Journal of Alloys and Compounds 762 (2018) 340e346

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Microstructure characterization of nanocrystalline bainitic steel

during tempering
Chih-Yuan Chen
Graduate Institute of Intellectual Property, National Taipei University of Technology, Taipei, 10608, Taiwan

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

Article history: The microstructure characterization and mechanical properties of tempered nanocrystalline bainitic
Received 24 March 2018 steel are investigated in the present study. It is found that the plastic relaxation in the thin film retained
Received in revised form austenite usually relies on the dislocation debris. On the other hand, an accommodation nanotwin
13 May 2018
structure can be found in the blocky retained austenite. Furthermore, the different accommodation
Accepted 15 May 2018
mechanisms in the bainitic steel result from the non-uniform carbon distribution in the retained
Available online 16 May 2018
austenite.
Microhardness data mainly revealed that, in the specimens tempered at 425
C, the average Vickers
Keywords:
Accommodation structure
hardnesses were 600 HV 0.1 for tempering of 5 min, 601 HV 0.1 for 10 min, and 595 HV 0.1 for 60 min. For
Temper the specimens tempered at 475
C, the average Vickers hardnesses were 598 HV 0.1 for tempering of
TEM 5 min, 596 HV 0.1 for 10 min, and 593 HV 0.1 for 60 min. Moreover, due to measurement error, the
Nanotwin hardness of the specimens that underwent the tempering process could be regarded as having almost
Dislocation debris maintained the initial hardness because the carbide precipitates in the interface further prevented the
Bainitic steel coalescence of bainitic ferrite plates during tempering treatment.
High resolution transmission electron microscopy provided new experimental evidence on the carbide
precipitation sequence, a subject critical to the understanding of the phase transformation mechanism
during the tempering process in bainitic steel. The presence of high carbon transition carbides (h-car-
bides) is the result of the low amount of dislocation debris, which acts as effective carbon traps, near the
blocky retained austenite.
© 2018 Elsevier B.V. All rights reserved.

1. Introduction solubility of silicon in cementite [7]. Without the cementite phase

Recently, nanocrystalline bainitic steel has attracted a great deal
of attention due to its high ultimate tensile strength of about
2.3 GPa and very high toughness (30 MPa m1/2), and it can be
produced in a very simple and cheap manufacturing process [1,2].
Therefore, the state-of-the-art nanocrystalline bainitic steel has
great potential for application in the automobile industry [3,4] and
as armor [5]. The excellent mechanical properties are mainly
attributed to the unusually high dislocation density (2  1015 to
6  1015/m2) within bainitic plates and the extremely thin bainitic
plates (20e40 nm thickness) with carbon-enriched thin film
retained austenite (10e20 nm) dispersed between them [6,7]. The
composition design strategy of this new generation of bainitic steel
is based on the addition of about 2 wt% of silicon to the high carbon
steel to prevent the precipitation of cementite, due to the poor
E-mail address: chen6563@gmail.com.
within the bainite microstructure, high toughness can be achieved
because of the decrease in the void-initiating phase (cementite) in
the steel [8]. In addition, the presence of carbon enriched austenite
instead of high carbon martensite also prevents decreases in
toughness [9e12]. On the other hand, molybdenum is added to
prevent temper embrittlement caused by scavenging of P in the
matrix, thereby decreasing P segregation to the grain boundaries
[13]. Besides the above alloy design concept, the bainite trans-
formation in this novel nanocrystalline bainitic steel can be
depressed to as low as 200
C or lower due to its high carbon
content (~1 wt%), which is beneficial for the formation of nanoscale
crystals of bainite ferrite plate. As pointed out by Chang and Bha-
deshia [14], the thickness of the bainite ferrite plates is influenced
heavily by the plastic accommodation ability of the bainite plate
and retained austenite in its proximity. Generally speaking, the
shape change accompanying bainitic transformation can usually be
accommodated by plastic relaxation and associated defects such as

https://doi.org/10.1016/j.jallcom.2018.05.174
0925-8388/© 2018 Elsevier B.V. All rights reserved.
 C.-Y. Chen / Journal of Alloys and Compounds 762 (2018) 340e346
dislocations [14e17].
For a bainitic steel to achieve better performance, it generally
needs to be treated with a further high temperature process, such
as a galvanizing treatment. The influence of a high temperature
process on the mechanical properties of the nanocrystalline bai-
nitic steel is still not very clear. It is well known that bainitic steel
has greater temper resistance than martensitic steel at the same
carbon content because of the completely different strengthening
mechanisms of these two kinds of steel [18,19]. For example, the
greatest contributor to the strength of martensitic steel is solid
solution hardening of interstitial carbon atoms, which can easily
precipitate as cementite in the tempered ferrite matrix through
moderate tempering due to the severe lattice distortion caused by
these carbon atoms [20]. On the other hand, the main strength-
ening mechanism in bainitic steel is the thickness of the bainitic
ferrite plates, especially in nanostructured bainitic steel, rather
than the solid solution strengthening caused by carbon atoms in
the lattice. Therefore, the bainitic ferrite plates must be kept small
during tempering to produce the temper resistance of bainitic steel.
According to other studies [18,19], carbides resulting from the
decomposition of thin film retained austenite pin the boundaries
and maintain the small size of the bainitic ferrite plates by pro-
hibiting further coalescence. However, few studies concerning the
thermal stability of retained austenite in nanocrystalline bainitic
steel and the carbide precipitation sequence have been conducted,
though it is an area worthy of further study [21e23].
In the present study, the tempered microstructure of nano-
crystalline bainitic steel and its plastic accommodation character-
ization were studied by traditional TEM and high resolution TEM
(HRTEM). The results provide new insight on the microstructure
evolution of novel bainitic steel during tempering treatment.
2. Experimental
The chemical composition of the alloy studied, measured after
homogenization at 1200
C for 2 days in a vacuum chamber, was Fe-
0.96C-1.41Si-1.93Mn-1.22Cr-0.26Mo-0.10 V (wt%). Cylindrical
samples of 3 mm in diameter and 4 cm in length were machined
from the homogenized material. Nanostructured bainite steel was
obtained by austenitization for 15 min at 1000
C, followed by
isothermal transformation at 200
C for 10 days before quenching
in water. The specimens were then tempered at 425
C and 475
C
for a variety of time periods (Fig. 1).
The samples were mainly characterized by optical microscopy
Fig. 1. Schematic diagram of the nanostructure bainitic steel heat treatment process: austenitizing at 1000
C for 15 min, isothermal transformation at 200
C for 10 days, and then
tempering at 425
C and 475
C for various times, respectively.
341
(OM), transmission electron microscopy (TEM, JEM-2000), and field
emission gun transmission electron microscopy (FEG-TEM Tecnai
F30) equipped with a nanometer probe energy dispersive spec-
trometer (EDS). Hardness measurements of the specimens to be
examined optically were taken using a Vickers hardness tester with
a load of 100 g. To realize the strengthening status in the bainitic
steel, for each processing condition, measurements from 50 indents
were used to estimate the final microhardness distribution. Thin
foil specimens were prepared for transmission electron microscopy
from 0.25 mm thick discs slit from the specimens used in the
dilatometric experiments. The discs were thinned to 0.5 mm by
abrasion on silicon carbide paper and then electropolished in a twin
jet electropolisher using a solution of 5 vol.% perchloric
acid þ25 vol.% glycerol þ70 vol.% ethanol at -2
C and 30 V
potential.
3. Results and discussion
3.1. Microstructure observation and mechanical property
measurement
The initial microstructure of the nanocrystalline bainitic steel
before tempering treatment was the outcome of the isothermal
decomposition of austenite at 200
C for 10 days. In Fig. 2 (a, b),
optical and transmission electron micrographs show slender and
tiny bainitic ferrite plates separated by thin film retained austenite
and a large area of blocky retained austenite. The bainite plates
have a very long shape with a tiny radius during solid state phase
transformation because the matrix material surrounding the iso-
lated bainitic plate needs to accommodate large strain. For bainite,
the strain energy amounts to about 400 J/mol, which is larger than
the chemical free energy change of reconstructive phase trans-
formation products such as allotriomorphic ferrite and pearlite
[24]. Christian, the famous physical metallurgist, pointed out that
the strain energy scales with the plate aspect ratio when the strain
is elastically accommodated [25]. Therefore, the morphology of
bainitic plates is usually a thin plate shape; i.e., the bainitic plate is
an isolated plate in the form of an oblate spheroid with its length
much greater than its thickness due to the minimization of strain
energy. The macroscopic characteristic of shape deformation con-
tains an invariant plane, i.e., an unrotated and undistorted plane
after phase transformation, and it is also associated with the plane
on which bainitic plates lengthen. Furthermore, the tiny thickness
of bainitic ferrite plates can be ascribed to the high carbon content
342 C.-Y. Chen / Journal of Alloys and Compounds 762 (2018) 340e346
Fig. 2. (a) Optical and (b) transmission electron microscopy images showing a nanocrystalline bainite microstructure after isothermal transformation at 200
C for 10 days.
and extremely low transformation temperature. Although no car-
bide precipitates can be observed within the bainitic ferrite in this
initial microstructure, other studies using advanced atom probe
facilities have found carbon enriched regions distributed inside the
bainitic ferrite plate, supporting the lower bainitic structure
[6,18,19].
For bainitic steel to be used as a structural material, its me-
chanical properties are critical. However, despite the above
microstructure observations, it is quite difficult to deduce the
plasticity, such as yielding and tensile stress, of individual, isolated
crystals in nanocrystalline bainitic steel because of their tiny size.
Therefore, the Vickers hardness test approach, which provides re-
searchers a handy and convenient way to evaluate the mechanical
properties of steel, was used. Table 1 shows the variation in the
average Vickers hardness of bainitic steel tempered at different
temperatures for various isothermal holding times. The extremely
high hardness (HV ~601) of bainitic steel before tempering mainly
results from the tiny size of the bainitic ferrite plates and numerous
defects [6e8]. However, in view of the measurement error of
Vickers hardness, namely the standard deviation, no matter what
tempering temperature was used, the average Vickers hardness can
be regarded as having maintained its initial Vickers hardness and
not changed with longer isothermal holding times. This result is
consistent with the tempering microstructure analysis, which
shows the transition carbides that precipitated in the interface
between bainitic ferrite plate and retained austenite. It is believed
that the carbides play an important role as obstacles that hinder the
bainitic ferrite plates from coalescence, resulting in gentle
tempering behavior [19].
3.2. Plastic relaxation structure in the nanocrystalline bainitic steel
Fig. 3(a) shows the dislocation debris distributed around the
austenite-bainitic ferrite interface. This dislocation debris
morphology is the result of displacive phase transformation, which
Table 1
The average microhardness of nanocrystalline bainitic steels after tempering
treatment. The initial microhardness of nanocrystalline bainitic steel after displacive
phase transformation was 601 ± 2.3 HV 0.1.
Tempering temperature Tempering time
5 min 25 min


425 C 600 ± 3.2 601 ± 6.1
475
C 598 ± 4.7 596 ± 5.9
causes shape deformation that must be accommodated in the
surrounding matrix by further plastic relaxation [20]. However, the
plastic deformation would not appear in the surrounding matrix if
the shape deformation were elastically accommodated. For
example, the thermoelasticity of shape memory alloys depends on
the elastic accommodation of shape deformation, and no move-
ment of the transformation interface would accompany any defects
[26]. The resulting dislocation debris impedes the advancement of
the austenite/bainite interface, thereby causing coherence losses.
Furthermore, as pointed out by Bhadeshia and Christian, the
amount of dislocations in the bainitic ferrite will increase due to
inheritance of the plastic relaxation dislocations due to the exten-
sion of the subsequently-formed bainitic ferrite plates [27]. For
instance, measured by TEM, the dislocation densities in the
austenite phase and bainitic ferrite in a similar steel transformed at
300
C for 3 days were found to be ð1:8±0:2Þ  1014 m2 and
ð5:1±2:7Þ  1014 m2 , respectively [28]. Fig. 3 (bed) reveals another
plastic accommodation morphology, a nanotwin structure in the
lenticular shape with thickness of about 20e30 nm, uniformly
dispersed within the retained austenite. This nanotwin structure,
called accommodation twinning to distinguish it from the trans-
formation twins that form in martensite because of invariant plane
strain, usually appears not in thin film austenite but in blocky
austenite, mainly due to the different dislocation activation modes
that occur in the retained austenite. The non-uniform distribution
characteristic of carbon atoms, i.e., more carbon atoms in the thin
film retained austenite and fewer carbon atoms in the blocky
retained austenite, has been reported in several studies to cause
different plastic accommodation mechanisms to dominate in the
proximity of austenite [6,29,30]. For example, measured by APT, the
average carbon content in the 80 nm thick austenite region and
3.5 nm thick austenite film were 6:4±1:8 at:% C and 9:8±0:4 at:% C,
respectively [6]. From TEM lattice fringe measurements, Shelf and
Bhadeshia noted the existence of non-uniform distributions of
carbon atoms in the retained austenite [29]. In the modern CMnSiAl
TRIP steel, Park et al. found that the average carbon content of film
type retained austenite (~5.9 at%) is much higher than that of
blocky type retained austenite (~4.9 at%) [30]. The reason why
twinning plastic relaxation induced by invariant plane strain usu-
ally occurs in blocky retained austenite and not thin film retained
austenite is mainly the different stacking fault energies, which both
types of retained austenite possess. The influence of the carbon
concentration on the stacking fault energy (SFE) in the austenite
60 min
phase has been investigated thoroughly in recent years [31e33].
595 ± 8.2 For example, Schramm and Reed found that SFE data strongly in-
593 ± 10.1
crease with carbon content [31], Petrov reported that SFE of fcc Fe-C
 C.-Y. Chen / Journal of Alloys and Compounds 762 (2018) 340e346 343

Fig. 3. (a) Bright field TEM image showing dislocation debris around the boundary of the austenite and bainitic ferrite plate. (b) Low- and (ced) High-magnification bright field TEM
images, (e) corresponding dark field TEM image revealing nanotwin structure within blocky retained austenite, (f) HRTEM image of twin structure, and (g) diffraction pattern.
344 C.-Y. Chen / Journal of Alloys and Compounds 762 (2018) 340e346
alloy decreases first and then increases with increasing carbon
content [32], and, as noted by Abbasi et al., SFE increases signifi-
cantly as a function of carbon concentration [33]. When the SFE of
the crystal is low, the dissociation of a full dislocation into two
partial dislocations is energetically favorable. This dissociation
impedes dislocation cross slip and climb, and it further induces the
activation of another deformation mechanism: twinning. There-
fore, accommodation twinning can usually be observed in most
blocky retained austenite crystals due to their low carbon
concentration.
The blocky retained austenite region with lower carbon content
is assumed to undergo twin deformation to accommodate plastic
relaxation for the subsequent bainitic transformation. In addition to
the nanotwin structure in the blocky austenite, other researchers
have discovered martensitic transformation occurring in this
blocky retained austenite region due to its relatively high Ms
temperature, which arises from the relatively low carbon content
[24]. On the other hand, the dislocation debris usually observed in
the vicinity of thin film retained austenite due to relatively high
carbon content in the austenite region leads to high yield strength
and a relatively low martensite start temperature.
3.3. Precipitation in the nanocrystalline bainitic steel during
tempering treatment
Fig. 4 (aec) reveals the fine carbides particles that precipitated
at the interface between bainitic ferrite and blocky retained
austenite after tempering treatment at 475
C for 10 min. Further-
more, after careful examination of three sets of electron diffraction
patterns, these precipitated particles were identified as h-carbides
Fig. 4. TEM micrographs showing h-carbides precipitated (see arrows) within a bainite plate near blocky retained austenite after tempering at 475
C for 10 min (a) Low- and (b)
high-magnification bright field images, (c) corresponding dark field image using (111) reflection of h-carbides, (def) three different sets of diffraction patterns confirming the
crystallography orientation of h-carbides with bainite plate.
(Fig. 4 (def)). The precipitation of carbides from supersaturated
lower bainite in a high temperature holding process is believed to
be identical to the tempering of martensite [34]. However, the
category of carbide, such as transition carbide or stable cementite,
that forms in the lower bainite after tempering treatment usually
depends on the tempering parameters. Austin and Schwartz were
the first to point out that the common transition carbide is ε-car-
bide [35]. Afterward, Matas and Hehemann proposed that the most
stable carbide in the hypoeutectoid bainitic steel after holding at
high isothermal temperature, cementite, resulted fromε-carbide
[36]. The transformation rate ofε-carbide to stable cementite relies
on both the treatment temperature and the steel composition. For
example, it is well known that silicon can retard the precipitation of
cementite because of the negligible solubility of silicon in
cementite. Therefore, the formation kinetics of cementite can be
accelerated if diffusion permits the silicon to partition into the
parent phase during cementite growth. Tempered martensitic steel
with high silicon content contains no cementite particles [34]. The
detection ofh-carbides instead of ε-carbides or cementite particles
in the present study implies the presence of a high proportion of
supersaturated carbon atoms near the blocky retained austenite
(i.e., 33 at.% for h-carbides versus 30 at.% for ε-carbides and 25% for
cementite). The absence of transition ε-carbides in the lower bai-
nitic ferrite plates during the tempering process can be also found
in other reports [6e8,37e39]. Bhadeshia and Edmonds detected
noε-carbides in a high silicon medium carbon steel even during the
early stages of lower bainite transformation [37]. Caballero et al.
found no carbide particles within bainitic ferrite plates despite
extensive TEM examination in the early stage of tempering. How-
ever, cementite was identified from a large and equivalent set of
 C.-Y. Chen / Journal of Alloys and Compounds 762 (2018) 340e346
accumulated atom probe results [6e8,38,39]. This phenomenon
was further explained by the carbon trapped mechanism proposed
by Kalish and Cohen [40]. Based on energetically theory, Kalish and
Cohen demonstrated that carbon atoms prefer to segregate at
dislocations rather than inε-carbides or cementite particles.
Moreover, Cochardt et al. showed that carbon atoms are more
stable in a dislocation atmosphere than in cementite because the
maximum interaction energy at a distance of one Burgers vector
from edge or screw dislocations is 0.75 eV, whereas the binding
energy of carbon in cementite is only 0.5 eV [41,42]. As a result,
more carbon atoms can be captured by dislocations, so transition
carbides disappear in the tempering process. Furthermore, Cabal-
lero also found that cementite precipitation occurs directly in such
a situation [6e8,38,39]. In short, the precipitation of h-carbides in
the lower bainitic ferrite near blocky retained austenite could occur
for the following two main reasons. First, different plastic accom-
modation mechanisms prevail in the different morphologies of
retained austenite. As mentioned above, the plastic relaxation
mechanism occurring in the blocky retained austenite can be
achieved primarily by nanotwin formation, which implies that less
dislocation debris forms. Second, it is found that a lower carbon
concentration can exist within blocky retained austenite. For
instance, fewer carbon atoms might exist in blocky retained
austenite than in thin film austenite [29,43,44]. Furthermore, the
segregation of solute atoms on defects associated with plastic ac-
commodation in blocky retained austenite is believed to play a
critical role in the carbide precipitation sequence during the
tempering treatment of bainitic steel. Hence, carbides with a su-
persaturated carbon concentration (i.e., h-carbide) have a high
potential to form initially during the tempering process, since fewer
dislocations are available to act as carbon sinks due to the twin
structures, which in turn are due to the plastic relaxation mecha-
nism instead of dislocation within blocky retained austenite.
4. Conclusion
Different plastic relaxation phenomena and the corresponding
tempered microstructure evolutions were analyzed by OM, TEM,
and microhardness tester in nanocrystalline bainitic steel after
various tempering treatments. The outcomes were mainly used to
elucidate the characterization of shape accommodation in a dis-
placive phase transformation as well as the influence of the
tempering processing parameters on the precipitation behavior in a
bainitic steel. Notable points are summarized as follows.
1. An ultra-fine bainitic microstructure, a mixture of retained
austenite and bainitic ferrite, with better mechanical properties
can be achieved by transformation of austenite at 200
C.
Furthermore, two types of retained austenite, namely, thin film
and blocky, can be found in nanocrystalline bainitic steel.
2. The lack of significant change in microhardness during
tempering treatment implies the resistance of this microstruc-
ture to tempering. This tempering behavior is probably due to
the difficulty of coalescence of bainitic ferrite plates, possibly
due to the formation of tiny carbides in the interface.
3. A dual plastic relaxation mechanism can be observed in a
nanocrystalline bainitic steel. The plastic relaxation associated
with dislocation debris usually occurs near thin film retained
austenite. In addition, in blocky retained austenite, the nano-
twin structure is the dominant accommodation mechanism.
This phenomenon can be explained by the intrinsic inhomoge-
neous distribution of carbon atoms within the retained
austenite.
4. The presence of h-carbides near blocky retained austenite re-
gions during the tempering process implies the high carbon
345
content within the carbide particles (33 at.% for h-carbide). This
finding can be ascribed to the lack of accommodation disloca-
tions, which can serve as carbon sinks, near the blocky retained
austenite; as a result, more carbon atoms can be incorporated in
the transition carbide. Therefore, carbon-rich carbides can be
formed initially during the tempering process.
Acknowledgements
This work was performed with financial support from the
Ministry of Science and Technology of the Republic of China,
Taiwan, under Contract MOST 106-2218-E-027-011-MY3.
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