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Revealing the role of dislocations on the stability of retained austenite in a

tempered bainite

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DOI: 10.1016/j.scriptamat.2019.04.019

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 Scripta Materialia 168 (2019) 23–27

Contents lists available at ScienceDirect

Scripta Materialia

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

Revealing the role of dislocations on the stability of retained austenite in a

tempered bainite
S.H. He a,b, B.B. He a,b, K.Y. Zhu c, R. Ding d, H. Chen d, M.X. Huang a,b,⁎
a
Shenzhen Institute of Research and Innovation, The University of Hong Kong, Shenzhen, China
b
Department of Mechanical Engineering, The University of Hong Kong, Pokfulam Road, Hong Kong, China
c
ArcelorMittal Research, Voie Romaine-BP30320, 57283 Maizières-lès-Metz cédex, France
d
Key Laboratory for Advanced Materials of Ministry of Education, School of Materials Science and Engineering, Tsinghua University, Beijing, China

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

Article history: The present study, for the first time, provides direct experimental evidence revealing the effect of dislocations of
Received 23 February 2018 the bainite matrix on the mechanical stability of retained austenite (RA) in a low carbon bainitic steel, while
Received in revised form 20 December 2018 keeping all other influencing factors unchanged. A lower strength of bainitic matrix caused by its reduced dislo-
Accepted 6 January 2019
cation density results in more stress partitioning onto RA during plastic deformation, which promotes the trans-
Available online xxxx
formation of RA to martensite. In addition, the annihilation of dislocations in the bainite matrix relaxes the
Keywords:
compressive stress field resulted from the bainitic transformation, facilitating the martensitic transformation
Tempered Bainite during deformation.
Dislocation density © 2019 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Carbide-free bainite
TRIP effect
Retained austenite

Owing to the excellent combination of strength, ductility, toughness
and weldability, low carbon carbide-free bainitic steels have been inten-
sively studied during the past decades [1–3]. It has been shown that the
transformation-induced plasticity (TRIP) effect is an effective way to
improve the strain hardening behavior of low carbon bainitic steels
[4]. The mechanical stability of retained austenite (RA) can be affected
by the chemical compositions [5]. In particular, the C content that is
enriched during bainitic transformation plays an important role in the
mechanical stability of RA [6,7]. In addition, the morphology of RA can
also affect its mechanical stability. For instance, filmy RA is usually
more stable than blocky RA [8,9]. Moreover, dislocations and deforma-
tion twins in RA tends to stabilize the RA by mechanical stabilization
mechanism [10–12]. Besides the aforementioned intrinsic factors, the
mechanical stability of RA can also be influenced by the microstructure
of the bainitic matrix [8,13,14]. Both lath thickness and dislocation den-
sity are important microstructure parameters that determine the me-
chanical properties of bainitic steels [15]. Therefore, it could be
expected that both lath thickness and dislocation density of the bainitic
matrix could also affect the mechanical stability of RA in the low carbon
carbide-free bainitic steels. Nevertheless, it is very challenging to distin-
guish the role of an individual factor in the mechanical stability of RA
when the above factors are varying simultaneously. The present work
⁎ Corresponding author at: Shenzhen Institute of Research and Innovation, The
University of Hong Kong, Shenzhen, China.
E-mail address: mxhuang@hku.hk (M.X. Huang).
intends to reveal the effect of dislocations of the bainite matrix on the
mechanical stability of RA, while keeping all other influencing factors
unchanged.
The chemical composition of the steel investigated in the present
work is Fe-0.25C-2Mn-1.5Al (in wt%). A 50 kg ingot is cast using vacuum
induction melting and hot rolled to a thickness of 2.8 mm with a finish
rolling temperature of 900 °C. Samples with a dimension of 10 mm
(length) x 4 mm (width) x 2.6 mm (thickness) are machined from the
hot rolled sample. Then, an austenitization at 1000 °C for 300 s followed
by isothermal holding at 400 °C for 600 s is carried out using a Linseis
dilatometer L78 to obtain the bainite microstructure. Some samples
are subjected to an additional tempering treatment at 200 °C for
1800 s, which are defined hereafter as tempered bainite. The samples
without such additional tempering treatment are termed as normal bai-
nite. Both the tempered bainite and normal bainite are then subjected to
cold rolling at room temperature with 3% and 20.6% thickness reduction
(corresponding to 3.1% and 23.1% equivalent strain, respectively) [16].
The Vicker hardness measurement is performed with an applied load
of 10 Kg and each measurement is comprised of 5 indents. The scanning
electron microscopy (SEM) observations are carried out using a Hitachi
S4800 FEG-SEM operated at 5 kV. The samples for SEM observation are
etched using 2% nital solution for 30 s after conventional mechanical
polishing of 1 μm. A PHI-710 type nano-auger electron spectroscopy
equipped with electron backscatter diffraction (AES-EBSD) is used to
measure the distribution of C content in RA. The spatial resolution is
about 18 nm under an operating voltage of 20 kV and a current of

https://doi.org/10.1016/j.scriptamat.2019.04.019
1359-6462/© 2019 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
24 S.H. He et al. / Scripta Materialia 168 (2019) 23–27

10 nA. The transmission electron microscopy (TEM) observations are
performed in an FEI Tecnai G20 scanning TEM (STEM) operated at
200 kV. The TEM samples are prepared by mechanical thinning down
to 0.1 mm, followed by twin-jet thinning in a solution of 5% perchloric
acid and 95% ethanol (vol%) at −30 °C with a potential of 40 V. The syn-
chrotron X-ray diffraction (XRD) data are obtained at the beamline
BL14B1 of the Shanghai Synchrotron Radiation Facility (SSRF) using X-
ray source with a wavelength of 0.68879 Å [17]. To record each line dif-
fraction patterns, a dwell time of 0.5 s is used. To fully utilize the limited
beam time without sacrificing the accuracy of measurement, the step
size selected as 0.01o for interested diffraction peaks while the step
size of other areas is chosen as 0.2o.
The initial microstructure of the normal bainite is shown in Fig. 1(a).
As it shows, the normal bainite consists of nearly equal-spaced bainitic
matrix and very thin lamellar structures. Such lamellar microstructure
remains in the tempered bainite after the tempering treatment as
shown in Fig. 1(b), indicating that the low-temperature tempering pro-
cess does not change the morphology of the bainite microstructure.
More interestingly, this lamellar microstructure can still be retained in
the normal bainite that is subjected to cold rolling with a thickness
reduction of 20.6% (Fig. 1(c)). Nevertheless, the lamellar microstructure
of the tempered bainite is altered after being subjected to cold rolling
with a 20.6% thickness reduction (Fig. 1(d)), exhibiting some wedge-
shaped structures (marked with red arrows) in the microstructure.
The lamellar structures in both normal and tempered bainite contain
filmy RA between bainite laths (Fig. 1(e)). The filmy RA has a
Kurdjumov-Sachs (K\\S) orientation relationship with the adjacent bai-
nite lath (Fig. 1(f)). Note that only a few carbide precipitations are ob-
served in both normal and tempered bainite (Fig. 1(a), (b) and (e)).
The formation of the wedge-shaped structure in the deformed structure
of the tempered bainite (Fig. 1(d)) could be due to the transformation of
RA into martensite.
The synchrotron XRD experiments are carried out to measure the
dislocation density, volume fraction and residual lattice strains of both
bainite and austenite phases. The dislocation density is calculated by
using the convolutional multiple whole profile (CMWP) method
[15,18,19]. The typical CMWP-fitted XRD pattern is shown in Fig. 2(a).
Five body-centered cubic (BCC) peaks are chosen to measure the dislo-
cation density in the bainitic matrix, while four face-centered cubic
(FCC) peaks are selected to calculate the dislocation density in RA. The

Fig. 1. SEM images of 0% cold rolled (a) normal bainite, (b) tempered bainite. SEM images of 20.6% cold rolled bainitic steel (c) normal bainite, (d) tempered bainite. (e) TEM dark field
images of 0% cold rolled normal bainite and (f) corresponding diffraction pattern showing an K\
\S orientation relationship between film-like retained austenite and adjacent bainite lath.
 S.H. He et al. / Scripta Materialia 168 (2019) 23–27 25

Fig. 2. (a) The observed (black symbol) and CMWP fitted (red line) synchrotron diffraction profiles for the normal bainite with 23% equivalent strain, in which d is the lattice spacing.
Residual between these two profiles is represented as blue line. The inset figure is the enlarged profiles with log scale in the vertical axis for the d values between 0.085 and 0.135 nm.
(b) The RA fraction evolution with plastic deformation. Measurement results of RA volume fraction are represented by solid dots. (For interpretation of the references to colour in this
figure legend, the reader is referred to the web version of this article.)

estimation of phase fraction is based on the integrated intensity of all
peaks [20,21], and the results are plotted in Fig. 2(b). The initial fractions
of RA in both normal and tempered bainite are almost the same, which
are consistent with the SEM observations (Fig. 1(a) and (b)). The vol-
ume fraction of RA in the normal bainite demonstrates negligible de-
crease after cold rolling (Fig. 2(b)). In contrast, the volume fraction of
RA in the tempered bainite decreases sharply (~40%) at a 3% thickness
reduction and then remains unchanged with further cold rolling reduc-
tion (Fig. 2(b)).
As shown in Fig. 3(a), the dislocation density of the bainitic matrix in
the tempered bainite before cold rolling is lower than that in the normal
bainite, indicating the tempering process reduces the dislocation den-
sity of the bainitic matrix. However, such tempering process does not
reduce the dislocation density of the RA. The dislocation densities of
the RA in both normal and tempered bainite increase with deformation
as shown in Fig. 3(a). Note that the deformation twins hardly exist in
filmy RA before large plastic deformation [11]. Thus, the twinning effect
on the RA stability is neglected in the present steel since the TRIP effect
only happens before 3% equivalent strain (Fig. 2(b)). Despite a lower
initial dislocation density of the bainite matrix in the tempered bainite,
it increases rapidly with cold rolling and finally reaches a higher value
than that of the normal bainite. Because the strength of the bainite

Fig. 3. (a) The dislocation density evolution in each phase of the bainitic steels with and without tempering. (b) The hardness of each sample with varying plastic deformation. (c) Evolution
of residual lattice strain in BCC matrix phase with tempering. (d) Evolution of average residual lattice strain in each phase without and with tempering.
26 S.H. He et al. / Scripta Materialia 168 (2019) 23–27

matrix increases with its dislocation density [15], the evolution of dislo-
cation density could be reflected from the hardness measurement. As
compared to the normal bainite, the tempered bainite has a lower hard-
ness before cold rolling (Fig. 3(b)), which is consistent with its reduced
dislocation density in the bainite matrix (Fig. 3(a)). More interestingly,
the hardness of the tempered bainite increases with deformation much
more significantly as compared to the normal bainite (Fig. 3(b)), which
is consistent with the observation on the evolution of dislocation den-
sity in the bainite matrix of both steels (Fig. 3(a)). Note that the initial
dislocation density in the RA is much higher than that in the bainite ma-
trix (Fig. 3(a)), which can be explained by the generation of dislocations
in the RA to accommodate the transformation strain during bainitic
transformation [22–24].
To further reveal the effect of bainite matrix on the stability of RA,
the residual lattice strain in each phase of the present bainitic steels
is analyzed. The lattice strain εhkl is calculated from the change in
lattice spacing d for 〈hkl〉 − oriented grain families along the normal
direction [25]:
 
0 0
εhkl ¼ dhkl −dhkl =dhkl ð1Þ
where the subscript “0” refers to the condition without tempering
and deformation. The calculated residual lattice strains in each
phase are summarized in Fig. 3(c) and (d). Tensile residual lattice
strain (positive value) has been observed in the bainite matrix
(Fig. 3(c)), while the RA develops a compressive residual strain (neg-
ative value) as shown in Fig. 3(d). These results indicate that RA is a
harder phase, which is the same as that in the TRIP-assisted multi-
phase steels [26,27]. Since the bainite matrix has a larger lath thick-
ness (Fig. 1(e)) and a lower dislocation density (Fig. 3(a)) as
compared to those in RA, the bainite matrix deforms as a soft phase.

Fig. 4. SEM images for the selected areas of the (a) normal bainite and (b) tempered bainite. EBSD image quality maps for the selected areas with phase maps marking RA in red and
corresponding C profiles of line scans in (c,e) normal bainite and (d,f) tempered bainite. (For interpretation of the references to colour in this figure legend, the reader is referred to
the web version of this article.)
 S.H. He et al. / Scripta Materialia 168 (2019) 23–27
The evolution of average residual lattice strain εhkl in each phase is
shown in Fig. 3(d). The amount of increased εhkl with an equivalent
strain in the tempered bainite is higher than that in the normal bainite,
indicating that deformation of the bainitic matrix in the tempered bai-
nite is more severe than that in the normal bainite. This could be due
to the recovery of initial dislocation density (Fig. 3(a)) so that the bai-
nite matrix in the tempered bainite has a lower strength. Consequently,
more strain is partitioned to the bainite matrix in the tempered bainite,
resulting in a higher ε hkl after deformation, which is consistent with the
SEM observation (Fig. 1(c) and (d)). Meanwhile, this partitioning of
strain also leads to a higher accumulation rate of dislocation density in
the bainite matrix of the tempered bainite (Fig. 3(a)). Since the trans-
formed martensite is much harder than the bainite matrix [28], the par-
tition of strain may cause the even higher value of dislocation density of
the bainite matrix in the tempered bainite than that in the normal bai-
nite at the final rolling state.
To examine the carbon partitioning during the tempering process,
the carbon content of RA is analyzed based on the XRD results. Detailed
discussion can be found in Section 1 of supplementary material. The av-
erage carbon content of RA in both normal bainite and tempered bainite
is in the range of 1.29–1.38 wt%, indicating an insignificant effect of tem-
pering process on carbon partitioning. However, the average value of
the carbon content provided by the XRD results may not be accurate
enough to study the carbon partitioning of individual RA [29]. To further
examine the carbon distribution in RA, C profiles across different phases
in both normal and tempered bainite are measured using the AES-EBSD
technique, as shown in Fig. 4. The lamellar second phase with darker
contrast (marked with yellow arrows in Fig. 4) in SEM images (Fig. 4
(a) and (b)) are confirmed as RA from EBSD observations (Fig. 4
(c) and (d)). The carbon content inside these RA is around 1.1–1.6 wt
% in both normal and tempered bainite (Fig. 4(e) and (f)), suggesting
the carbon flux between RA and the surrounding phase are not signifi-
cant during the 200 °C tempering process. Such insignificant effect can
be explained by the long bainitic holding duration at 400 °C, which al-
lows sufficient carbon partitioning between RA and the matrix. Since
the carbon content in RA is already close to its saturated value (Fig. 4
(e)) [29], Thus, both the AES-EBSD and synchrotron XRD results prove
that the carbon content of RA remains the same after the 200 °C temper-
ature process. The effect of carbon content on the destabilization of RA
in the tempered bainite can be eliminated. Texture evolution is analyzed
in Section 2 of supplementary material and its effect on RA stability is
also eliminated. In addition, the effect of morphology and grain size of
the RA can also be excluded because the 200 °C tempering process
does not change these factors (Fig. 1(a) and (b)). Therefore, the more
significant TRIP effect in the tempered bainite (Fig. 2(b)) could be only
explained by the reduced dislocation density in the bainite matrix. A
more quantitative estimation of the strength in each phase is given in
Section 3 of the supplementary material to further support this
statement.
The reduced dislocation density in the bainitic matrix may destabilize
the RA in two ways. Firstly, the lower strength of the bainite matrix re-
sults in more stress partitioning onto RA during plastic deformation.
The higher phase stress provides more mechanical driving force for the
transformation of RA into martensite. Secondly, the formation of bainite
accompanies with an expansion strain during the bainitic transforma-
tion, which may result in compressive residual stress between the adja-
cent lamellar RA. The annihilation of initial dislocation density in the
bainite matrix during the low-temperature tempering relaxes such com-
pressive stress field and develops an initial tensile residual stress after
recovery (Fig. 3(d)), facilitating the martensitic transformation in RA.
View publication stats
27
In summary, the present study demonstrates experimentally, for the
first time, that the mechanical stability of RA in a low carbon bainitic
steel can be affected by the dislocation density of the bainite matrix. A
lower dislocation density in the bainite matrix can lead to a lower me-
chanical stability of RA.
Acknowledgments
M.X. Huang acknowledges the financial support from National Key
Research and Development Program of China (No. 2017YFB0304401),
National Natural Science Foundation of China (No. U1764252,
U1560204), and Research Grants Council of Hong Kong (No.
17255016, 17203014). The authors thank the beamline BL14B1 (Shang-
hai Synchrotron Radiation Facility) for providing the beam time and
technical supports during experiments.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.dummy.2019.01.002.
References
[1] F.G. Caballero, H.K.D.H. Bhadeshia, Curr. Opin. Solid State Mater. Sci. 8 (3–4) (2004)
251–257.
[2] M. Soliman, H. Palkowski, Arch. Civ. Mech. Eng. 16 (3) (2016) 403–412.
[3] C. Garcia-Mateo, G. Paul, M.C. Somani, D.A. Porter, L. Bracke, A. Latz, C.G. de Andres,
F.G. Caballero, Metals 7 (5) (2017).
[4] P. Jacques, Q. Furnémont, A. Mertens, F. Delannay, Philos. Mag. A Phys. Condens.
Matter Struct. Defects Mech. Prop. 81 (7) (2001) 1789–1812.
[5] H.K.D.H. Bhadeshia, R.W.K. Honeycombe, Steels: Microstructure and Properties,
Fourth edition, 2017.
[6] H.K. Yeddu, A. Borgenstam, P. Hedström, J. Ågren, Mater. Sci. Eng. A 538 (2012)
173–181.
[7] Y.K. Lee, J. Mater. Sci. Lett. 21 (16) (2002) 1253–1255.
[8] X.C. Xiong, B. Chen, M.X. Huang, J.F. Wang, L. Wang, Scr. Mater. 68 (5) (2013)
321–324.
[9] P.J. Jacques, F. Delannay, J. Ladrière, Metall. Mater. Trans. A Phys. Metall. Mater. Sci.
32 (11) (2001) 2759–2768.
[10] H.K.D.H. Bhadeshia, Mater. Sci. Technol. 15 (1) (1999) 22–29.
[11] Z. Xiong, G. Casillas, A.A. Saleh, S. Cui, E.V. Pereloma, Sci. Rep. 7 (1) (2017).
[12] I.B. Timokhina, P.D. Hodgson, E.V. Pereloma, Metall. Mater. Trans. A Phys. Metall.
Mater. Sci. 38 (10) (2007) 2442–2454.
[13] J. Han, S.J. Lee, J.G. Jung, Y.K. Lee, Acta Mater. 78 (2014) 369–377.
[14] J.H. Ryu, D.I. Kim, H.S. Kim, H.K.D.H. Bhadeshia, D.W. Suh, Scr. Mater. 63 (3) (2010)
297–299.
[15] S.H. He, B.B. He, K.Y. Zhu, M.X. Huang, Acta Mater. 135 (2017) 382–389.
[16] H.P. Stüwe, Adv. Eng. Mater. 5 (5) (2003) 291–295.
[17] T.Y. Yang, W. Wen, G.Z. Yin, X.L. Li, M. Gao, Y.L. Gu, L. Li, Y. Liu, H. Lin, X.M. Zhang, B.
Zhao, T.K. Liu, Y.G. Yang, Z. Li, X.T. Zhou, X.Y. Gao, Nucl. Sci. Tech. 26 (2) (2015).
[18] Z.Y. Liang, Y.Z. Li, M.X. Huang, Scr. Mater. 112 (2016) 28–31.
[19] T. Ungár, S. Harjo, T. Kawasaki, Y. Tomota, G. Ribárik, Z. Shi, Metall. Mater. Trans. A
Phys. Metall. Mater. Sci. 48 (1) (2017) 159–167.
[20] A.K. De, D.C. Murdock, M.C. Mataya, J.G. Speer, D.K. Matlock, Scr. Mater. 50 (12)
(2004) 1445–1449.
[21] X.H. Hu, X. Sun, L.G. Hector Jr., Y. Ren, Acta Mater. 132 (2017) 230–244.
[22] F.C. Frank, Acta Metall. 1 (1) (1953) 15–21.
[23] G.B. Olson, M. Cohen, Acta Metall. 27 (12) (1979) 1907–1918.
[24] B.P.J. Sandvik, C.M. Wayman, MTA 14 (4) (1983) 809–822.
[25] Y. Wang, T. Ohnuki, Y. Tomota, S. Harjo, T. Ohmura, Scr. Mater. 140 (2017) 45–49.
[26] S. Harjo, T. Kawasaki, Y. Tomota, W. Gong, K. Aizawa, G. Tichy, Z. Shi, T. Ungár,
Metall. Mater. Trans. A Phys. Metall. Mater. Sci. 48 (9) (2017) 4080–4092.
[27] Y. Tomota, H. Tokuda, Y. Adachi, M. Wakita, N. Minakawa, A. Moriai, Y. Morii, Acta
Mater. 52 (20) (2004) 5737–5745.
[28] B.B. He, K. Zhu, M.X. Huang, Philos. Mag. Lett. 94 (7) (2014) 439–446.
[29] C. Garcia-Mateo, F.G. Caballero, M.K. Miller, J.A. Jimenez, J. Mater. Sci. 47 (2) (2012)
1004–1010.