Materials Science & Engineering A 615 (2014) 436–446

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Materials Science & Engineering A

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

Study of microstructural evolution and strength–toughness

mechanism of heavy-wall induction bend pipe
Tao Zhou, Hao Yu n, Junli Hu, Shaoyang Wang
School of Materials Science and Engineering, University of Science and Technology Beijing, No. 30 Xueyuan Road, Haidian District, Beijing 100083, China

art ic l e i nf o a b s t r a c t

Article history: The induction bending and subsequent tempering process has recently been proven to be an optimal
Received 30 June 2014 technological route for the manufacture of bend pipe with a better combination of strength and
Received in revised form toughness. In this work, high temperature quenching followed by tempering treatment from 500 1C to
28 July 2014
700 1C has been applied to heavy-wall bend pipe steel produced by the ultra fast cooling technology. The
Accepted 29 July 2014
Available online 6 August 2014
evolutions of microstructure and dislocation were characterized by means of an optical microscope, the
positron annihilation technique (PAT), SEM, TEM, XRD and EBSD. Microstructure observations showed
Keywords: that fine and homogenous M/A islands as well as dislocation packages in a quasi-polygonal ferrite (QPF)
Induction bend pipe matrix after tempering at 600–650 1C generated an optimal combination of strength and toughness. At
Microstructure
higher tempering temperature, the yield strength decreased dramatically; however, the impact
Dislocation
toughness still remained at a high value of more than 300 J. Dislocation analysis by means of TEM,
Toughness
Microcrack propagation EBSD and PAT suggested that the decrease and pile-up of dislocation could provide better toughness and
tempering stability. EBSD analysis indicated that the average misorientation angle enlarged and the
effective grain size diminished with the tempering temperature increasing, and these caused more
energy cost during the microcrack propagation process with subsequent improvement in impact
toughness. Microcracks mainly originated from the interfaces between ferrite matrix and M/A islands.
The ring-type join-up of microcracks and the large number of branches formed during the propagation
process effectively improved the toughness. All these results benefit the cost-effective commercialization
of heavy-wall induction bend pipe with high performance.
& 2014 Elsevier B.V. All rights reserved.

1. Introduction
In the long-distance transportation of oil and gas, pipeline
transmission dominates because of its high safety, high efficiency
and low cost. Meanwhile, there is an increasing demand for
transporting oil and gas by pipeline at high operating pressure in
an attempt to increase the capacity [1]. This requires the use of
high strength parent steel, which allows wall thickness to be
significantly reduced and consequent reduction in weight [2]. It is
well known that the microstructure depends on alloy chemistry
and thermo-mechanical processing. During the production of
pipeline steels, the thermo-mechanical control process is the
preferred route due to the resulting fine-grained and desirable
microstructure. However, regarding higher strength steel grades
and/or heavy-wall thickness pipe designed for long-distance
transportation pipeline projects, the conventional laminar cooling
system cannot meet the requirements for producing a hot rolled
n
Corresponding author. Tel./fax: þ 86 10 62326588.
E-mail address: yhzhmr@126.com (H. Yu).
plate [3]. On account of low cooling capacity of the laminar cooling
system, more alloy elements, for instance Mo, are usually needed
to achieve the desired hardenability, which will not only lead to
increasing the alloying cost, but also cause problems such as
microstructural nonuniformity, higher hardness and poor welding
performance. In particular, for the heavy-wall thickness pipeline
steels, insufficient cooling capacity by the laminar cooling system
yields instability of comprehensive performance. Therefore, cool-
ing has become the bottleneck for developing and commercializ-
ing heavy-wall thickness pipeline steels. In this context, an ultra
fast cooling (UFC) device has been developed as the available
method for producing hot rolled products with high performance
and low cost [4]. In the process of pipeline steel, a UFC device can
achieve 2–5 times cooling rate higher than that of a regular
laminar cooling device [5]. This advanced technology presents
the advantages of increasing the strength and reducing alloy
addition levels through the strengthening contribution by finer
and uniform carbonitrides as a result of high undercooling degree
during the UFC process.
Confronted with the persistent development of oil and gas
pipeline project, bend pipes, as important fittings for changing

http://dx.doi.org/10.1016/j.msea.2014.07.101
0921-5093/& 2014 Elsevier B.V. All rights reserved.
 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446
transportation directions of oil and gas, present a huge demand.
Approximately 30–40% of the pipes are bent in the construction of
a pipeline project [6]. Cold bending is preferred, because it can be
performed in the field. When the bend radius is small, it is
necessary to apply a hot bending process, which applies localized
induction heating and fast water cooling on the pipe body. This
process allows the microstructure to be significantly changed with
consequent variations in mechanical properties, especially the
yield strength, resulting in the mechanical property below the
standard requirement [7]. And most of the invalidation accidents
are related to the quality of bends. The manufacturing process of
bends is one of the key technologies directly affecting the safety of
a pipeline. In order to guarantee the safety, subsequent tempering
heat treatment after induction bending is usually required to
obtain excellent comprehensive mechanical properties, and the
final quality and performance of bend pipe greatly depend on the
tempering process.
Published studies [6–11] about induction bend pipe mostly
focused on the choice of the manufacturing process and the
mechanical variation of different sampling locations around the
pipe circumference in the corresponding process. Wang et al. [1]
introduced a new alloy system for the induction bend pipe based
on the chemical composition of commercial X80 steel. There are
few finished papers concerning the mechanism of toughness and
strength during the manufacturing process of bend pipe, especially
for low-cost parent steel produced by UFC technology. In the
present work, the heat treatment process in the manufacturing
process of induction bend pipe has been stimulated. The micro-
structural evolution is discussed in details. More efforts are made
to understand the relationship between strength–toughness and
dislocation, misorientation angle, effective grain size as well as
microcrack propagation. These research findings have been uti-
lized to cost effectively commercialize heavy-wall induction bend
pipe with high performance.
2. Experimental
2.1. Material and process
The materials investigated are X80 grade parent steel designed
for induction bend pipe. The parent steel, with a thickness of
22 mm, is produced by thermo-mechanical controlled rolling via
UFC technology. The chemical composition of the investigated
steel is shown in Table 1. The carbon equivalent (CE) value is 0.445,
with both weldability and hardenability considered. Kondo [12]
suggested that the higher CE of induction bend pipe was beneficial
to increasing hardenability and minimizing the yield strength loss
during quenching. The equilibrium transformation temperatures
Ae3 and Ae1 calculated using Thermo-Calc software are 843 1C
and 712 1C, respectively. The specimens with dimensions of
12 mm  12 mm  75 mm for heat treatments were cut from the
middle of the tested plates along wall thickness direction, and
separated from the transverse direction. The details of the heat
treatment process used in this study are described in Fig. 1.
Table 1
Chemical composition of the investigated steel (wt%).
C Si Mn P S
0.04–0.07 0.1–0.3 1.5–2.0 r 0.020
a
CEIIW ¼ Cþ Mn/6 þ(Mo þ Crþ V)/5 þ(Cu þ Ni)/15.
b
CEPcm ¼ Cþ Si/30 þ(Mn þ Crþ Cu)/20 þMo/15 þNi/60 þ V/10 þ5B.
437
2.2. Microstructural investigation
Samples for metallographic analysis were prepared by wire cut
electrical discharge machining, mechanical grinding, polishing and
then etched with 4% nital. The microstructures before and after
heat treatments were investigated by an optical microscope (OM)
and a Zeiss Auriga field emission scanning electron microscope
(FE-SEM). To evaluate the microstructural characteristics of the
metallographic samples, the color tint-etching method was
employed with LePera agentia (equal portions of solutions: 1%
aqueous sodium metabisulfite and 4% Picral) [13–16]. The volume
fractions of individual microstructural constituents were deter-
mined by the Image Pro-Plus 6.0 software. Fractographic exam-
ination of tensile and impact specimens was performed to obtain a
better understanding of the microscopic fracture mechanism. For
further microstructural analysis, transmission electron microscopy
(TEM) observation was carried out on thin foils which were
prepared by cutting thin wafers from small coupons and grinding
them to 60–70 μm. Discs of about 3 mm diameter were punched
from the wafers and electropolished using a solution of 4%
perchloric acid in alcohol kept below  20 1C by liquid nitrogen.
These foils were examined by a JEM-2100(HR) TEM operated at
200 kV. Besides, the positron annihilation technique (PAT) was
used to analyze the change in dislocation density. A fast–slow
positron annihilation lifetime spectrometer was applied to mea-
sure positron annihilation lifetime of the specimens tempered at
different temperatures.
Electron back scatter diffraction (EBSD) analysis was performed
under the condition of tilt angle 701 and step size 0.2 μm in order
to study effective grain size and grain misorientation. The data
were post-processed with Channel 5 software provided by Oxford
HKL Technologys. Local misorientation was used to evaluate small
local strain gradients in the material. The local misorientation
distribution component calculated the average misorientation
between every pixel and its surrounding pixels, and assigned the
mean value to that pixel. In the present study, 8 neighbors were
used in this calculation and misorientations of over 51 were
discarded. Because the magnitude of local misorientation corre-
lated well with the density of dislocations and local strain, the
Fig. 1. A diagrammatic sketch of the heat treatment process.
Nbþ V þ Ti Crþ Mo CEIIWa CEPcmb
r 0.005 r 0.10 r 0.50 0.445 0.177
438 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446
magnitude of stress distribution in the tested steel can thus be
assessed by the magnitude of local misorientation.
X-ray diffraction (XRD) analysis was carried out to determine
the content of the retained austenite. Samples were scanned over
a 2θ range from 471 to 931 with a step size of 0.021 and a scanning
speed of 11/min in a Rigaku DMAX-RB X-ray diffractometer, oper-
ated at 40 V and 150 mA with a graphite monochromator and
filtered Cu radiation (λ ¼ 0.1506 nm). The volume fraction of the
retained austenite was calculated in accordance with Chinese
standard YB/T 5338–2006. Samples for XRD and EBSD analysis
were first ground and mechanically polished, and then electro-
lytically polished for stress relief in an electrolyte of 5% perchloric
acid in alcohol at 30 V for 25 s.
2.3. Mechanical properties testing
In order to assess the comprehensive mechanical properties,
the tensile test, the Vickers hardness test and the Charpy V-notch
impact test were performed. For tensile tests, specimens with
round cross-section of 5 mm in diameter and 25 mm of original
gage length were machined, according to Chinese standard GB/T
228.1-2010. Tensile tests were conducted at ambient temperature
on a universal tensile testing machine of 200 kN capacity at a
crosshead speed of 1.5 mm/min. According to Chinese standard
GB/T 229-2007, the Charpy V-notch impact specimens, with
dimensions of 10 mm  10 mm  55 mm were prepared. Charpy
impact tests were performed at  20 1C on an instrumented
impact machine of 450 J capacity. Vickers hardness tests were
conducted with testing force of 98 N on a digital display Vickers
hardness instrument (model: 430SVD), according to Chinese
standard GB/T 4340.1-2009. For an individual sample, the mean
value of seven test results was taken as hardness.
3. Results and discussion
3.1. Microstructural characteristics
3.1.1. Microstructural evolution
The optical and scanning microscopes photographs in Figs. 2–4
show the microstructural evolution during the heat treatment process.
The original as-rolled microstructure is a mixed microstructure of
granular bainite (GB) and quasi-polygonal ferrite (QPF) as shown in
Fig. 2, resulting from thermo-mechanical controlled processing with
UFC technology. Fig. 3a is the optical micrograph etched with LePera
etchant, where the yellowish, khaki, and white colored phases indicate
ferrite, bainite and M/A (martensite and retained austenite) islands,
respectively. The volume fraction of M/A islands in the quenching
microstructure is 3.08%. The corresponding XRD spectra are presented
Fig. 2. The (a) optical and (b) FE-SEM micrographs of as-rolled microstructures.
in Fig. 3c. The integrated intensity of austenite peaks of (200), (220)
and ferrite peaks of (200), (211) were used for calculating the volume
fraction of the retained austenite, the results showing that 1.24%
retained austenite is acquired. It can be seen from Fig. 3a and b that
the quenching microstructure predominantly consists of lath-bainite
(LB), acicular ferrite (AF) and a small fraction of M/A islands. The
austenite grain boundaries are clearly visible, as indicated by the
arrows. These observations indicate that the AF nucleates at prior
austenite grains boundary and then divides the austenite grains into
different regions. The latter are further divided by AF nucleated inside
the austenite grains. As the temperature becomes lower than the
bainite starting transformation temperature, the remaining austenite
transforms into LB [2].
The tempering microstructures at different temperatures after
water quenching are shown in Fig. 4. The microstructural compo-
nent of the investigated steel tempered at temperatures of 500 1C
and 550 1C are LBþGB, as shown in Fig. 4a and b. The prior
austenite grain boundaries can be clearly observed, and strip M/A
constituents exist at prior austenite grain boundaries as well as
interfaces of bainitic ferrite (BF) laths. The M/A constituents in GB
are dot-like type. With increasing tempering temperature, BF
begins to merge and widen, and strip M/A islands in LB matrix
transform into dot-like or/and shot rod-like type, resulting in
augmenting volume fraction of GB, which is well indicated in
Fig. 4c. The M/A constituents distributing on prior austenite grain
boundaries have fully decomposed, leading to invisible prior
austenite grain boundaries. When tempered at 650 1C, the micro-
structure of the investigated steel mostly comprises GB þQPF, as
shown in Fig. 4d. The original BF becomes further widened and
polygonized, which refines the effective grain size. The M/A
constituents in the ferrite matrix become finer and partial ones
decompose to disappear. Fig. 4e reveals that microstructures after
tempering at 700 1C are QPF and large M/A particles. Due to the
higher tempering temperature, non-equilibrium microstructure
formed after quenching completely converts into QPF which has
less free energy. Furthermore, the austenite-reverted transforma-
tion occurs at high tempering temperature, because of element
enrichment of carbon and manganese around the grain boundaries
during the QPF transformation process, which leads to A1 trans-
formation temperature at grain boundary regions lower than
700 1C [17,18]. As shown in Fig. 4f, IPP analysis indicates that the
volume fraction of M/A islands is 5.96%, which has almost doubled
compared with that of quenched microstructures as shown in
Fig. 3a. This kind of reverted austenite is usually stable and most of
these austenites can be retained at ambient temperature.
3.1.2. TEM investigation
In order to further reveal the substructure of the investigated
steel after tempering at different temperatures, a transmission
 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446 439

Fig. 3. The microstructures after 950 1C quenching characterized by (a) color tint-etching optical micrograph, (b) FE-SEM micrograph and (c) XRD spectra analysis. (For
interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)

Fig. 4. The optical micrographs of X80 pipeline steel after tempering at (a) 500 1C, (b) 550 1C, (c) 600 1C, (d) 650 1C, and (e) 700 1C; (f) is color tint-etching optical micrograph
after tempering at 700 1C. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)

Fig. 5. TEM micrographs of bainitic ferrite tempered at (a) 500 1C and (b) 600 1C.

electron microscope was used for a detailed observation. TEM
investigation indicates that bainitic ferrite laths become large with
tempering temperature increasing, from 0.28 to 0.78 μm in width
after tempering at 500 1C to 0.42–1.58 μm at 600 1C, as shown in
Fig. 5. High dislocation density can be found inside the bainitic
ferrite matrix (Fig. 5a). When tempered at 600 1C, partial bainitic
ferrites become rod-like, showing a distinct trend to polygonize,
and dislocation density decreases due to recovery and recrystalli-
zation (Fig. 5b). Morphology and size of M/A islands varying with
tempering temperature are shown in Fig. 6. The results indicate
that large band-like M/A islands embedded in the ferrite matrix
have decomposed to be granular and their size decreases to
 250 nm. In general, M/A constituent is a kind of brittle phase,
and its shape, size and distribution have a great effect on the
440 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446
Fig. 6. TEM micrographs of M/A island tempered at (a) 500 1C and (b) 600 1C.
Fig. 7. Nominal stress–strain curves of the room temperature tensile tests of the
specimens as quenched and as tempered at 500 1C, 600 1C and 700 1C.
toughness of steel [19]. However, fine dot-like M/A constituent is
beneficial for the improvement of toughness and strength [10].
3.2. Mechanical properties
The nominal stress–strain curve of the quenching sample is
shown in Fig. 7 indicated by black color. The tensile test result
indicates that yield strength (Rt0.5) is 514 MPa, lower than the
standard requirement of 555 MPa. The decrease of yield strength
can be attributed to the so-called round-house type stress–strain
curve where no Luders elongation can be observed. It can also be
seen that the stress–strain curves of specimens tempered at both
500 1C and 600 1C exhibit high strength. Besides, the specimen
tempered at 600 1C shows better ductility than that at 500 1C.
Moreover, after tempering at 500 1C, the specimen exhibits small
yield platform, which is attributed to stress relief of solution atoms
of C and N divorced from Cottrell gas mass in LB microstructure.
When tempered at 700 1C, the specimen exhibits continuous
yielding behavior during transformation from elastic to plastic
deformation, with low yield strength and high elongation as a
result of increasing volume fraction of weak QPF in this condition.
The analytical results of tensile tests, the Charpy V-notch
impact tests and the Vickers hardness tests are presented in
Fig. 8. It can be seen that tensile strength and yield strength show
no observed change except that total elongation keeps a steadily
growing trend, with the tempering temperature increasing from
500 1C to 650 1C. After tempering at 700 1C, total elongation shows
a sharp increase and tensile strength exhibits a slight decrease, but
the yield strength reduces dramatically. Fig. 8b shows the curves of
the Charpy impact energy and the Vickers hardness with temper-
ing temperature. At relatively lower tempering temperatures,
improvement of impact energy is mainly attributed to stress relief
and the formation of finely distributed M/A islands decomposed
from larger strip ones. These fine M/A islands effectively suppress
the formation and extension of tiny microcracks. The weak QPF
equilibrium microstructure is the main cause for the reduction in
impact toughness after tempering at 700 1C. Besides, the second-
ary hardening phenomenon of high temperature tempering occurs
after tempering at 600 1C and 650 1C, with the Vickers hardness
value being 269 and 261, respectively. It can be attributed to
precipitation of various kinds of carbides in conjunction with
decomposition of M/A islands. Ma et al. [20] evidenced that
carbide precipitation of Cr and Mo could give rise to secondary
hardening in high temperature tempering process of Mo–Cr alloy
steel and precipitation temperature was related to volume fraction
of the retained austenite as well as precipitation thermodynamics
and kinetics. It can be seen from EDX analysis (Fig. 9d) that some
carbides of Mo and Cr precipitate in the investigated steel after
tempering at 600 1C.
3.3. Dislocation investigation
3.3.1. Dislocation morphology by TEM
Fig. 9 shows the dislocation morphology in the investigated
steel after tempering at 600 1C. From Fig. 9 it can be seen that
dislocations mostly exist in the form of dislocation package
distributed in the ferrite matrix (Fig. 9a) or near grain boundaries
(Fig. 9b). Wu et al. [21] suggested that two types of dislocations
existed in the bainite lath. One type is high-density dislocation
which tangles with each other, on which precipitates can be seen,
and it is difficult to eliminate dislocation by tempering. The other
type of dislocation is usually well distributed and arrayed parallel
to each other, ready to slip to grain boundaries and disappear, and
cannot accommodate precipitates. It can be inferred that disloca-
tion in the investigated steel belongs to the first type. Such kind of
dislocation generates good tempering stability and similar
strength property after tempering from 500 1C to 650 1C. At high
magnification of TEM (Fig. 9c), it can be seen that most disloca-
tions in the ferrite matrix are pinned by precipitates. This kind of
dislocation is well distributed and arrayed parallel to each other
but on which precipitates are observed. Therefore, it is not
completely consistent with the second type as Wu et al. suggested.
These tangled and pinned dislocations are conducive to steady and
high tempering strength of the investigated steel. The energy
dispersive X-ray (EDX) analysis in Fig. 9d indicates that these
particles are precipitates of (Nb,Ti)(C,N). Guo et al. [2] pointed out
that there are two kinds of strengthening mechanisms for Nb
microalloyed steel based on its precipitation of carbide and nitride
at different temperatures. One kind of precipitates forms in
austenite grains, with coarse size of 30–150 nm, which hinders
the recrystallization of austenite grains. The other kind of particle
precipitates within ferrite grains, whose size is 10–30 nm or even
 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446 441

Fig. 8. The curves of mechanical properties versus temperature. (For interpretation of the references to color in this figure, the reader is referred to the web version of this
article.)

Fig. 9. Dislocation morphology of the investigated steel after tempering at 600 1C.

much smaller, contributing to precipitation strengthening. In the
present work, most precipitates are in size of less than 10 nm and
belong to the second type as Guo et al. suggested, and they are
closely related to high cooling rate and high undercooling degree
during the UFC process.
3.3.2. Local strain distribution by EBSD
Fig. 10 shows local misorientation distribution maps of the
investigated steel at various tempering temperatures. The local
misorientation distribution maps are used to evaluate small local
strain gradients in the material [22–24]. This is a very efficient way
to localize the areas of stress concentration by a misorientation
range between 01 and 51. In Fig. 8, the blue color indicates
misorientations less than 11, green between 11 and 21, yellow
between 21 and 31, orange between 31 and 41 and red between 41
and 51. The misorientations larger than 51 are not taken into
consideration, because they may be due to the development of low
angle grain boundaries. Mapping results show that most of the
areas in blue, i.e., local misorientation range between 01 and 11,
correspond to the ferrite areas. And the areas of misorientations
larger than 11 become smaller with tempering temperature
increasing from 500 1C to 700 1C, which is related to the decrease
of dislocation density and stress relief in the process of recovery
and recrystallization. The areas indicated by yellow color are
characterized with lath-like distribution as shown in Fig. 10a, as
442 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446

Fig. 11. Change of (a) local misorientation and (b) misorientation angle at various
tempering temperatures.

led to shear stress and dislocation pile-up. It can also be observed

in Fig. 10c that some orange areas exist in the boundaries of
equilibrium ferrite microstructure due to dislocation pile-up
around hard reverted austenite phase. Microvoid nucleation initi-
ally takes place around these areas during the deformation
process.

Fig. 10. Local misorientation distribution maps showing strain distribution of X80
pipeline steel at various tempering temperatures: (a) 500 1C, (b) 600 1C, and 3.3.3. Dislocation density analysis by positron annihilation technique
(c) 700 1C. The high-angle grain boundaries ( 4 151) are delineated in black solid Being sensitive to defects in the solid materials, positron has
lines. (For interpretation of the references to color in this figure, the reader is been widely used to study the defects such as dislocation and
referred to the web version of this article.)
vacancy in iron [26]. In the present work, a fast–slow positron
annihilation lifetime spectrometer is used to measure the positron
Table 2 annihilation lifetime of the specimens at different tempering
Parameters of the dislocation density obtained by the positron annihilation temperatures, with Table 2 showing the measured parameters.
technique.
Among which, τ1 is positron lifetime affected by perfect body and
Tempering temperature τ1 I1 τ2 I2 τ3 I3 small defects (vacancies and dislocation); τ2 is positron lifetime
(1C) (10  10 s) (%) (10  10 s) (%) (10  9 s) (%) affected by larger defects (vacancy clusters, voids and micro-
fractures); τ3 is positron lifetime affected by source and surface
500 0.693 30.2 1.586 68.3 1.605 1.56 of specimens; I1, I2 and I3 are intensities of τ1, τ2 and τ3 in positron
600 0.938 45.0 1.839 52.2 1.327 2.75
700 1.369 78.3 3.000 18.7 1.743 2.96
annihilation lifetime spectrum, respectively. A previous study [27]
shows that positron lifetime depends on its annihilation state. The
annihilation rate in a given state, i.e., the inverse of the lifetime, is
a consequence of dislocation pile-up in the interfaces of quenching proportional to overlap of electron and position densities. Because
LB laths. Zaefferer [25] suggested that significant volume expan- the testing specimen in this study has undergone high tempera-
sion occurred during the bainitic transformation process and thus ture tempering treatment, τ1 is mainly attributed to perfect body
 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446
and dislocation, and it is inversely proportional to dislocation
density. It can be concluded that dislocation density has a clear
trend to decrease with the tempering temperature increasing. The
decrease of dislocation density is beneficial to the toughness.
Because high dislocation density can increase the trend of disloca-
tion pile-up and internal stress, and it promotes the nucleation
and propagation of microcrack, leading to decrease in toughness,
this result together with TEM and EBSD analysis suggest that the
decrease of dislocation density in conjunction with local pile-up
and pinning of dislocation partially contribute to the favorable
combination of strength and toughness.
3.4. Misorientation angle and effective grain size analysis by EBSD
Fig. 11a presents the quantitative analysis of strain distribution
in the ferrite matrix at tempering temperatures of 500 1C, 600 1C
and 700 1C. It is observed that the curve of local misorientation
moves left with increasing tempering temperature. The average
local misorientation decreases from 0.81 to 0.75 and 0.71 with the
tempering temperature increasing from 500 1C to 600 1C and
700 1C, which is in good agreement with the variation of blue
and yellow color regions in Fig. 10. The misorientation angle
distributions from 01 to 601 are shown in Fig. 11b. It is observed
that the relative frequency of low misorientation angle less than
151 is much higher at tempering temperature of 500 1C in contrast
with 600 1C and 700 1C. This is due to the presence of LB with more
subgrains in this condition. When the tempering temperature
Table 3
Effective grain size analyzed by EBSD (threshold angle with 151).
Tempering Average size Average equivalent circle
temperature (1C) (μm) diameter (μm)
500 16.117 2.05 4.45 7 0.39
600 9.05 7 1.83 3.36 7 0.34
700 8.52 7 1.21 3.197 0.29
Fig. 12. SEM images of the tensile fracture appearance of the investigated steel after tempering at (a) 500 1C, (b) 600 1C, and (c) 700 1C.
Fig. 13. SEM images of the  20 1C impact fracture morphology of the investigated steel after tempering at 600 1C: (a) macrograph of fracture; (b) pars fibrosa; (c) shear zone.
443
increases to 600 1C and 700 1C, recrystallization occurs, consequently
relative frequency of low misorientation angle less than 151 reduces
and that of high misorientation angle larger than 501 increases.
Moreover, this kind of microstructure transformation refines the
effective grain size, and the detailed data is summarized in Table 3.
The calculated results reveal that the average misorientation angle
increases from 28.191 to 30.501 and 34.121 with the tempering
temperature increasing from 500 1C to 600 1C and 700 1C. Previous
published studies [28–30] suggested that grain interfaces with large
angle could effectively boost the impact toughness. In the course of
fracture, larger angle twist will take place when crack propagation
encounters the large angle interfaces. The more the large angle
interfaces, the more the crack twist as well as energy cost in the
process of crack propagation. However, the small angle interfaces
have less effect on the crack twist as well as the improvement of
impact toughness compared with the large ones. In the present
study, the average misorientation angle increases and the effective
grain size decreases with the rise of tempering temperature. The
smaller the effective grain size, the more the large angle interfaces
that crack propagation need to pass through, with consequent
increase in energy cost and subsequent improvement in impact
toughness.
3.5. Microscopic fracture analysis
3.5.1. The morphology of fracture surface
To evaluate the microfracture mechanism, fractography was
applied on the uniaxial tensile and the Charpy impact specimens
as shown in Figs. 12 and 13, respectively.
The tensile fracture surfaces of the investigated steel under
various tempering temperatures are all characterized by tremen-
dous small dimples and a few large ones (large dimples about
7.51–31.26 μm at tempering temperature of 500 1C, around 5.76–
21.26 μm at 600 1C, and approximately 3.87–18.86 μm at 700 1C),
a typical characteristic of ductile fracture mechanism. On the
fracture surface, dimples with different sizes can correspond to
444 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446
various void-nucleating mechanisms. The small dimples mainly
originate from fine carbonitride particles precipitated in the
matrix during the cooling and tempering processes. Because of
the weak bonding force between the fine precipitated phases and
the relatively soft matrix, microvoids readily form in the interfaces
during tensile deformation. For the big dimples, they mainly result
from M/A islands and inclusion particles. At the bottom of large
dimples, no inclusion such as MnS or oxide particles [31,32] has
been observed in the present work. It can be partly attributed to
relatively lower volume of inclusions than M/A constituents. With
more voids generating and joining up in the interfaces between
M/A islands and the ferrite matrix during tensile deformation, the
former are finally pulled out from the latter. There are more large
dimples in Fig. 12a in contrast with those in Fig. 12b, which is
attributed to the decomposition of large size and quantity of M/A
islands into small ones or even disappearing during the tempering
process from 500 1C to 600 1C. The small dimples become larger
and more uniform where the fine carbonitride particles gather and
grow in the equilibrium microstructure after tempering at 700 1C
(Fig. 12c), showing excellent ductility. The tensile fracture analysis
is well in agreement with tensile testing results in Figs. 7 and 8.
As described in Fig. 8b, the investigated steel shows favorable
impact toughness after tempering heat treatment. In order to
further verify this result, the impact fracture morphology of the
investigated steel after tempering at 600 1C has been studied, as
shown in Fig. 13. The macrograph (Fig. 13a) indicates that the
fracture is composed of V-shaped notch, shear lip and pars fibrosa,
and no obvious radiation area is observed. Large amounts of
dimples can be seen in the pars fibrosa, which is a typical feature
of excellent impact toughness. Moreover, tearing ridges are clearly
observed in areas of both pars fibrosa and shear lip.
3.5.2. The initiation and propagation of microcrack
To study the correlation between microcrack initiation as well
as crack propagation and microstructure, the cross-sectional sec-
tion beneath the impact fracture surface of the Charpy impact
specimens has been investigated [33] as illustrated in Fig. 14.
From Fig. 15a and b, it can be seen that microcracks mainly
nucleate around fine dot-like M/A islands which are hard phases
in contrast with the weak ferrite matrix so that high stress
concentration readily emerges on their interfaces. The microcracks
can nucleate at the interfaces once the concentrated stress is
higher than the binding force of M/A phase and matrix. Chen et al.
[34] also evidenced that due to the heavy strain of ferrite, the
stress concentrated on the interfaces between M/A constituent
and ferrite and caused the former to debond from the latter.
Fig. 14. Schematic of the observed section of impact fracture.
During impact deformation, with more microcracks generating
and gathering to merge with each other, a large crack forms and
propagates along the interfaces of M/A islands and the ferrite
matrix. Besides, obvious plastic deformation is observed in the two
photographs, which means that it consumes a large amount of
energy in the final fracture process of the tested specimen.
In Fig. 15c and d, two types of crack propagation models are
presented in the investigated steel. One type is that the microvoids
nucleated at the interfaces between M/A constituent and the
ferrite matrix propagate to connect with each other until forming
many independent ring-like units, as shown in Fig. 15c. The crack
is related to the size of M/A islands, which is inversely propor-
tional to the binding force. Thus, the larger the size of M/A islands,
the higher the possibility that the microcracks will come up and
connect with each other [35]. As EBSD analysis indicated in
Fig. 10c, many fine reverted austenite grains form in the bound-
aries of ferrite, which are preferential positions for microvoid
nucleation. These micovoids are prone to join up with each other
along the ferrite boundaries; consequently one or several ferrite
grains have been divorced from the matrix in the form of ring-like
units. These units can effectively prevent the follow-up extension
of crack. The other type of crack propagation is that the microvoids
can join up to extend forward along the deformed microstructural
interfaces as presented in Fig. 15d. The crack is tortuous and many
branch cracks form on both sides of the main crack. These
phenomena happen when the concentrated stress falls into the
value between the binding force of M/A islands and that of the
M/A island and the ferrite matrix. The M/A islands are hard to be
cut through with the presence of soft ferrite phase. These indicate
that the process of crack propagation can absorb more energy with
resulting improvement in impact toughness. The above two types
of crack propagation can explain the reason why the investigated
steel retain excellent impact toughness even at higher tempering
temperature.
4. Conclusions
The heat treatment process of induction bend pipe manufac-
turing has been simulated on the heavy-wall parent steel pro-
duced via UFC technology. Microstructural evolution, mechanical
properties, microcrack propagation and strength–toughness
mechanism have been systematically studied. The results are
summarized as follows:
(1) The investigated steel achieves optimal combination of
strength and toughness after tempering at 600–650 1C, with
 T. Zhou et al. / Materials Science & Engineering A 615 (2014) 436–446
Fig. 15. Microcracks underneath the fracture surface of the Charpy V-notch impact tests for the investigated steel after tempering at (a and b) 600 1C and (c and d) 700 1C.
the microstructure comprising fine and homogenous M/A
islands as well as dislocation packages in the quasi-polygonal
ferrite (QPF) matrix. At higher tempering temperature, the
yield strength decreases dramatically.
(2) The tangled and pinned dislocation as well as carbide pre-
cipitation results in good tempering stability and high strength
property of the investigated steel.
(3) The decrease of dislocation density can reduce the trend of
dislocation pile-up and internal stress and weaken the nuclea-
tion and propagation of microcrack, which are beneficial for
toughness.
(4) The average misorientation angle grows and the effective grain
size diminishes with increasing tempering temperature, which
can cause more energy loss during the process of microcrack
propagation, leading to improvement in impact toughness.
(5) Microcrack mainly originates from the interface between
ferrite and M/A island. The ring-type join-up of microcracks
and the large amount of branches formed in the propagation
process can effectively improve the toughness.
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