Materials and Design 181 (2019) 107921

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Materials and Design

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

Interaction of martensite and bainite transformations and its dependence

on quenching temperature in intercritical quenching and
partitioning steels
Fei Peng, Yunbo Xu ⁎, Jiayu Li, Xingli Gu, Xu Wang
State Key Laboratory of Rolling and Automation, Northeastern University, Shenyang 110819, China

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

• All of the constituent phase fractions

showed multiple-stage variations by
controlling quenching temperature.
• The attributions of martensite and bai-
nite to austenite retention were
significantly related to quenching tem-
perature.
• An identical partitioning end between
T0 line and paraequilibrium condition
was achieved in all heat treatments.
• The carbon gradient in parent austenite
influenced subsequent martensite
transformation and corresponding
structure.

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

Article history: A series of quenching temperatures (QT) were applied to investigate the interaction of bainite and martensite
Received 3 April 2019 transformations in intercritical quenching and partitioning steels with multiple-stage martensite transformation.
Received in revised form 25 May 2019 It reveals that the fractions of initial martensite, bainite, whole retained austenite and austenite respectively
Accepted 6 June 2019
retained by bainite or martensite showed obvious three-stage variations, coincided with first stage, stagnant
Available online 7 June 2019
stage and second stage of martensite transformation. In the case of high QT that near Ms., the retained austenite
Keywords:
was mainly ascribed to bainite carbon enrichment. As quenched to relatively low QT in stage-1 region or lower,
Quenching and partitioning steel the austenite retained by martensite carbon partitioning occupied the majority and the decrease of RA was
Multiple-stage martensite transformation mainly ascribed to inter-lath austenite and packet boundary austenite. In addition, an identical partitioning
Quenching temperature end was achieved with mean austenite carbon contents between T0 line and paraequilibrium condition, irrespec-
Austenite retention tive of initial martensite and bainite fractions. The heterogeneous carbon distribution in parent austenite deriving
from ferrite formation significantly influenced the subsequent martensite transformation and corresponding
martensite structure. The martensite block in high carbon region possessed much smaller size, while the corre-
sponding packet size was still larger. Moreover, the significant martensite variant absence and variant combina-
tion were also observed.
© 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).

⁎ Corresponding author.
E-mail address: Yunbo_xu@126.com (Y. Xu).

https://doi.org/10.1016/j.matdes.2019.107921
0264-1275/© 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
2 F. Peng et al. / Materials and Design 181 (2019) 107921
1. Introduction
As representative automobile steel with high performance,
quenching and partitioning (Q&P) steel can obtain excellent mechanical
properties with high strength and fine ductility [1–3]. This heat treat-
ment is fully or partially austenitized followed by quenching to a tem-
perature (indicated as QT) between martensite start (Ms) and finish
(Mf) temperatures to form a precisely controlled fraction of initial mar-
tensite (M1). Subsequently, as the core of Q&P process, carbon atoms in
M1 partition to neighbored austenite during partitioning process at a
temperature the same as or higher than QT (indicated as PT) [1,2]. Fi-
nally, a considerable amount of austenite is retained at ambient temper-
ature, which can give rise to transformation induced plasticity (TRIP)
effect during deformation process to improve the final strength and
ductility [4,5].
As Q&P heat treatment initially proposed, all of reactions that det-
rimental to austenite retention, like pearlite formation, bainite for-
mation and carbide precipitation, are inhibited completely [1].
However, as for Q&P steel with low alloy addition, the entire Q&P
process, especially partitioning process, is actually a synergistic pro-
cess of carbon partitioning from M1 to austenite, initial martensite
temper and bainite formation [6]. Although Si and/or Al elements
are usually added to avoid cementite formation, it has been found
that the transition carbide was stabilized by Si and Al addition [7]
and hence the existence of transition carbide was always observed
in Q&P steel with Si/Al addition [6,8,9]. Moreover, as the bainite
formation, especially carbide free bainite (CFB) formation, is accom-
panied by carbon enrichment from bainitic ferrite (BF) into neigh-
bored austenite [10], both of the martensite carbon partitioning
and bainite formation are favorable to final austenite retention [6].
Up to now, although some authors have deduced the dominant
role of martensite carbon partitioning on final austenite retention
[11], a more reliable evaluation of the contribution of bainite forma-
tion on austenite retention should be obtained based on the results
of a relatively wider range of heat treatment. In this paper, various
QTs were applied to control the proportions of M1 and bainite
fractions.
Moreover, it is well known that heterogeneous carbon distribution
in austenite is usually obtained after partial austenitization [12], which
significantly influences subsequent transformation sequences, transfor-
mation locations, morphologies of products and corresponding crystal-
lographic characteristics [13,14]. In particular, controlling the carbon
gradient in austenite to appropriate extent, the nonisothermal martens-
ite transformation would occur discontinuously or called as multiple-
stage martensite transformation, which means that austenite with low
carbon content transformed into martensite at high temperature re-
gime, while the high carbon austenite transformed at low temperature
regime [13]. Actually, some authors have reported this multiple-stage
martensite transformation in Q&P steels, in which the gradient of
carbon content was introduced by martensite carbon partitioning dur-
ing continuous cooling process [15]. As the core of Q&P process, mar-
tensite carbon partitioning is considerably dependent on the
characteristics of initial martensite. Hence, it can be deduced that the in-
troduction of multiple-stage martensite transformation in Q&P steels
would significantly influence the microstructure evolution and charac-
teristics of constituent phases, as well as final austenite retention. How-
ever, few articles were reported on this view and the role of multiple-
stage martensite transformation in Q&P steels was still lack of knowl-
edge [13,15].
Hence, this paper provides an insight into the interaction of mar-
tensite and bainite transformations in partially austenitized quenching
and partitioning steels with multiple-stage martensite transformation,
especially focused on respective characteristics of austenite retained
by initial martensite and bainite. Meanwhile, the crystallographic char-
acteristics of retained austenite and martensite variant were obtained
and analyzed by EBSD technique.
2. Experimental procedures
A low carbon steel with composition of 0.225C-1.97Mn-1.43Si
(wt%) was investigated here. The microstructure of as-received
hot-rolled sheet was composed of ferrite and pearlite. Then the
sheet was cold rolled to 1.2 mm thickness. The specimens with di-
mensions of 4 mm × 10 mm were machined with length parallel to
the rolling direction. All of the heat treatments were conducted by
DIL 805 A/D dilatometry and the corresponding schematic diagram
is presented in Fig. 1. The samples were partially austenitized at
800 °C for 180 s followed by fast cooling at 50 °C/s to different QTs
(65/100/120/180/220/250/320 °C) for 10s, and then an isothermal
holding at 400 °C for 180 s was applied. Finally, all of the
samples were quenched to ambient temperature with a cooling
rate of 50 °C/s. Hereafter, the Q&P samples were referred to as
Q&P-65/100/120/180/220/250/320, respectively. Meanwhile, the
as-quenched sample that directly quenched to room temperature
after annealing was also prepared.
The microstructure and element distribution were characterized by
JEOL JXA-8530F electron probe microanalyzer (EPMA) equipped with
wavelength dispersive spectrometer (WDS). The volume fraction of
retained austenite and corresponding austenite carbon content were
calculated based on the integrated intensities of (200)α, (211)α,
(200)γ, (220)γ and (311)γ peaks using D/max 2400 X-ray diffractome-
ter (XRD) (step size: 4°/min, 2θ:40–100°).
The electron backscatter diffraction (EBSD) measurement were per-
formed using a Zeiss Ultra-55 field emission scanning electron micro-
scope (FE-SEM) with step size of 50 nm and tilt angle of 70°. The
corresponding samples were electropolished at 25 V for 20s using a
electrolyte of 12.5 vol% perchloric acid and 87.5 vol% alcohol. The ac-
quired data was post-processed by Channel 5 software.
A Φ3 mm foil with thickness of 45 μm was prepared and twin-jet
polished by 12.5 vol% perchloric acid alcohol at −23 °C and 32 V. Then
the specimens were applied for microstructure observation using a FEI
G2 F20 transmission electron microscope (TEM) with operation voltage
of 200 KV.
3. Results and discussion
3.1. Dilatation analysis of phase transformation
3.1.1. Partial austenitization and epitaxial ferrite formation
The dilation curves for specimens with different QTs are shown in
Fig. 2. It is clear that the partial austenitization accompanied by signifi-
cant volume contraction was proceeded during reheating and isother-
mal annealing process. Subsequently, a phase transformation with
Fig. 1. The schematic diagram of heat treatments.
 F. Peng et al. / Materials and Design 181 (2019) 107921 3

Here, it is assumed that the martensite expansion of different stages

is only related to the transformed fraction, irrespective of the discrep-
ancy in austenite carbon content. Then the transformed martensite frac-
tion (i.e. M1) of different QTs can be calculated using lever rule method,
as shown in Table 1. It is clearly that the maximum fraction of martens-
ite formed in the stage-1 was ~87% of the entire martensite, while the
stage-2 martensite was ~13%. Moreover, although the martensite trans-
formation was finished at 72 °C, there was still some austenite retained
at ambient temperature and the corresponding volume fraction can be
measured by XRD as 4.5 vol%.

3.1.3. Phase transformations synergistically occurred during partitioning

Fig. 2. Dilatometric results of different Q&P samples.
distinct expansion is observed during the cooling procedure, with tem-
perature range of 600–700 °C (Fig. 2). This phase transformation is well
known as epitaxial ferrite (EF) transformation, which is formed on basis
of intercritical ferrite (IF) without nucleation and grows by epitaxial
type [12,16]. Actually, the formation of EF was confirmed to consider-
ably promote the heterogeneity of carbon content in remaining austen-
ite [12]. Moreover, due to the identical annealing process before Q&P
process, the total volume fraction of ferrite (fF), including IF and EF,
was considered as a constant value and determined by metallographic
method to be 15 ± 3 vol%.
3.1.2. Multiple-stage martensite transformation during quenching process
The martensite transformation behavior of as-quenched specimen is
shown in Fig. 3. As the slopes of straight lines respectively indicated as
L1, L2 and L3 decreased successively, it can be concluded that the
nonisothermal martensite transformation process can be divided into
three stages, i.e. two-stage martensite transformation that separated
by a martensite stagnant stage. As quenching process proceeded, it re-
veals that partial austenite with low carbon content transformed into
martensite at relatively high temperature range (stage-1), followed by
a martensite stagnant stage (i.e. austenite stable stage) until quenched
to a critical temperature that satisfied the necessary driving force to
occur second-stage martensite transformation with high carbon con-
tent (stage-2). The corresponding martensite transformation tempera-
ture ranges are measured as 338–235 °C and 163–72 °C, respectively.
process
The relative length changes during partitioning process are pre-
sented in Fig. 4. It is obvious that all of the samples possess significant
expansions, and continuous expansion is observed at high QTs (larger
than 180 °C), while expansion followed by constant or contraction
was observed at relatively low QTs (smaller than 120 °C). Meanwhile,
it is clear that the values of entire expansion increase with decreasing
QT.
Actually, three different processes were synergistically occurred
during partitioning process: carbon partitioning from martensite into
austenite, tempered process of initial martensite and bainite formation
of unstable austenite. As is well known that, carbon partitioning process
hardly influences the dilatation [17]. Hence, the significant expansion is
ascribed to bainite formation, while contraction is attributed to mar-
tensite tempered process, which is proportional to the fraction of tem-
pered martensite. Moreover, the martensite tempering process takes
place with a relatively sluggish rate and then accelerates gradually
[18], while the bainite formation occurred and proceeded with a rapid
transformation rate during the whole partitioning process. When
quenching to a higher temperature (180 °C or above), the expansion in-
troduced by bainite formation plays a major role, while the contraction
of martensite tempered process was negligible. With decreasing QT to
100 °C and 120 °C, the expansion of bainite formation was dominant
at the early stage, while gradually counteracted by the contraction of
martensite tempering at the subsequent stage. As a result, the relative
length changes increase firstly followed by keeping stable or showing
a slight contraction in the latter part of partitioning process. As to the
specimen quenched to 65 °C, few bainite was formed during
partitioning and significant contraction deriving from the tempered be-
havior of abundant M1 was observed.
3.2. Observation of constituent phases and corresponding carbon
distribution

Fig. 5 shows the secondary electron (SE) micrographs of typical heat

treatments. All of the microstructures comprise ferrite, bainite, initial
martensite (M1) and retained austenite (RA)/secondary martensite

Table 1
The measured or calculated phase fractions of Q&P samples with different quenching tem-
peratures. fRA, fF, fB, fBγ and fM1 indicate the volume fraction of retained austenite, ferrite,
bainite, retained austenite in bainite and initial martensite, respectively. Cγ represents
the average carbon content in retained austenite. Here, fRA and Cγ were calculated based
on XRD results, fF, and fB were obtained by metallographic method, fγB was calculated by
lever rule method on basis of fRA and fB (detailed explained in Section 3.3.2), fM1 was ob-
tained by lever rule method based on dilatometric result of as-quenched sample.

QT/°C Cγ/% fRA/% fF/% fB/% fBγ/% fM1 /%

65 1.369 5.4 15 ± 3 1.91 0.913 78.5

100 1.368 7.0 15 ± 3 3.02 1.23 76.38
120 1.362 8.96 15 ± 3 4.03 1.58 73.08
Fig. 3. The length change of low temperature region in as-quenched specimen. The dash
180 1.320 10.06 15 ± 3 9.55 2.74 68.01
lines indicated as L1, L2 and L3 correspond to the straight parts of dilatation before,
220 1.317 10.57 15 ± 3 10.39 2.98 68.01
between and after martensite transformation, respectively. Stage-1, stagnant and stage-
250 1.318 11.41 15 ± 3 11.51 3.15 66.54
2 indicates the first-stage, stagnant-stage and second-stage martensite transformation,
320 1.315 12.98 15 ± 3 14.76 11.56 9.27
respectively.
4 F. Peng et al. / Materials and Design 181 (2019) 107921

(M2). The characteristics of ferrite in different heat treatments are anal-

Fig. 4. The relative length changes of Q&P specimens during partitioning process.
ogous, which show polygonal morphology with location mainly along
the parent austenite grain boundary (PAGB).
In the case of Q&P-65, which exceeds the martensite transformation
regime, most of the austenite has transformed into M1 and then tem-
pered during the following partitioning process. Meanwhile, a small
fraction of CFB, which consists of bainitic ferrite and retained austenite,
is also observed (Fig. 5a), consistent with the dilatation result in Fig. 4.
Some lath-like RA is also found to be located inside M1 due to the car-
bon partitioning effect from martensite lath into neighbored austenite
[1]. Moreover, some blocky RA is observed to be inside ferrite matrix
or located in the outside of M1 neighbored to ferrite, mainly attributing
to the carbon enrichment from ferrite into austenite [12]. It should be
note that the existence of M2 was hardly observed and hence can be ig-
nored in Q&P-65. Furthermore, it is noteworthy that considerable
amount of plate-like carbide is observed inside M1, which is easily
etched to obtain interior tempered structure (Fig. 5b). With quenching
temperature increased to 120 °C, the microstructure is nearly the
same as that of Q&P-65. However, some blocky RA/M2 with relatively

(a) (b)
RA
B

M1
F Carbide

F RA

5μm 2μm

(c) (d)
RA

B
Carbide
RA/M2. RA

5μm 2μm

(e) (f)
RA/M2

RA RA

M2

M1
B
M1

5μm 2μm

Fig. 5. The SE micrographs of typical heat treatments. (a) (b) Q&P-65; (c) (d) Q&P-120; (e) (f) Q&P-320.
 F. Peng et al. / Materials and Design 181 (2019) 107921
large size is observed, which means that some austenite carbon-
enriched during partitioning is still insufficient stable and transformed
into M2 during the final quenching process (Fig. 5c).
Furthermore, when the quenching temperature increased to a rela-
tively higher temperature, such as 320 °C, the M1 fraction decreased sig-
nificantly (Fig. 5e), while the microstructure is mainly composed of RA/
M2 and CFB. It can be revealed that the abundant austenite after
quenching could not be retained completely via martensite carbon
partitioning. As a consequence, some carbon-enriched austenite with
insufficient stability will transform into bainite during isothermal
partitioning process or M2 during the final quenching. Actually, the for-
mation of CFB is favorable to austenite retention by carbon-enrichment
from BF into austenite and the enhancement of hydrostatic stresses in
austenite [10]. Notably, the parent austenite with size of larger than
10 μm after partial austenitization was refined into small regions
with size of 1–2 μm due to the refinement effect of martensite and bai-
nite transformations [19]. Moreover, due to the slight fraction of M1 at
320 °C (~9.27 vol%), the existence of carbide inside M1 was not ob-
served in SE images, while it can be found by TEM as mentioned in fol-
lowing section. The volume fraction of bainite can be measured by
metallurgical method and the result shows that the bainite fraction in-
creased with increasing QT (Table 1), which is coincident with the dila-
tation result (Fig. 4).
In order to analyze the characteristics of carbon partitioning in
different heat treatments, the carbon distributions of typical speci-
mens were depicted by WDS technique, as shown in Fig. 6. It is
clearly that both of ferrite and M1 are significantly carbon-
depleted, while the carbon-enriched region was mainly determiend
to be RA on basis of corresponding morphology features. As to Q&P-
65, the carbon-enriched region is mainly located in the exterior of
parent austenite that adjacent to ferrite, whilst some lath-like re-
gions in the interior of M1 and some blocky regions in the packet
boundary of M1 or inside ferrite are also found to be carbon-
enriched, as indicated by triangle in Fig. 6. With increasing QT to
120 °C and 320 °C, the locations of carbon-enriched region are
identical to those of Q&P-65, while the carbon-enriched regions
expand to the interior of parent austenite and corresponding sizes
increase significantly. Hence, it can be concluded that more austen-
ite was retained at a relatively higher QT. Moreover, as abundant
bainite was formed at high QT, the carbon-enriched RA in bainite
Q&P-65 Q&P-120
F
M1
M1
B
5µm
Fig. 6. Microstructures and carbon distributions of Q&P-65, Q&P-120 and Q&P-320. Carbon-enriched RA was indicated by triangles.
5
with lath-like morphology was also observed in Q&P-120 and
Q&P-320.
3.3. Characterization and analysis of retained austenite characteristics
3.3.1. Microstructure observation by TEM and EBSD
As a representative sample, the typical TEM micrographs of Q&P-150
are shown in Fig. 7. It is clearly that both of lath martensite and twin
martensite are observed in all specimens. Meanwhile, due to the mar-
tensite tempering during partitioning process, some dislocation cells
are found inside M1 laths (Fig. 7a), while some dislocations are ob-
served in the exterior of twin martensite (Fig. 7b). Moreover, abundant
carbides with rod-like morphology were both observed inside lath mar-
tensite and twin martensite, which can be determined as ε carbide by
SAED (Fig. 7f). Actually, the precipitation of ε carbide was usually con-
sidered to be nucleated during quenching process and growed during
subsequent Q&P process [6]. As the high carbon M2 formed during
final quenching shows much lower Ms. temperature, it can be deduced
that the ε carbide has not enough time to precipitate inside M2 [8].
Hence, some twin martensite was considered to be formed during initial
quenching process due to the carbon enrichement of ferrite formation,
and then tempered during partitioning process to obtain ε carbide pre-
cipitation and partial decompsition of twin structure.
Furthermore, the EBSD technique was applied to distinguish ferrite,
austenite, M1 and M2. Due to the specific crystal structure, austenite
with FCC structure can be recognized readily. As for ferrite, M1 and
M2, which are all BCC structure, they can be distinguished effectively
via the difference of band slope (BS) and internal substructure. It
means that ferrite possesses the highest BS value, while M1 shows a rel-
atively lower BS value with abundant low angle boundaries and M2 pre-
sents the lowest BS value. Furthermore, the typical bainite can be
recognized on basis of its complex components, i.e. bainitic ferrite
with similar BS value as M1 but slight substructure, retained austenite
and/or M2. All of the typical constituent phases are indicated in Fig. 8.
As Fig. 8 shows, the RA in Q&P-320 is mainly located in bainite ma-
trix with blocky morphology, whilst some blocky RA with relatively
smaller size was found in the packet boundary of M1 or inside the ferrite
matrix. In reality, most of the retained austenite is adjacent to ferrite,
due to the inheritance of carbon-enrichment effect from ferrite. As to
Q&P-120, the size of RA decreased significantly, while the location of
Q&P-320
F
F
M2
B
5µm 5µm
6 F. Peng et al. / Materials and Design 181 (2019) 107921

(a) (b) (c)

RA
Packet
Dislocation cell Twin M

Lath M
Dislocation
Packet boundary

(d) (e) (f)

carbide

Twin M
carbide

Fig. 7. Typical TEM micrographs of Q&P-150. (a) Lath martnsite and retianed austenite between laths; (b) twin martensite and (c) corresponding selected area electron diffraction (SAED)
image; (d) ε carbide precipitated inside twin martensite; (e) ε carbide precipitated inside lath martensite and (f) corresponding SAED image.

RA is still adjacent to ferrite. Hence, it can be concluded that the austen-
ite that closer to the austenite/ferrite interface was only transformed
into M1 at a lower QT. It can also deduce that the austenite carbon het-
erogeneity deriving from ferrite formation significantly influences the
distribution, size and morphology of RA. In particular, some blocky RA
with much larger size was observed in Q&P-120, which can be deter-
mined to be twin austenite by further analysis. Actually, the austenite
twin boundary in Q&P-120 occupied 35% of the entire austenite bound-
aries, while that in Q&P-320 was about 40.4%. It reveals that a significant
volume fraction of twin austenite retained after Q&P process.
Furthermore, due to the detect limit of EBSD technique, the nano-
scale retained austenite between martensite laths should be character-
ized by TEM and the results are shown in Fig. 9. Here, the dark field
images are used to depict the actual width of retained austenite. As to
Q&P-65, the retained austenite presents discrete film-like morphology
and approximately straight interface with thickness of 20–50 nm.
With QT increases to 120 °C, the austenite expands to a thickness of
60–70 nm with continuous and straight interface (Fig. 9d). In the case
of Q&P-320, the further coarsened lath-like retained austenite impinged
and connected together with curved interface (Fig. 9f). Actually, the
curved interface of austenite/martensite was usually related to interface
migration during partitioning process [20]. When QT is relatively high,
i.e. limited M1 formed during quenching process, the interface of mar-
tensite/austenite would move to austenite or move to martensite firstly
followed by an inverse moving to austenite, depending on the interface
condition [21]. Hence, it can be deduced that the effect of interface mi-
gration was more significant in samples with relatively high QT.
3.3.2. Estimation of the respective contributions of bainite and martensite
on austenite retention
In order to estimate the respective contributions of bainite formation
and martensite carbon partitioning on austenite retention, the volume
fraction of austenite in bainite can be calculated by an analytical method
as follows:
!
B CIC
γ −Cα QT
fγ ¼  fγ ð1Þ
Cγ −Cα

(a) (b)
Twin RA
M1

M1 F
F
B B
B
M2
M2

5µm 5µm

Fig. 8. Comined EBSD maps of BS + FCC (blue) + high angle boundary (N10°, black line) + low angle boundary (2–10°, green line) for (a) Q&P-120 and (b) Q&P-320.
 F. Peng et al. / Materials and Design 181 (2019) 107921 7

(a) (b) (c)

(d) (e) (f)

Lath
Lath
Lath
64nm Curved interface
43nm 20nm 20nm
101nm

Lath
Lath
60nm 68nm

Fig. 9. TEM observation of retained austenite located between martensite laths. Q&P-65: (a) bright field image, (d) dark field image; Q&P-120: (b) bright field image, (e) dark field image;
Q&P-320: (c) bright field image and (f) dark field image.

where fBγ is the volume fraction of austenite in bainite, CIC QT

γ , Cα, Cγ and fγ
are the carbon content in initial austenite (~0.264 wt% with 15 vol% F)
before martensite transformation, bainitic ferrite carbon content
(~0.10 wt% reported by ref. [11]), retained austenite carbon content (de-
termined by XRD) and austenite fraction at QT, respectively.
The value of fQTγ can be calculated by the following equation:
QT
f γ ¼ 1−f F −f M1
where fF and fM1 indicate the volume fractions of ferrite and M1, respec-
tively (see Table 1).
Based on the Eqs. (1)–(2), fbγ can be calculated and the results are
shown in Table 1 and Fig. 10b.
As the summarized results shown in Fig. 10, with decreasing QT, the
volume fraction of M1 increases dramatically in stage-1, followed by
keeping stable in stagnant stage and then shows a sluggish increase in
stage-2. Meanwhile, both of the fractions of RA and bainite decrease
with three stages, which coincide with the stage-1, stagnant and
stage-2 of martensite transformation. Actually, the two-stage martens-
ite transformation separated by stagnant stage significantly influenced
the microstructure evolution during Q&P process by controlling M1
fraction and austenite characteristics before partitioning process, and
further influenced the subsequent bainite formation and martensite
ð2Þ carbon partitioning behavior.
Furthermore, it is recognized that the whole austenite retention is
mainly attributed to bainite carbon enrichment and martensite carbon
partitioning, after which the influence of carbon enrichment from fer-
rite into austenite is overlapped. Then the corresponding attributions
of M1 and bainite to the final retained austenite can be obtained, as
shown in Fig. 10b. It is noteworthy that the fractions of RA respectively
retained by martensite and bainite show three-stage variations with in-
creasing QT, consistent with the multiple martensite transformation.

Fig. 10. (a) Volume fractions of bainite and initial martensite (metallographic method); (b) volume fractions of whole retained austenite (XRD) and the portions corresponding to bainite
and martensite transformation, respectively (calculated method). XC: carbon content (wt%); Stage-1: first-stage martensite transformation; Stage-2: second-stage martensite
transformation; Stagnant: martensite transformation stagnant stage.
8 F. Peng et al. / Materials and Design 181 (2019) 107921
Due to the austenite carbon heterogeneity deriving from ferrite for-
mation, the austenite in the center with low carbon content has trans-
formed into M1 during stage-1 martensite transformation. Actually, as
the low carbon region occupied the majority of parent austenite, the
volume fraction of M1 significantly increased with decreasing QT in
stage-1. Meanwhile, the bainite fraction decreased due to the decrease
in austenite fraction and relatively high thermal stability of austenite
after quenching. Moreover, in stage-1, the RA fraction corresponding
to bainite decreased significantly with decreasing QT (Fig. 10b), while
the RA in M1 presents a distinct increase inversely. Hence, it can be con-
cluded that the decreased fraction of entire RA principally corresponds
to RA in bainite. It is necessary to note that the RA corresponding to bai-
nite plays a crucial role on the final austenite retention when quenching
to a high temperature, which means that the austenite retained by bai-
nite formation was dominant at a high QT close to Ms. temperature.
When decreasing QT into martensite stagnant stage, both of the bainite
fraction and RA fraction varied slightly due to the constant volume frac-
tion of M1. Simultaneously, the RA in bainite and martensite keeps con-
stant approximately.
Furthermore, as the QT decreased into stage-2 region, the high car-
bon austenite that close to the periphery of parent austenite has trans-
formed into M1. However, due to the size of austenite region with
high carbon is relatively narrow, the increase of M1 fraction with de-
creasing QT is sluggish in this stage. Meanwhile, the bainite fraction de-
creased slightly and corresponding RA in bainite shows a relatively
sluggish decrease as compared with that in stage-1 region. Actually,
due to the identical partitioning process, the bainite fraction is mainly
relevant to the number density of nucleation sites [22]. With decreasing
QT, the increasing number of austenite/M1 interface can effectively
counteracted the deteriorated effect of decreasing austenite fraction
and hence the bainite fraction decreased sluggishly in all stages. In par-
ticular, the sudden decrease of bainite fraction at the onset of stage-2 re-
gion was ascribed to the sudden decrease of remaining austenite after
quenching, which corresponds to the sudden increase in M1 fraction
in stage-2. Moreover, the RA in martensite occupied the majority of en-
tire RA in stage-2, while the values of RA in M and whole RA are both
rapidly decreased with decreasing QT. It can be deduced that the de-
crease of RA in stage-2 was mainly ascribed to the decrease of RA in
martensite, i.e. mainly the inter-lath austenite, which is consistent
with the result that observed in Fig. 9. It should be noted that some aus-
tenite was still retained after quenching to a temperature exceed the Mf
temperature, due to the carbon enrichment from ferrite into austenite.
Actually, this austenite was further carbon enriched via subsequent
martensite carbon partitioning and bainite carbon enrichment.
3.3.3. Thermodynamic analysis of carbon partitioning end
Although the fractions of constituent phases showed three-stage
variation (Fig. 11), the measured carbon contents of RA at different
QTs show approximate values (1.31–1.37 wt%), irrespective of the ini-
tial heterogeneous carbon distribution [13]. Hence, the initial austenite
carbon distribution hardly influences the final carbon content in
retained austenite, i.e. an identical partitioning end was achieved at dif-
ferent QTs.
Moreover, compared with the austenite carbon content after anneal-
ing (0.274 wt%), the retained austenite is significantly carbon-enriched
as a synergistic result of martensite carbon partitioning and bainite
carbon-enrichment. It should be noted that the final average carbon
content in RA has exceeded the T0 line (0.974 wt% at 400 °C), which cor-
responds to the end of bainite formation, while still far from the
paraequilibrium (PE) composition. Actually, the PE condition is a
constrained local equilibrium, under which Mn and Si elements are
hardly redistribution, while carbon can diffuse between ferrite and aus-
tenite. Hence, the PE composition represents the maximum austenite
carbon content possibility obtained by carbon diffusion process. As to
the sample with QT close to Ms., slight M1 was formed and majority
of the RA was attributed to bainite carbon enrichment. However, the
Fig. 11. (a) Comparison of average carbon content in retained austenite (XRD result) with
T0 and pare-Ae3 composition. (b) Enlarged image of XRD result. T0: the equivalent state of
Gibbs energy in both bainitic ferrite and austenite, PE: the calculated carbon content in
austenite under paraequilibrium condition. Note that, both of the T0 and PE values were
calculated based on the compositions of austenite after intercritical annealing, i.e.
0.274C-2.189Mn-1.375Si (wt%), which was calculated by Thermal-calc software based
on TCFE9 database. XγC : austenite carbon content after annealing; XRAC : average carbon
content in retained austenite.
final carbon content in RA still exceeded the T0 line, attributing to crucial
role of martensite carbon partitioning on final carbon-enrichment of RA.
With decreasing QT, the attribution of martensite carbon partitioning on
austenite retention increased significantly with M1 fraction increased
and bainite fraction decreased. Hence, it can be deduced that the carbon
partitioning from M1 was dominant on the final austenite carbon-
enrichment in all Q&P samples.
3.4. Crystallographic analysis of retained austenite and martensite variants
In order to obtain crystallographic characteristics of retained austen-
ite and neighbored martensite, a detained crystallographic analysis was
typically applied in Q&P-120. As shown in Fig. 14a, the parent austenite
has transformed into ferrite, bainite and martensite, whilst some aus-
tenite was still retained. As is well known that, the retained austenite
corresponding to identical parent austenite grain shows same orienta-
tion, while the products transformed by displacive mechanism, like bai-
nite and martensite, were confirmed to maintain Kurdjumov-Sachs
(K\\S) and/or Nishiyama-Wassermann (N\\W) orientation relation-
ships with neighbored retained austenite.
The dashed rectangle in Fig. 12a was selected to analyze in detail and
was enlarged as Fig. 12b. Two different misorientations between
retained austenite were measured, 10–15° (line 1 in Fig. 12b) or larger
than 40° (line 2 in Fig. 12b). As the PAGB is usually a high angle grain
boundary of 20–40° [23], then the measured misorientation of larger
than 40° in Fig. 12b can correspond to two neighbored parent austenite,
while different retained austenite regions with small misorientation of
10–15° belong to identical parent austenite. Actually, this small misori-
entation can be ascribed to austenite rotation, which is a result of aus-
tenite plastic accommodation during martensite transformation [24].
Hence, the region 1 and region 2 in Fig. 12b correspond to identical par-
ent austenite and were further analyzed.
Furthermore, as mentioned above, abundant amount of twin bound-
ary was found in retained austenite and some individual retained aus-
tenite can be also confirmed as twin austenite by orientation analysis.
As shown in Fig. 12b, the retained austenite grains in region1 have
two different orientations (indicated by triangles), which show twin re-
lationship. Assumed that the orientation corresponding to majority of
retained austenite is matrix, then the austenite with another orientation
 F. Peng et al. / Materials and Design 181 (2019) 107921 9

(a) (b) RD

F F
M
M
M

Region 2
F F
Region 1
5µm
M F 2µm

Fig. 12. Combined maps of Q&P-120 with BC + IPF of FCC + grain boundary (2–10°,r ed color, N10°: black color) + twin boundary (yellow color), in which (b) is the enlarged image of
dashed rectangle in (a). BC: band contrast, IPF: inverse pole figure. The misorientations of different retained austenite regions were measured along line 1 and line2 as 13.5°and 47.5°,
respectively.

can be confirmed as twin austenite. In particular, some blocky twin aus-
tenite grains with relatively large size were also observed (Fig. 12a).
Hence, it can be concluded that twin austenite was prevalently existed
during annealing process.
As mentioned above, the austenite in region 2 rotated slightly com-
pared with that in region 1. As a result, the transformed martensite of
region 2 also rotated slightly, as indicated by triangles in Fig. 13b. It is
well known that the K\\S relationship between martensite and parent
austenite has 24 variants, indicated as V1~V24 [24]. In order to analysis
the martensite variant, here the V1 was determined to be austenite of
(111)γ and [101]γ that transformed into martensite with (011)α and
[111]α. Then the other martensite variants can be calculated based on
the orientation transformation matrix and the calculated results are
the same as those listed in ref. [25]. Based on the calculated results,
the standard {100} pole figure of 24 K-S variants can be plotted and
then rotated to be coincided with the experimental results [24,25]. By
comparison with the ideal {100} pole figure, the analysis of martensite
variant was conducted in region 1 and 2. As a representative one, the
corresponding comparative result of region 1 was plotted as Fig. 13c,
in which only the existed variant was indicated. And the corresponding
analyzed result is combined with the location information, as shown in
Fig. 14.
It can be revealed that not all variant existed in this parent austenite,
in which the variants V3, V7, V13, V14, V16 and V18 were disappeared.
These variants were called as naturally absent variants and were as-
cribed to the lack of transformation space [26]. Actually, more variants
were absent in the region 2 with relatively smaller size. Meanwhile, a
significant variant combination phenomenon was observed, which
means that some specific martensite variants occurred as a group
[24,25], i.e. V1&V4, V2&V5, V9&V12, V19&V22, V20&V23 and
V21&V24. This particular variant combination, which is also called as
sub-blocks [24], possesses the minimum misorientation (10.53°) be-
tween different variants. This variant combination is usually recognized
to accommodate the transformation strain [27]. It is worthwhile to note
that the size of martensite block decreased from downside to the upside
in region 1. As the block size decreased with increasing carbon content
of parent austenite [24], it can be concluded that the parent austenite
possessed heterogeneous carbon distribution, i.e. carbon enriched in
upside region, while carbon-depleted in downside region. As higher car-
bon content corresponding to higher crystal defects with lower BS

(a) (b) (c)

Fig. 13. Orientation analysis of retained austenite and martensite in Q&P-120 (a) {111} pole figure corresponds to the retained austenite in region 1(circles and rectangles correspond to
austenite with different orientation), (b) {100} pole figure of martensite in region 1 and 2 (triangles indicate the typical orientations of martensite in region 2), (b) {100} pole figure of
martensite in region 1.
10 F. Peng et al. / Materials and Design 181 (2019) 107921

Fig. 14. Analyzed result of martensite variant in Q&P-120, in which the background image is the combined map of IPF+ block boundary (black line) + packet boundary (yellow line).

value, the lower BS values of martensite block located in the upside of
region 1 can also confirm the existence of high carbon content
(Fig. 8a). This heterogeneous carbon distribution in parent austenite
was mainly attributed to carbon enrichment from ferrite, which
shows much larger fraction in the upside of region 1. Actually, although
the variant distribution was much complex in the upside region with
higher carbon content, the corresponding packet size was still much
larger, which showed a different result from that in ref. [24]. In particu-
lar, some martensite blocks with particle morphology showed much
small size and were surrounded by neighbored blocks. These particle
blocks possessed much lower BS values (Fig. 8a), which can be
determined to be M2 that formed in the final quenching. Hence, it can
be concluded that the heterogeneous carbon distribution in parent aus-
tenite could influence the subsequent martensite transformation and
corresponding martensite structure, especially variant characteristics.
3.5. Comprehensive analysis of austenite decomposition and retention dur-
ing Q&P process
The Schematic diagrams of microstructure evolution with multiple-
stage martensite transformation are presented in Fig. 15. As for Q&P
steel after intercritical annealing, the final austenite retention is

F Stage-1
F F

F F
F Stage-2

Carbon atoms ε carbide M1 before partitioning

Parent Austenite M2 M1 after partitioning
Austenite in M1 after partitioning Bainite ferrite
Austenite in bainite after partitioning

Fig. 15. Schematic diagrams of microstructure evolution with multiple-stage martensite transformation. Note that, the parent austenite after partial annealing is still plotted as hexagon,
which is beneficial to analyze.
 F. Peng et al. / Materials and Design 181 (2019) 107921
significant dependent on ferrite, martensite and bainite transforma-
tions. Firstly, the intercritical ferrite (IF) is preferentially nucleates and
grows in the PAGB during intercritical annealing. Subsequently, the ep-
itaxial ferrite (EF) grows without a nucleation process from IF into aus-
tenite during quenching process [10]. Simultaneously, a considerable
carbon gradient deriving from ferrite formation, including IF and EF for-
mations, occurs in austenite with high carbon content in the periphery
and low carbon content in the center [12]. By controlling the carbon gra-
dient to appropriate extent, a special two-stage martensite transforma-
tion separated by martensite stagnant stage was obtained during
quenching process (Fig. 3).
When quenching to a relatively high temperature that close to Ms.
temperature, such as 320 °C in this article, the center of parent austenite
with low carbon content has transformed into M1, i.e. occurred stage-1
martensite transformation (Fig. 5e). Meanwhile, a relatively larger vol-
ume fraction of austenite is retained after quenching. During the
partitioning process, some of the austenite carbon-enriched from ferrite
was still insufficient and transformed into CFB that preferentially nucle-
ated in the ferrite/austenite interface and austenite/M1 interface [28],
while some small particle or film-like austenite inside ferrite matrix
was sufficiently carbon-enriched and can be retained to room tempera-
ture (Fig. 5f). Simultaneously, the synergistic effect of carbon enrich-
ment from bainitic ferrite into neighbored austenite and carbon
partitioning from martensite lath into austenite, including inter-lath
austenite and austenite located in packet boundaries or ferrite/M1 in-
terface, plays a significant role on the austenite carbon enrichment. Fi-
nally, some austenite with insufficient stability transformed into M/A
island with M2 in the center and RA in the periphery (Fig. 5f). It should
be noted that the interface migration between austenite and initial mar-
tensite during partitioning also influences the final retained austenite
fraction and morphology (Fig. 9f), whilst the deterioration effect of ε
carbide precipitation on austenite retention should also take into con-
sideration (Fig. 7e). Finally, the retained austenite located in packet
boundary of M1, the periphery of M/A island, the interface of ferrite/
M1 and some austenite in CFB present blocky morphology, while the
retained austenite between martensite laths shows film-like morphol-
ogy with curved interface (Fig. 9f) and some retained austenite in CFB
possesses plate-like morphology with relatively larger size. In this
case, the austenite retention was mainly ascribed to ferrite and bainite
formation, while the carbon partitioning of M1 was not dominant.
When quenching temperature further decreased to a low tempera-
ture in stage-1 region, the low carbon region that transformed into
M1 expanded (Fig. 6), whilst some metastable austenite has also trans-
formed into bainite with corresponding volume fraction decreased
slightly (Fig. 10b). As a result, the austenite retained by martensite car-
bon partitioning increased significantly and played a dominant role on
the austenite retention, while the proportion of retained austenite cor-
responding to bainite decreased drastically. Hence, in the case of low
QT in stage-1 region (Q&P-250), the effect of carbon partitioning from
M1 is much more significant than that of carbon enrichment from
bainitic ferrite. As to the situation in martensite stagnant region (Q&P-
180/220), similar characteristics of constituent phases were observed.
As for specimen quenched to stage-2 region (Q&P-100/120) or
below (Q&P-65), most of the unstable retained austenite has trans-
formed into M1 during quenching process (Fig. 5a). As a result, the aus-
tenite retained after quenching possesses a much smaller size in all
locations, as compared to those of high QT cases. Hence, the final
retained austenite in all locations decreased to a smaller size compared
with the corresponding locations in high QT cases. Meanwhile, the de-
crease of RA is mainly ascribed to the decrease of austenite in martensite
(Fig. 10b), i.e. inter-lath austenite or packet boundary austenite. In addi-
tion, the effect of interface migration was negligible and therefore the
inter-lath retained austenite showed straight interface with continuous
(Q&P-120) or discrete (Q&P-65) morphology (Fig. 9a and b).
As a whole, it can be concluded that the selection of quenching tem-
perature determines the initial martensite fraction and austenite
11
characteristics before partitioning process, such as morphology, size, lo-
cation and carbon distribution, then further influences the subsequent
bainite formation and carbon partitioning behavior. As a result, the
final volume fraction, size, morphology, location and interface charac-
teristics of retained austenite are obtained significantly depending on
the selection of quenching temperature.
4. Conclusions
In this work, different quenching temperatures were applied in par-
tially austenitized Q&P steels with multiple-stage martensite transfor-
mation to investigate the interaction of martensite and bainite
transformations. The conclusions are as follows:
(1) All of the phase fractions, including initial martensite, bainite and
retained austenite, showed obvious three-stage variations, coin-
cided with the stage-1, stagnant and stage-2 of martensite trans-
formation, whilst the respective fraction of austenite retained by
bainite and initial martensite also represented three-stage varia-
tion.
(2) The characteristics of retained austenite were significantly de-
pendent on quenching temperature. In the case of high QT that
close to Ms. temperature, the retained austenite was mainly as-
cribed to carbon enrichment of bainite. With decreasing QT to
low temperature in stage-1 martensite transformation, the aus-
tenite retained by bainite principally decreased. When quenched
to stage-2 region or exceeding martensite regime, the austenite
retained by martensite carbon partitioning occupied the majority
of whole RA and the decrease of RA mainly corresponded to RA in
martensite, i.e. inter-lath austenite or packet boundary austenite.
(3) An identical partitioning end was achieved at different QTs with
similar mean carbon contents in RA (1.31–1.37 wt%), which sig-
nificantly exceeded the T0 line (0.974 wt% at 400 °C), while far
from the austenite carbon content under paraequilibrium condi-
tion. Hence, the effect of carbon partitioning from initial mar-
tensite played a crucial role on the final austenite carbon-
enrichment, irrespective of the initial martensite and bainite
fractions.
(4) The heterogeneous carbon distribution in parent austenite deriv-
ing from ferrite formation could influence the subsequent mar-
tensite transformation and corresponding martensite structure.
The block possessed much smaller size in high carbon content re-
gion, while the corresponding packet size was still much larger.
In particular, some particle martensite blocks surrounded by
neighbored blocks showed much smaller size and can be deter-
mined to be secondary martensite that formed in the final
quenching. Moreover, the significant martensite variant absence
and variant combination were observed.
Credit author statement
Fei Peng is the main researcher and main author of this work. Jiayu
Li, Xingli Gu and Xu Wang are co-workers of the research project and
provided experimental samples during the research. Pr. Yunbo Xu pro-
vided project management and consultation (including in-depth review
and enhancement of the manuscript before submission and revision).
Acknowledgements
This work was financially supported by the National Key R&D Pro-
gram of China (2017YFB0304105).
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