering. In comparison to sample
A, samples B and C indicated improvement in yield strength and
elongation. In spite of loss in tensile strength, samples B and C
were characterized by a good combination of strength and ductil-
ity. After the tempering process, sample C exhibited superior
mechanical properties: yield strength 720 MPa, tensile strength
920 MPa, uniform elongation 21%, total elongation 31%, and
yield ratio 0.78. The product of tensile strength and total elonga-
tion was 30 GPa%, which is remarkable for steels with yield
strength greater than 700 MPa.
Generally, the increase in yield strength is accompanied by a
drop in tensile strength and relative increase in yield ratio during
Fig. 3. Representative SEM micrographs of experimental steel illustrating the general microstructure. (a) Ferrite–bainite/martensite microstructure in sample A, (b and c)
multi-phase microstructure consisting of ferrite, retained austenite, and tempered bainite/martensite in samples B and C, respectively, and (d) volume percentage of different
phases in the microstructure.
the tempering process. Surprisingly, an opposite behavior was
observed in samples B and C. After tempering, the yield strength
was increased from 707 MPa to 723 MPa, and the tensile strength
was increased by 9% (from 845 MPa to 923 MPa). There was small
change in elongation (uniform elongation: from 23% to 21%,
total elongation: from 35% to 31%). The above behavior is an unu-
sual behavior observed in the experimental steel.
3.2. General microstructure
Scanning electron micrograph (SEM) of as-annealed steel (sam-
ple A) indicated a typical dual-phase microstructure consisting of
ferrite and bainite/martensite (Fig. 3a). Whereas, the annealed
and tempered steel (sample B) was characterized by a multi-phase
microstructure comprising of ferrite, retained austenite, and bai-
nite/martensite constituents (Fig. 3b). A similar observation was
made with sample C (Fig. 3c). In Fig. 3d, a summary of the percent-
age of different phases is presented. The fraction of ferrite
increased from sample A to sample C, while bainite/martensite
fraction followed an opposite behavior and decreased from sample
A to sample C. Since the tempering temperature was far below the
A1 temperature, the microstructure was expected to remain
unchanged. However, recovery during the tempering process
reduced the dislocation density in bainite/martensite constituents.
In this condition, the bainite/martensite with low dislocation
density is referred as ferrite. This is the reason for the decrease
in bainite/martensite during the tempering process.
The retained austenite characterized using EBSD is presented in
Fig. 4. The volume fraction of retained austenite in sample A was
low, while it was significantly high in samples B and C (Fig. 4a–c).
An estimate of retained austenite obtained using XRD data indi-
cated that the retained austenite content was 29% in samples B
 W.H. Zhou et al. / Materials and Design 63 (2014) 42–49 45

Fig. 4. EBSD characterization showing distribution of retained austenite in (a) sample A, (b) sample B, and (c) sample C. (d) XRD spectra illustrating different volume fraction
of retained austenite in samples A, B, and C. Size-distribution histogram of retained austenite in sample B (e) and sample C (f).

and C (Fig. 4d). The average diameter of retained austenite grains in
sample B and C was 0.30 lm and 0.35 lm, respectively (Fig. 4e
and f).
In conventional TRIP steels, retained austenite has a carbon con-
tent in the range of 1.1–1.7 wt%, while in our case, the carbon con-
tent was 0.5% [15]. It is believed that carbon enrichment did not
occur during the second and third step, because the lattice con-
stant ac that determines the carbon concentration was similar,
based on XRD peaks, namely (2 0 0)c, (2 2 0)c, and (3 1 1)c. There
can be two reasons for such a behavior. First, manganese and nickel
addition lowered T0 temperature, where austenite and ferrite of
similar chemical composition have identical free energy [20], such
that the carbon concentration in austenite at T0 temperature was
reduced [1]. Second, NbC and/or (Nb,Mo)C carbide precipitates
consumed carbon, leading to low carbon-content in the retained
austenite. Despite the low carbon-content, the retained austenite
had high stability because of enrichment with Mn and Ni.
It was interesting to note that the high volume fraction of
retained austenite was retained and not decomposed during tem-
pering at 500 °C. The decomposition temperature of retained aus-
tenite is governed by its stability [21,22]. Retained austenite with
high stability has high decomposition temperature, which means
that retained austenite can be stable even at high temperatures.
Additionally, the increase in carbon-content in retained austenite
is favorable for decomposition of retained austenite into a+M3C
because of high chemical driving force for nucleation of carbides
[22]. In our case, the retained austenite was stabilized by Mn and
Ni. Second, the retained austenite had low carbon-content and
the formation of cementite was suppressed by the addition of Si
and Al. Third, copper enrichment and precipitation in retained aus-
tenite is believed to be beneficial in stabilizing retained austenite,
and is discussed in the next section. Thus, if we consider the above
factors, retained austenite was stabilized without undergoing
decomposition during the tempering process.
3.3. Fine-scale microstructure
The TEM micrographs of three-step heat treated sample (sam-
ple C) is presented in Fig. 5. The retained austenite was blocky
and acicular in shape and present between laths of ferrite or at fer-
rite/bainite or martensite phase boundaries (Fig. 5a). Retained aus-
tenite was in the size range of 100–400 nm. Precipitation was less
uniform (Fig. 5a–c) and some ferrite and bainitic laths contained
low density of precipitates, while others had high density of pre-
cipitates (Fig. 5a and b). It is believed that former precipitates were
formed during annealing, when ferrite was depleted of alloying
elements. On the other hand, latter precipitates nucleated during
recovery of alloying element-enriched bainite/martensite. Further-
more, the tempering process reduced the dislocation density in the
microstructural constituents. In addition to the enrichment of
46 W.H. Zhou et al. / Materials and Design 63 (2014) 42–49
Fig. 5. Representative TEM micrographs of sample C showing (a) precipitates in retained austenite (marked by white dash line) and some ferrite; (b) enrichment of Mn, Ni
and Cu in retained austenite as determined by EDS; (c–e) bright and dark field images, and diffraction pattern of retained austenite with large majority of precipitates.
austenite with Mn and Ni, the EDX analysis indicated an increase in
the concentration of Cu in retained austenite in comparison to the
surrounding ferrite matrix (Fig. 5b). In retained austenite, large
fraction of copper-containing precipitates of size range 10–
15 nm were observed. This observation suggests the possibility of
enrichment of retained austenite with copper.
It is known that copper has high solubility in austenite. Never-
theless, copper precipitation has been previously observed in
austenitic stainless steels [23–25]. The fcc copper precipitates were
formed from the copper-rich zones during the aging process and
grew slowly with increase in aging time. Thus, high copper content
(>2 wt%) and long aging duration (>2 h) were the underlying rea-
sons for the precipitation of copper. It is unreasonable to apply
the above mentioned reasons to explain copper precipitation in
retained austenite in our case because of low copper-content and
short tempering time.
In our case, the reversion transformation is responsible for cop-
per-enrichment and it is believed that alloy-rich reversed austenite
and alloy-depleted ferrite are obtained in the intercritical region.
The concentration of alloying elements is governed by the inter-
critical temperature. In Cu-bearing steels, the start temperature
for copper precipitation was 680 °C and the peak temperature
was 500–550 °C [11,12]. This means that the diffusion of copper
is the dominant reaction at 780 °C and 660 °C. The diffusion dis-
tance is related to 2Dt1/2, where D is the diffusion coefficient, and
t is the aging time. The value of D can be calculated using activation
energy and pre-exponential constant from the literature [26]. The
diffusion distance of copper in the three steps was estimated to
be 970 nm, 120 nm and 2.7 nm, respectively (Table 1). If the
distribution of copper was uniform, then it is possible that copper
diffused from ferrite to adjacent reversed austenite because of the
fine size of ferrite grains. Meanwhile, copper precipitates were
observed in some large ferrite grains and in some ferrite that
was transformed from Cu-rich bainite/martensite during temper-
ing. This is the reason for non-uniform precipitation of copper in
ferrite after tempering. Moreover, the alloy enrichment in reversed
austenite decreased the A1 temperature such that the reversion
transformation restarted at a lower temperature in this region. This
led to the occurrence of reversion transformation in some part of
the alloy-rich zones during the tempering step. This repeated
reversion transformation and alloy enrichment increased the cop-
per-content in the reversed austenite. Furthermore, copper enrich-
ment may take place at the phase boundary, where nucleation of
reversed austenite occurs. Thus, copper was enriched in reversed
austenite, when reversion transformation occurred. Therefore, high
fraction of copper was precipitated in retained austenite.
Table 1
The diffusion distance of copper at different step in ferrite.
Temperature (°C) Diffusion coefficient Diffusion distance (nm)
DCu (cm2/s) (2DCut)1/2, t = 30 min
780 2.6  10 12
970
14
660 4.0  10 120
17
500 2.0  10 2.7
 W.H. Zhou et al. / Materials and Design 63 (2014) 42–49
3.4. Microstructural evolution mechanism
On the basis of previous work using two-step intercritical heat
treatment [15] and present study, the microstructural changes in
the behavior of experimental steel are illustrated in Fig. 6 and
are described as follows.
Intercritical annealing: When the steel was reheated at a temper-
ature between A1 and A3 temperature, a dual-phase microstructure
comprising of ferrite and reversed austenite was obtained.
Reversed austenite was enriched with carbon, manganese, nickel,
and copper during this step. Bainite/martensite with high density
of dislocations that were transformed from unstable reversed aus-
tenite contained high concentration of these alloying elements.
Some Nb-containing particles also precipitated in ferrite and bai-
nite/martensite.
Intercritical tempering: On tempering steel at a temperature
slightly above the A1 temperature, the bainite/martensite experi-
enced a ? c reversion transformation. The enrichment of alloying
elements again occurred in reversed austenite. The reversed aus-
tenite was adequately stable to be retained at room temperature.
Fine Nb-containing precipitates and some copper precipitates were
formed during this step and the dislocation density was decreased.
Tempering: On heating the steel below A1 temperature, exten-
sive precipitation of copper occurred in retained austenite and in
some ferrite. Bainite/martensite transformed to ferrite because of
recovery. The dislocation density was decreased in this step and
the retained austenite remained stable.
3.5. The effect of copper precipitation on the mechanical behavior
The copper precipitation in retained austenite increased the sta-
bility of retained austenite, and significantly influenced the
mechanical properties. The work hardening rate as a function of
true strain is presented in Fig. 7. In sample A, the work hardening
rate decreased with increase in true strain, while three stage work-
hardening behavior was observed in samples B and C (Fig. 7a): the
working hardening rate was first decreased (stage I), and then
increased (stage II), followed by a final decrease (stage III). This
behavior is consistent with the observation in 0.25C–5Mn steel
[27]. This three stage work hardening behavior and high work
hardening rate has not been previously reported in conventional
low alloy steels and TRIP steels [1,28].
Fig. 6. Schematic illustration of microstructural evolution in stage I through III of experimental steel during three-step heat treatment.
47
If compare samples A with B, it is apparent that the increase in
work hardening rate in stage II is induced by TRIP effect of retained
austenite. Although samples B and C had similar retained austenite
content of 29%, the work hardening rates were significantly dif-
ferent in stage II. The maximum work hardening rate in the transi-
tion stage (i.e., stage II to stage III) was 2 GPa for sample B and
3 GPa for sample C. This implies that there are other factors that
contributed to the difference in work hardening rates, in addition
to the TRIP effect of retained austenite.
From the microstructural observations, the enhancement of
work hardening rate can be attributed to copper precipitation in
the retained austenite. First, copper is an austenite stabilizing ele-
ment and its enrichment in austenite favors stability. Second, cop-
per precipitates pin dislocations in retained austenite during
deformation, which delays transformation of austenite to martens-
ite. Finally, copper precipitates have fcc structure, and dislocations
can cut through them, relaxing the stress concentration in the
retained austenite.
To further enhance our understanding, Kocks–Mecking analysis
(work hardening rate as a function of true stress) was conducted.
Fig. 7b shows that the hardening effect begins at a higher stress
of 750 MPa in sample C, as compared to 700 MPa in sample B.
This suggests that the retained austenite had higher stability. Fur-
thermore, the higher work hardening plateau in sample C sug-
gested that copper precipitates contributed to work hardening
rate by Orowan hardening mechanism. Similar behavior was
observed in a high strength maraging steel [7].
From the above discussion, it can be summarized that the multi-
step reversion transformation is an effective route to obtain stable
retained austenite. The copper precipitation in retained austenite
increases the stability of austenite, resulting in significant increase
in work hardening rate, such that the steel experiences significant
increase in yield strength without loss in elongation after the
third-step of tempering. The data presented here provides an insight
that copper precipitation in retained austenite is a viable approach
to obtain good mechanical properties by enhancing strength with-
out loss in elongation. However, in the investigated steel, the quan-
tification of precipitation in each step and theory concerning
precipitation of copper in retained austenite is unclear and requires
further investigation. Our ongoing work is focused on the quantita-
tive analysis of copper in retained austenite in each step and in
developing the associated theory behind such a behavior.
48 W.H. Zhou et al. / Materials and Design 63 (2014) 42–49
Fig. 7. (a) Work hardening behaviors and (b) Kocks–Mecking analysis (working
hardening-true stress plot) of samples A, B and C.
4. Conclusions
The mechanical properties and the microstructural evolution in
a low carbon Cu-bearing alloyed steel was studied in a three-step
heat treatment process. The effect of the third-step tempering pro-
cess on the structure–mechanical properties relationship was
emphasized. The conclusions are as follows:
(1) The experimental steel exhibited outstanding mechanical
properties after three-step heat treatment: yield strength
of 724 MPa, tensile strength of 923 MPa, yield ratio of 0.78,
uniform elongation of 21%, and total elongation of 31%.
(2) The microstructure primarily comprised of ferrite, retained
austenite, and small amount of bainite/martensite in the
three-step heat treatment process. Ferrite was the dominant
microstructure and the volume fraction of retained austenite
was 29%. Two-step and three-step heat treatment yielded
approximately similar retained austenite content. This was
associated with the enrichment of Mn, Ni, and Cu in the
reversed austenite.
(3) The third-step tempering process resulted in significant
increase in yield and tensile strength and low yield ratio
without loss in high elongation. This is attributed to copper
precipitation in retained austenite and in some ferrite during
the tempering process. Copper precipitation increased the
stability of retained austenite and contributed to strength
and work hardening rate by Orowan hardening mechanism.
Acknowledgements
The authors wish to thank the support from National Basic
Research Program of China (973 Program) through contact number
2010CB630801, and the China Scholarship Council for the award of
a scholarship to W.H. Zhou to study at the University of Louisiana
at Lafayette, USA. R.D.K. Misra gratefully acknowledges support
from the Center for Structural and Functional Materials, University
of Louisiana at Lafayette, USA.
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