metals
Article
Correlation between Microstructure and Mechanical Properties
of Welded Joint of X70 Submarine Pipeline Steel with Heavy
Wall Thickness
Yifan Dong 1 , Denghui Liu 1,2 , Liang Hong 1 , Jingjing Liu 1 and Xiurong Zuo 1, *
Citation: Dong, Y.; Liu, D.; Hong, L.;
Liu, J.; Zuo, X. Correlation between
Microstructure and Mechanical
Properties of Welded Joint of X70
Submarine Pipeline Steel with Heavy
Wall Thickness. Metals 2022, 12, 716.
https://doi.org/10.3390/
met12050716
Academic Editor: Andrea Di Schino
Received: 20 March 2022
Accepted: 19 April 2022
Published: 22 April 2022
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Metals 2022, 12, 716. https://doi.org/10.3390/met12050716
1 Key Laboratory of Material Physics, Ministry of Education, School of Physics and Microelectronics,
Zhengzhou University, Zhengzhou 450052, China; dyifan2022@163.com (Y.D.); liuyaoru0623@163.com (D.L.);
hl1638@foxmail.com (L.H.); liujingjing1239@163.com (J.L.)
2 School of Electrical Engineering, Zhengzhou University, Zhengzhou 450001, China
* Correspondence: zuoxiurong@zzu.edu.cn
Abstract: This paper aims to study the relationship between the microstructure and the mechanical
properties of X70 submarine pipeline steel with 40.5 mm thickness. The microstructure was examined
by using optical microscopy, scanning electron microscopy and an electron backscattered diffrac-
tometer, while the mechanical properties were examined by using a hardness test, a tensile test, a
Charpy impact test and a drop weight tear test (DWTT), respectively. The results show that the base
metal (BM) of the pipe has a low yield ratio of 0.83 and an excellent elongation of more than 45%.
The DWTT shear area of the steel plate reaches 87%, showing excellent low-temperature toughness.
The Charpy impact energy increases when the distance from the fusion line increases, and it reaches
a maximum at the BM near the heat-affected zone (HAZ) due to the small martensite-austenite (MA)
constituents and fine grains. The concentrated distribution of blocky/slender MA constituents along
the prior austenite grain boundaries of the intercritically reheated coarse-grained HAZ and the large
MA constituents are the main reasons for the deteriorating impact toughness. Delamination cracks in
the DWTT fracture surface only occurred in the midthickness of a sample with a small opening width
that spread about 2.1 mm perpendicular to the DWTT fracture surface and were finally arrested at
the acicular ferrite clusters containing a high density of high-angle boundaries.
Keywords: X70 submarine pipeline steel; heat-affected zone; microstructure; DWTT shear area;
Charpy impact energy; delamination cracks
1. Introduction
In recent decades, pipeline transportation has been widely considered the most effi-
cient and economical transportation method for crude oil and natural gas. However, the
environment of the deep sea is changeable and complex, not only with respect to the sea
water temperature at the bottom but also to sundry geological hazards, such as underwater
landslides and earthquakes, that can easily cause pipes to break and fracture. Therefore,
high-strength and toughness and highly weldable pipeline steel with a high gauge is re-
quired to ensure transportation efficiency and safety [1–4]. However, the properties of high
strength and excellent toughness in pipeline steel can be deteriorated by local brittle zones
that form during welding thermal cycles [3,5], especially in thick submarine pipelines with
high heat input.
The coarse grain heat-affected zone (CGHAZ) adjacent to the fusion line (FL) always
has the lowest fracture toughness due to the formation of unfavorable microstructures
such as large prior austenite grains, coarse bainite microstructures and martensite-austenite
(MA) constituents and precipitates [5–7].
It is well established that the presence of large and high-volume fraction MA con-
stituents in the heat-affected zone (HAZ) causes decreased toughness [6]. In addition, the
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 lack of space between blocky MA constituents exhibits a deleterious influence on
toughness because the stress concentration will be enlarged due to the transfor
induced, overlapping stress fields [8]. Di and Cai et al. [9] also suggested that thi
ness shows a considerable decrease when MA constituents are distributed at t
Metals 2022, 12, 716 boundaries and connected into chains. 2 of 12
The microstructure of a welded joint is dependent on the chemical composi
welding conditions of the pipe, including the welding heat input and pipe th
lack of space
which between
define blocky MA
the cooling constituents
rates exhibits athere
[10]. Although deleterious
haveinfluence
been many on fracture
studies on t
toughness because the stress concentration will be enlarged due to the transformation-
erties of the welded joint of pipeline steel [4,11], further research on submarine
induced, overlapping stress fields [8]. Di and Cai et al. [9] also suggested that this toughness
steel awith
shows thicknesses
considerable greater
decrease when MA than 40 mm isareneeded
constituents dueat to
distributed thethe
grainrigorous
bound- requi
regarding
aries low-temperature
and connected into chains. toughness and strength.
The microstructure of a welded
In the present study, X70joint is dependent
submarine on the chemical
pipeline steel withcomposition
a thicknessand of ove
welding conditions
has excellent of the properties
tensile pipe, including
andthedrop
welding heat input
weight tear and
testpipe thickness,
(DWTT) which feature
fracture
define the cooling rates [10]. Although there have been many studies on the properties
a the
of large heatjoint
welded input was applied
of pipeline during
steel [4,11], the research
further weldingonprocess,
submarine variations in the mic
pipeline steel
ture and mechanical properties of different regions of the welded
with thicknesses greater than 40 mm is needed due to the rigorous requirements regarding joint occurred
scribe the detailed
low-temperature mechanism
toughness of microstructural evolution and mechanical prop
and strength.
In the present study, X70 submarine
iation after welding, hardness testing, pipeline steel with
tensile a thickness
testing, of over 40 mm Charpy
low-temperature has V
excellent tensile properties and drop weight tear test (DWTT) fracture features. When a
impact testing and DWTT were carried out.
large heat input was applied during the welding process, variations in the microstructure
and mechanical properties of different regions of the welded joint occurred. To describe
2. Materials
the and Methods
detailed mechanism of microstructural evolution and mechanical property variation
after welding, hardness testing, tensile testing, low-temperature Charpy V notched impact
The material used in this study was X70 submarine pipeline steel plate wi
testing and DWTT were carried out.
mm thickness, which was obtained after thermo-mechanical control processing, f
2.by generating
Materials a pipe with outer diameter of 691 mm. The chemical composit
and Methods
mainly composed
The material used inofthis
C 0.044,
study wasMnX701.56, P 0.009,
submarine S 0.009,
pipeline steelSi 0.25,
plate withNia 40.5
+ Crmm + Cu + M
thickness, which was obtained
Nb 0.049 and Ti 0.020, wt.%. after thermo-mechanical control processing, followed by
generating a pipe with outer diameter of 691 mm. The chemical composition was mainly
Due to the thickness of the pipeline steel, a heat input of 96 kJ/cm was used t
composed of C 0.044, Mn 1.56, P 0.009, S 0.009, Si 0.25, Ni + Cr + Cu + Mo 0.475, Nb 0.049
theTiwelding
and process occurred consistently and as expected. As shown in Figu
0.020, wt.%.
welded
Due tojoint includesofthe
the thickness weld metal
the pipeline steel, zone
a heat (WM),
input of the HAZwas
96 kJ/cm and thetobase
used ensuremetal zo
the welding process occurred consistently and as expected. As shown
Under the effects of double-pass longitudinal submerged arc welding, the HAZ in Figure 1, the
welded joint includes the weld metal zone (WM), the HAZ and the base metal zone (BM).
separated into CGHAZ, the fine grain HAZ (FGHAZ), the intercritical HAZ (ICH
Under the effects of double-pass longitudinal submerged arc welding, the HAZ can be
the subcritical
separated HAZ (SCHAZ)
into CGHAZ, [3].HAZ
the fine grain Moreover,
(FGHAZ), deep
the weld deposition
intercritical was formed as
HAZ (ICHAZ)
and the subcritical HAZ (SCHAZ) [3]. Moreover, deep weld deposition was formed as a CGH
of the large heat input. Reheated CGHAZ, which consists of unaltered
CGHAZ),
result supercritically
of the large reheated
heat input. Reheated CGHAZ
CGHAZ, which(SC CGHAZ),
consists intercritically
of unaltered CGHAZ (UA reheated
CGHAZ), supercritically reheated CGHAZ (SC CGHAZ), intercritically
(IC CGHAZ) and subcritically reheated CGHAZ (S CGHAZ), could have been v reheated CGHAZ
(IC CGHAZ) and subcritically reheated CGHAZ (S CGHAZ), could have been very different
ferent from the CGHAZ due to the different second peak temperatures.
from the CGHAZ due to the different second peak temperatures.

Figure
Figure Schematic
1. 1. diagram
Schematic of welded
diagram joint. The joint.
of welded abbreviations in the figure arein
The abbreviations explained as follows:
the figure are explained
the base metal zone (BM), the coarse grain heat-affected zone (CGHAZ), the fine grain HAZ (FGHAZ),
lows: the base metal zone (BM), the coarse grain heat-affected zone (CGHAZ), the fine gra
the intercritical HAZ (ICHAZ) and the subcritical HAZ (SCHAZ), unaltered CGHAZ (UA CGHAZ),
(FGHAZ), the intercritical HAZ (ICHAZ) and the subcritical HAZ (SCHAZ), unaltered CG
supercritically reheated CGHAZ (SC CGHAZ), intercritically reheated CGHAZ (IC CGHAZ) and
(UA CGHAZ), supercritically reheated CGHAZ (SC CGHAZ), intercritically reheated CG
subcritically reheated CGHAZ (S CGHAZ).
CGHAZ) and subcritically reheated CGHAZ (S CGHAZ).
 directions, far from the HAZ. The tensile test on the BM was carried out using a tensile
testing machine (ZWICK 1600; ZwickRoell, Ulm, Germany), and the gauge size of plate
tensile specimens was 38.1 mm wide by 50 mm long by full material thickness. Round
tensile specimens with a diameter of 12.7 mm were adopted on the WM in the midthick-
Metalsness.
2022, 12,Three
716 identical specimens were tested at each position during tensile test at room 3 of 12

temperature.
Hardness test was performed on a digital hardness tester (XHD-2000TMSC; Vickers,
The tensile specimens were cut from the BM along the transverse and longitudinal
Shanghai, China), with an indenting
directions, far from theloadHAZ.of 9.8
TheN and test
tensile loading
on thetime
BM wasof 15 s. Measurements
carried out using a tensile
were made at four different positions
testing machine (ZWICKof1600; theZwickRoell,
welded joint, as shownand
Ulm, Germany), bythethe solid
gauge sizered lineten-
of plate
sile specimens was 38.1 mm wide by 50 mm long
in Figure 1. The positions of the hardness test were 2 mm away from the outside surfaceby full material thickness. Round tensile
specimens with a diameter of 12.7 mm were adopted on the WM in the midthickness. Three
and midthickness, respectively. The distance between each neighboring indentation
identical specimens were tested at each position during tensile test at room temperature.
caused by the tester wasHardness0.5 mm,test inwas
a direction
performedfrom the FL
on a digital to thetester
hardness BM (XHD-2000TMSC;
near the HAZ. Vickers,
V-notch Charpy impactChina),
Shanghai, test was
with anconducted
indenting load at −30
of 9.8°C on loading
N and a Charpy time impact test ma-
of 15 s. Measurements
chine (RKP 450; Derui, Guangdong, China) using specimens with dimensions of 10 red
were made at four different positions of the welded joint, as shown by the solid mm line× in
Figure 1. The positions of the hardness test were 2 mm away from the outside surface and
10 mm × 50 mm. Tomidthickness,
indicate the change in toughness in the direction of thickness of the
respectively. The distance between each neighboring indentation caused by
X70 steel welded joint, the specimens
the tester was 0.5 mm, in were sampled
a direction 2 mm
from the FL toaway
the BMfrom theHAZ.
near the outside weld
− ◦ C on a Charpy impact test
surface and weld root in the midthickness located in the outside weld, respectively, and
V-notch Charpy impact test was conducted at 30
machine (RKP 450; Derui, Guangdong, China) using specimens with dimensions of
two identical specimens were tested at each position. The sampling locations are shown
10 mm × 10 mm × 50 mm. To indicate the change in toughness in the direction of thickness
in Figure 2a. Four notchof thezones were
X70 steel chosen
welded joint,for
the Charpy
specimensV-notch
were sampledtesting,
2 mm including
away fromthe theWM
outside
centerline zone, FL weld zone, HAZand
surface and
weld BMrootzones. V-notch specimens
in the midthickness located in the atoutside
the FL zone
weld, were
respectively,
sampled at both 50%and WM twoandidentical
50% specimens
HAZ, whereas were tested
other at specimens
each position.were The notched
sampling locations
at 2 mmare
shown in Figure 2a. Four notch zones were chosen for Charpy V-notch testing, including
away from the FL (FL + 2 mm), 5 mm away from the FL (FL + 5 mm) and in the BM zone
the WM centerline zone, FL zone, HAZ and BM zones. V-notch specimens at the FL zone
near HAZ, in accordance with DNV-OS-F101
were sampled at both 50% WM[12]. DWTT
and 50% HAZ, was performed
whereas on the steel
other specimens were plate
notched
with dimensions of at 3052 mmmmaway × 76.2
frommm × 40.5
the FL (FL +mm.
2 mm), The5 mmtestaway
wasfromcarried
the FLout(FLat
+ 5−20
mm)°C andoninathe
BM zone near HAZ, in accordance with DNV-OS-F101
drop weight tear testing machine (JL–100000; Shengwei, Shandong, China). The DWTT [12]. DWTT was performed on the
steel plate with dimensions of 305 mm × 76.2 mm × 40.5 mm. The test was carried out at
macroscopic fracture−20 morphology
◦ C on a drop is shown
weight tearin Figure
testing 2b and
machine was cutShengwei,
(JL–100000; along the red lineChina).
Shandong, on
the specimen to observe delamination
The DWTT macroscopic cracks.
fracture Microstructural
morphology is shown analysis was2bconducted
in Figure and was cutus- along
the red line on the specimen to observe delamination
ing a scanning electron microscope (SEM; JSM 6700F; Jeol, Tokyo, Japan) and optical mi- cracks. Microstructural analysis
was conducted using a scanning electron microscope (SEM; JSM 6700F; Jeol, Tokyo, Japan)
croscope (OM; BX51M; OLYMPUS, Tokyo, Japan), and the specimens were mechanically
and optical microscope (OM; BX51M; OLYMPUS, Tokyo, Japan), and the specimens were
polished and chemically etchedpolished
mechanically for about and25 s using etched
chemically 4% Nital solution.
for about To denote
25 s using 4% Nitalthe pres-To
solution.
ence of MA constituents,denotepolished
the presence samples were etched
of MA constituents, usingsamples
polished LePera’s reagent.
were The aver-
etched using LePera’s
reagent. The average size and volume fraction of the
age size and volume fraction of the MA constituents in different regions of the HAZ were MA constituents in different regions
of the HAZ were measured by using Image-Pro Plus software (IPP; Media Cybernetics,
measured by using Image-Pro
New York, UK).
Plus software (IPP; Media Cybernetics, New York, UK).

(a) (b)
Figure 2. Macromorphology
Figure 2.of the welded joint
Macromorphology (a);
of the and DWTT
welded fracture
joint (a); and DWTTsurface (b). (b).
fracture surface

Electron backscattered diffractometry (EBSD) analysis was used for the crystal analysis
Electron backscattered diffractometry
of the delamination cracks in a(EBSD) analysis
field emission waselectron
scanning used microscope
for the crystal
(FESEM; anal-
ZEISS,
ysis of the delamination cracksGermany).
Oberkochen, in a fieldInemission scanning
this study, EBSD electron
data were acquiredmicroscope
at 20 kV with(FESEM;
a 0.2 µm step
ZEISS, Oberkochen,size. The raw data
Germany). werestudy,
In this analyzed usingdata
EBSD HKLwere
Channel 5 software
acquired at (2007
20 kVversion;
with aBuehler,
0.2
Oxford, UK) to acquire the crystallographic features.
μm step size. The raw data were analyzed using HKL Channel 5 software (2007 version;
Buehler, Oxford, UK) to acquire the crystallographic features.
Metals 2022, 12, 716 4 of 12

3. Results
3.1. Mechanical Properties
The results of the tensile testing of the studied steel are shown in Table 1. According to
the specification of DNV-OS-F101, all of the specimens tested in the present work satisfy the
requirements of X70 submarine pipeline steel. For the BM, there is no significant difference
in the tensile properties, whether in the longitudinal or transverse directions. The BM
shows a low yield ratio of 0.83 and an excellent elongation of more than 45%. For WM, the
yield strength and tensile strength are both higher than those of BM, which ensures that
fractures will not occur in the WM (Table 1).

Table 1. Tensile properties of the pipe.

Single Value
Specimen Parameter Mean Values Standard Deviation
1 2 3
Yield strength (MPa) 535 557 534 542 13.0
Tensile strength (MPa) 650 660 641 650 9.5
Base metal (T)
Yield ratio 0.82 0.84 0.83 0.83 0.010
Elongation (%) 47 48 42 46 3.21
Yield strength (MPa) 536 529 525 530 5.6
Tensile strength (MPa) 646 633 640 640 6.5
Base metal (L)
Yield ratio 0.83 0.84 0.82 0.83 0.010
Elongation (%) 46 43 45 45 1.53
Yield strength (MPa) 650 641 630 640 10.0
Tensile strength (MPa) 730 718 713 720 8.7
Weld metal (L)
Yield ratio 0.89 0.89 0.88 0.89 0.006
Elongation (%) 40 35 47 41 6.03
Note: L is longitudinal; T is transverse.

The DWTT is one of the most effective methods available to explore the fracture
properties of steel. According to the API 5L SP3 standard of the American Petroleum
Institute, the shear area of the plate’s fracture surface must attain more than 85%.
The DWTT fracture surface can be divided into four parts, as shown in Figure 2b:
(1) the initial cleavage fracture surface near the pressed notch; (2) the ductile fracture;
(3) the inverse cleavage fracture surface; (4) the hammer impact zone. The DWTT fracture
surface was tortuous (Figure 2b), showing that the main crack propagation consumed a lot
of energy [13,14]. However, when the main crack propagated to about half of the DWTT
specimen width, its propagation direction was deflected by a large angle, and the ductile
fracture mode was transformed into a brittle fracture mode in the inverse cleavage fracture.
In this study, the DWTT shear area of the steel plate was calculated according to
the method in the literature [2], which reaches 87%, showing excellent low-temperature
toughness. Delamination cracks exist in the midthickness of the plate of the DWTT fracture
surface (Figure 2b). The propagation direction of the delamination cracks is perpendicular
to the fracture surface and parallel to the rolling direction. The opening width of the
delamination cracks in this study is small, so the delamination cracks are not included in
the brittle fracture area, according to API RP 5L3.
Figure 3 shows the hardness values of the welded joint. The results indicate that the
hardness of WM is relatively higher than that of the other regions. The hardness gradually
decreases from the WM to the FGHAZ due to the welding softening that occurred during
the thermal cycle of the welding process, which is where the quasi-polygonal ferrite (QPF)
and fine polygonal ferrite (PF) occur and the second particles dissolve. It should be
mentioned that the hardness of the samples that were 2 mm away from the outside weld
surface is slightly higher than that of the midthickness region (see Figure 3a,b), which can
be attributed to the differences in cooling rates during thermal welding cycles. Welding
softening also occurs at the WM after second-pass welding has been carried out, so the
hardness of the outside weld is a bit higher than that of the inside weld (see Figure 3c). The
 hardness of the outside weld is a bit higher than that of the inside weld (see Figure 3c).
The12,hardness
Metals 2022, 716 values of the reheated CGHAZ are presented in Figure 3d. IC CGHAZ 5 of 12

shows the highest hardness, with an average value of up to 262 HV. The hardness of the
S CGHAZ far away from the weld root returns to that of CGHAZ, approximately 240 HV
hardness values of the reheated CGHAZ are presented in Figure 3d. IC CGHAZ shows the
(Figure 3d). highest hardness, with an average value of up to 262 HV. The hardness of the S CGHAZ far
away from the weld root returns to that of CGHAZ, approximately 240 HV (Figure 3d).

(a) (b)

(c) (d)
Figure 3. Hardness distribution of thedistribution
Figure 3. Hardness welded joint inwelded
of the different
jointregions. (a)regions.
in different 2 mm (a)
from outside
2 mm sur-
from outside
surface; (b) midthickness; (c) WM center;
face; (b) midthickness; (c) WM center; (d) reheated CGHAZ. (d) reheated CGHAZ.

3.2. Microstructure
3.2. Microstructure The X70 submarine pipeline steel plate in this study includes PF, QPF, acicular ferrite
(AF), granular bainite (GB), bainite ferrite (BF) and MA constituents [13,15]. The tempera-
The X70 submarine pipeline steel plate in this study includes PF, QPF, acicular ferrite
tures of Ac1 and Ac3 of the steel are 710 ◦ C and 919 ◦ C, respectively, which were predicted
(AF), granular bainite (GB),tobainite
according empiricalferrite
formulas(BF) and MA
proposed constituents
by Andrews [16]. Due[13,15]. The temper-
to the inevitable thermal
atures of Ac1 and Ac 3 of the
cycling steel
effects of are 710 °Cprocess,
the welding and 919 °C,are
there respectively, whichinwere
significant differences predicted
the grain sizes and
microstructure types of each region of the welded joint, resulting
according to empirical formulas proposed by Andrews [16]. Due to the inevitable thermal in significant differences
in mechanical properties.
cycling effects of the welding process, there are significant differences in the grain sizes
SEM photographs of the welded joint are shown in Figure 4. The microstructure of the
and microstructureCGHAZ
types of each
with region
a peak of the welded
temperature joint,
of up to 1350 ◦ C resulting
is completely in austenitized
significantdue differ-
to the
ences in mechanical properties.
influence of the welding thermal cycle, which leads to grain-coarsened bainite structures
SEM photographswith anofaverage prior austenite
the welded grain
joint are size of about
shown 55 µm,4.thereby
in Figure strongly deteriorating
The microstructure of
the impact properties.
the CGHAZ with a peak Thetemperature
FL zone mainlyof up toof1350
consists °C is completely
two distinct microstructures, austenitized due to
namely intragranular
the influence of theacicular
welding thermal
ferrite cycle,
(IAF) in WM andwhich leads
coarse BF to grain-coarsened
in CGHAZ, resulting in stressbainite struc-in
concentration
the FL, which has the lowest Charpy impact performance (Figure
tures with an average prior austenite grain size of about 55 μm, thereby strongly deterio- 4a). The microstructures
of the FGHAZ primarily consist of fine GB and PF, which present a good combination of
rating the impact properties.
both high strength and toughness (Figure 4b).
The ICHAZ, which includes fine GB and PF, as well as MA, is a partially-transformed
region with a peak temperature between Ac1 and Ac3 , where only a portion of the mi-
crostructure transforms into austenite again during heating thermal cycles, and grains of
 atures of Ac1 and Ac3 of the steel are 710 °C and 919 °C, respectively, which were predicted
according to empirical formulas proposed by Andrews [16]. Due to the inevitable thermal
cycling effects of the welding process, there are significant differences in the grain sizes
and microstructure types of each region of the welded joint, resulting in significant differ-
Metals 2022, 12, 716
ences in mechanical properties. 6 of 12

SEM photographs of the welded joint are shown in Figure 4. The microstructure of
the CGHAZ with a peak temperature of up to 1350 °C is completely austenitized due to
the untransformed region continue to coarsen and grow. As a result, the grain size distri-
the influence of the welding thermal cycle, which leads to grain-coarsened bainite struc-
bution in ICHAZ is nonuniform, and banded microstructures (GB bands) are observed in
tures with an average priorwhich
ICHAZ, austenite
would grain sizedeteriorate
further of about the
55 μm, thereby
Charpy impactstrongly deterio-
properties (Figure 4c). As
rating the impact properties.
shown in Figure 4d, the microstructure of SCHAZ primarily consists of PF and GB.

OR PEER REVIEW 6 of 12

(a) (b) (c)

(d) (e) (f)

Figure 4. SEM imagesFigure
of the welded
4. SEM joint.
images (a)welded
of the FL; (b) FGHAZ;
joint. (c)FGHAZ;
(a) FL; (b) ICHAZ; (d) SCHAZ;
(c) ICHAZ; (e) weld
(d) SCHAZ; (e) weld center
center at 2 mm away from
at 2 mmtheaway
outside
fromweld surface;
the outside weld(f)surface;
weld center
(f) weldin midthickness.
center in midthickness.

The microstructures of WM primarily include IAF, a small amount of widmanstat-

The FL zone mainly consists of two distinct microstructures, namely intragranular
ten ferrite (WF) and GB, where PF is also occasionally presented in the weld root in the
acicular ferrite (IAF)midthickness.
in WM and coarse BF in CGHAZ, resulting in stress concentration in
Ti-containing complex oxide inclusions in the WM promote the forma-
the FL, which has the lowest
tion of IAFCharpy impact
with a radial performance
distribution [17]. (Figure
Research 4a). The microstructures
indicates that the IAF is generally
of the FGHAZ primarily consist
associated withof fine
high GB and
strength PF,
and which present
toughness because of a good combination
the interlocked of
and fine-grained
structures [18,19]. However,
both high strength and toughness (Figure 4b). the Charpy impact properties would deteriorate when PF and
WF microstructures appear [5,18,20]. Therefore, the values
The ICHAZ, which includes fine GB and PF, as well as MA, is a partially-transformed of Charpy impact energy at
the weld center near the outer surface are much higher than those of the weld root in the
region with a peak temperature between Ac1 and Ac3, where only a portion of the micro-
midthickness with higher volume fractions of PF and WF (Figure 4e,f) [21].
structure transforms into austenite
Figure again
5 presents theduring heating
distribution andthermal
morphology cycles, andconstituents
of MA grains of thein different
untransformed region continue to coarsen and grow. As a result, the grain
regions. The average size and volume fraction of MA constituents in different size distribu-regions are
tion in ICHAZ is nonuniform,
given in Tableand 2. Duebanded microstructures
to the thickness (GB bands)
of the investigated steel,are
theobserved
cooling rateinand peak
ICHAZ, which would temperature
furtherare quite different
deteriorate theinCharpy
differentimpact
regions of the welded(Figure
properties joint, resulting
4c). As in different
MA volume fractions and morphologies [6,22].
shown in Figure 4d, the microstructure of SCHAZ primarily consists of PF and GB.
MA constituents in CGHAZ are slender along the lath boundaries of BF (Figure 5b),
The microstructures of WM primarily include IAF, a small amount of widmanstatten
and the maximum width and length values of MA constituents can reach 5.2 µm and
ferrite (WF) and GB,12.0
where PF is also occasionally
µm, respectively. presented
The MA constituents in the weld
in CGHAZ root in
are larger theexhibit
and mid- a higher
thickness. Ti-containing
volume fraction with elongated block shapes compared with other positions in of
complex oxide inclusions in the WM promote the formation the welded
IAF with a radial distribution
joint due to the[17]. Research
high indicatesand
peak temperature thatthethelowIAF is generally
cooling associated
rate of CGHAZ, which would
be thetoughness
with high strength and zone with the lowest of
because toughness and highest
the interlocked andhardness [6].
fine-grained structures
[18,19]. However, the Charpy impact properties would deteriorate when PFrate
In FGHAZ, the peak temperature decreases, and the cooling andincreases,
WF mi-compared
with CGHAZ, where the majority of the MA is blocky with different sizes, which were
crostructures appear [5,18,20]. Therefore, the values of Charpy impact energy at the weld
formed at the triple junction, grain boundary and the inner portions of the ferrite grains
center near the outer surface
(Figure 5c).are much higher
In ICHAZ, there isthan
morethose
residualof austenite,
the weldwhichroot in the midthick-
always concentrates on the
ness with higher volume fractions
prior austenite of PF
grain and WF (Figure
boundaries, 4e,f) into
transforming [21].MA constituents during the cooling
Figure 5 presents
stagethe
duedistribution and morphology
to carbon enrichment, as shown inofFigure
MA 5d.constituents in different
regions. The average size and volume fraction of MA constituents in different regions are
given in Table 2. Due to the thickness of the investigated steel, the cooling rate and peak
temperature are quite different in different regions of the welded joint, resulting in differ-
ent MA volume fractions and morphologies [6,22].
 ness with higher volume fractions of PF and WF (Figure 4e,f) [21].
Figure 5 presents the distribution and morphology of MA constituents in different
regions. The average size and volume fraction of MA constituents in different regions are
given in Table 2. Due to the thickness of the investigated steel, the cooling rate and peak
Metals temperature
2022, 12, 716 are quite different in different regions of the welded joint, resulting in differ- 7 of 12

ent MA volume fractions and morphologies [6,22].

Metals 2022, 12, x FOR PEER REVIEW 7 of 12

(a) (b) (c)

(d) (e)

Figure
Figure 5.5. OM
OMimages
imagesshowing
showingthe
thedistribution
distributionand
andmorphology
morphologyofofMA
MAconstituents
constituentsin
indifferent
different
regions.
regions.(a)
(a)WM;
WM;(b)
(b)CGHAZ;
CGHAZ;(c)
(c)FGHAZ;
FGHAZ;(d)(d)ICHAZ;
ICHAZ;(e)
(e)SCHAZ.
SCHAZ.

Table
Table 2.
2. Average
Average size
size and
and volume
volume fraction
fraction of
of MA
MA constituents
constituents in
in different
different regions.
regions.
Region
Region WMWM CGHAZ
CGHAZ FGHAZ
FGHAZ ICHAZ
ICHAZ
Average size (μm) 1.28 1.84 1.74 1.70
Average size (µm) 1.28 1.84 1.74 1.70
Volume fraction (%) 4.36 5.46 5.26 4.59
Volume fraction (%) 4.36 5.46 5.26 4.59

MA constituents in CGHAZ are slender along the lath boundaries of BF (Figure 5b),
and theThe volume fraction
maximum width andof MA constituents
length values of MA in CGHAZ and FGHAZ
constituents can reach could
5.2 μmreach
andabout
12.0
5.46%
μm, and 5.26%,The
respectively. respectively, which are
MA constituents apparently
in CGHAZ are higher thanexhibit
larger and that ofaICHAZ (4.59%),
higher volume
while the
fraction WM
with has the smallest
elongated amount
block shapes of MA constituents
compared at only 4.36%.
with other positions in the The initiation
welded joint
of the cleavage fracture preferentially occurs around coarse MA
due to the high peak temperature and the low cooling rate of CGHAZ, which would be particles, especially for
those spaced closely together [8,23]. It should
the zone with the lowest toughness and highest hardness [6]. be mentioned that large, hard and brittle
MA Inparticles
FGHAZ, appear in all
the peak HAZ regions,
temperature compared
decreases, withcooling
and the BM, initiating microcracks
rate increases, compared and
weakening
with CGHAZ, thewhere
toughness of the welded
the majority of thejoint.
MA is blocky with different sizes, which were
Figure 6 shows the micrographs
formed at the triple junction, grain boundary of the subzones
and theininner
reheated CGHAZ.
portions of theReheating with
ferrite grains
the peak temperature above Ac 3 produces a refined microstructure different
(Figure 5c). In ICHAZ, there is more residual austenite, which always concentrates on the from the origi-
nal CGHAZ,
prior austenitewhere
graincomplete reaustenitization
boundaries, transformingatinto a relatively low second
MA constituents peak temperature
during the cooling
of about 1000 ◦ C for a short time leads to small grain sizes in the SC CGHAZ (Figure 6a) [3].
stage due to carbon enrichment, as shown in Figure 5d.
The microstructure of S CGHAZ (Figure 6c), which can scarcely be distinguished from
The volume fraction of MA constituents in CGHAZ and FGHAZ could reach about
original CGHAZ, mainly consists of coarse GB and BF. The reason for this is that no phase
5.46% and 5.26%, respectively, which are apparently higher than that of ICHAZ (4.59%),
transformation occurs at the lower peak temperature of the secondary thermal cycle below
while the WM has the smallest amount of MA constituents at only 4.36%. The initiation
Ac1 . The IC CGHAZ is a region where CGHAZ resulting from the first pass welding was
of the cleavage fracture preferentially occurs around coarse MA particles, especially for
reheated to the intercritical temperature range between Ac1 and Ac3 , and the microstructure
those spaced closely together [8,23]. It should be mentioned that large, hard and brittle
was partially transformed into austenite, followed by transformations into MA constituents
MA particles appear in all HAZ regions, compared with BM, initiating microcracks and
during the cooling stage. The IC CGHAZ has coarse and inhomogeneous grains (Figure 6b).
weakening the toughness of the welded joint.
The MA constituents are rough and blocky in SC CGHAZ (Figure 6d), while fine,
Figure 6 shows the micrographs of the subzones in reheated CGHAZ. Reheating with
blocky MA constituents are found in S CGHAZ regions (Figure 6f). In the IC CGHAZ, the
the peak temperature above Ac3 produces a refined microstructure different from the orig-
concentrated distribution of blocky/slender MA constituents is formed along the prior
inal CGHAZ, where complete reaustenitization at a relatively low second peak tempera-
austenite grain boundaries (Figure 6e). The presence of a necklace structure in the MA
ture of aboutis1000
constituent °C for
always a short time
considered to beleads to small grain
the dominant sizes
factor in the SC CGHAZ
in determining (Figure
the toughness,
6a) [3]. The microstructure of S CGHAZ (Figure 6c), which can scarcely
which would provide an initiation site for cracks and cause cleavage fracture [6,9,10]. be distinguished
from original CGHAZ, mainly consists of coarse GB and BF. The reason for this is that no
phase transformation occurs at the lower peak temperature of the secondary thermal cycle
below Ac1. The IC CGHAZ is a region where CGHAZ resulting from the first pass welding
was reheated to the intercritical temperature range between Ac1 and Ac3, and the micro-
structure was partially transformed into austenite, followed by transformations into MA
constituents during the cooling stage. The IC CGHAZ has coarse and inhomogeneous
 Metals 2022, 12, 716 8 of 12

PEER REVIEW 8 of 12
Therefore, the IC CGHAZ may show a deteriorated toughness, which is lower than that of
(d)
the original CGHAZ. (e)
Figure 6. OM images showing the microstructure and MA constituen
(a,d) SC CGHAZ; (b,e) IC CGHAZ; (c,f) S CGHAZ.

The MA constituents are rough and blocky in SC CGHAZ

blocky MA constituents are found in S CGHAZ regions (Figure
concentrated distribution of blocky/slender MA constituents i
(a) (b) (c)
austenite grain boundaries (Figure 6e). The presence of a neck
constituent is always considered to be the dominant factor in de
which would provide an initiation site for cracks and cause c
Therefore, the IC CGHAZ may show a deteriorated toughness,
of the original CGHAZ.

(d)
4. Discussion (e) (f)
4.1.showing
Figure 6. OM images Influence
Figure 6. OM of Microstructure
theimages
microstructure
showing theand onand
Impact
MA constituents
microstructure Energy
of the reheated
MA constituents of the CGHAZ.
reheated CGHAZ.
(a,d) SC CGHAZ; (b,e)(a,d)
IC CGHAZ;
SC CGHAZ; (c,f) S IC
(b,e) CGHAZ.
CGHAZ; (c,f) S CGHAZ.
The Charpy impact energy is presented in Figure 7. The C
4. Discussion
The MA creases with increasing distance from
constituents are rough
4.1. Influence and blocky
of Microstructure in SC
on Impact CGHAZ
Energy the 6d),
(Figure FL while
and fine,reaches a ma
blocky MA constituents
that ofare
TheFLfound inimpact
is lowest
Charpy S CGHAZjustregions
energy below (Figure
is presented 6f).
50inJ.Figure In7.the
In addition,
TheICCharpy
CGHAZ,
the theenergyof the
values
impact
concentrated distribution ofwith
increases blocky/slender MA from
increasing distance constituents
the FL andisreaches
formed along the
a maximum prior
at the BM, while
the midthickness
austenite grain boundaries
that of FL(Figure
is lowest6e). are much
The presence
just below higher than
of a necklace
50 J. In addition, the
the values structurevalues
of the Charpy of
in impact
the MA thosein that a
energy
surface,
constituent is alwaysthe while
midthickness
considered toarethe
be theresults
much higher than
dominant offactor
the
the WM
values
in arethat
of those
determining opposite.
arethe
2 mm from the outside
toughness,
surface, while the results of the WM are opposite.
which would provide an initiation site for cracks and cause cleavage fracture [6,9,10].
Therefore, the IC CGHAZ may show a deteriorated toughness, which is lower than that
of the original CGHAZ.

4. Discussion
4.1. Influence of Microstructure on Impact Energy
The Charpy impact energy is presented in Figure 7. The Charpy impact energy in-
creases with increasing distance from the FL and reaches a maximum at the BM, while
that of FL is lowest just below 50 J. In addition, the values of the Charpy impact energy in
the midthickness are much higher than the values of those that are 2 mm from the outside
surface, while the results of the WM are opposite.

Figure 7. Charpy impact energy of the welded joint notched in different regions.
Figure 7. Charpy impact energy of the welded joint notched in differen

Under the impact load, microcracks form from MA constitu

MA constituent, the lower the energy needed for microcrack init
Metals 2022, 12, 716 9 of 12

Under the impact load, microcracks form from MA constituents, where the larger the
MA constituent, the lower the energy needed for microcrack initiation. These microcracks
propagate along the prior austenite grain boundaries or inside the grains, eventually
leading to the sample fracture. However, the thermal cycle temperature declines rapidly as
the distance away from the FL increases, which is accompanied by refined microstructures.
Therefore, the initiation of microcracks around MA constituents is difficult due to the small
size of the MA constituents. Likewise, because of the small grain size, crack propagation
may be more difficult and might even be arrested by these fine grains.
As presented in Figure 7, for samples that are 2 mm away from the outside weld
surface, the FL zone samples have the lowest impact energy, whose notch regions contain
the WM and CGHAZ, occupying about 50% each. The lowest impact energy of the FL
zone samples can be attributed to coarse prior austenite grains and coarse lath bainite with
large MA in CGHAZ, accompanied by a high stress concentration in FL, which not only
provides a site for crack initiation, but also an easy path for crack propagation. However,
for samples in the midthickness zone, FL zone samples also show the lowest impact energy
in the notch regions containing 50% WM, 50% CGHAZ and reheated CGHAZ, in which
low-toughness IC CGHAZ are contained.
However, the FL + 2 mm samples contain almost the whole HAZ and small parts of
WM. If the crack initiates in low-toughness regions of CGHAZ or FL, it would be arrested
by the high-toughness regions of FGHAZ or ICHAZ, which are dominated by finer ferrite
and bainite, resulting in increased impact toughness.
For the notch regions of FL + 5 mm samples, only about 50% of SCHAZ are contained.
Cracks tend to preferentially occur in the CGHAZ, but both the initiation and propagation
of microcracks in SCHAZ are relatively difficult, so the total impact energy is increased
further compared with the FL + 2 mm samples.
The reason for the highest absorbed energy in BM (SCHAZ) is that the microstructure
of this notch region is PF and GB entirely, which proves to be an excellent combination of
strength and toughness. Therefore, the increased Charpy impact energy from the FL zone
to the BM zone can be attributed to the combined effects of the microstructures obtained in
each notch region.
For samples from the weld root in the midthickness containing outside and inside
welds, the notch regions of FL + 2 mm and FL + 5 mm contain more SCHAZ with high
impact toughness compared with that of the samples that are 2 mm away from the outside
weld surface, resulting in higher impact toughness in the midthickness.

4.2. EBSD Analysis of Delamination Cracks

In the present study, delamination cracks only occurred in the midthickness of the
steel plate with a small opening width, which spread about 2.1 mm perpendicular to the
DWTT fracture surface. The microstructure near the tip of the delamination crack is shown
in Figure 8. The nonequiaxed, fine-grained AFs with the variously sized grains randomly
distributed in different orientations are found near the crack tip [24]. The delamination
crack extends along the grain boundaries of GB with the AF clusters nearby, which is finally
arrested at the AF clusters.
As reported in previous studies [14,25–27], the preferred plane of crack propagation
is the {001} plane for the body-centered cubic (bcc) structured steels. Figure 9 shows the
schematic diagram of the EBSD sampling location and EBSD analysis diagrams around
the tip of the delamination crack. Low-angle (LAGBs, 2◦ –15◦ ) and high-angle boundaries
(HAGBs, >15◦ ) are represented by green and red lines, respectively (Figure 9b). HAGBs can
effectively prevent crack propagation by consuming more energy [17]. The delamination
crack tip is surrounded by the HAGBs. A careful analysis of the color-coded inverse pole
figure (Figure 9c) shows that there are a large number of HAGBs in AFs with fine effective
grain size, which impede crack propagation and even arrest the crack, while the GB matrix
is composed of fine ferrite grains separated by LAGBs [28]. AF and bainite belong to
different Bain groups, and AFs increase the number of HAGBs [17].
 DWTT fracture surface. The microstructure near the tip of the delamina
shown in Figure 8. The nonequiaxed, fine-grained AFs with the variously
randomly distributed in different orientations are found near the crack tip
Metals 2022, 12, 716 lamination crack extends along the grain boundaries of GB with10the
of 12 AF clu
which is finally arrested at the AF clusters.
ER REVIEW 10 of 12

schematic diagram of the EBSD sampling location and EBSD analysis diagrams around
the tip of the delamination crack. Low-angle (LAGBs, 2°–15°) and high-angle boundaries
(HAGBs, >15°) are represented by green and red lines, respectively (Figure 9b). HAGBs
can effectively prevent crack propagation by consuming more energy [17]. The delamina-
tion crack tip is surrounded by the HAGBs. A careful analysis of the color-coded inverse
pole figure (Figure 9c) shows that there are a large number of HAGBs in AFs with fine
effective grain size, which impede crack (a) propagation and even arrest the(b) crack, while the
GB matrix is composed of 8.fine ferrite grains separated by LAGBs [28]. AF and bainite
Figure
Figure 8.Microstructure near the
Microstructure tip
near of thetip
the delamination crack. (a)
of the delamination Low-magnification SEM micro-
crack. (a) Low-magnificatio
belong to different Bain groups,
graph; and AFs increase
(b) high-magnification the
SEM micrograph.
graph; (b) high-magnification SEM micrograph. number of HAGBs [17].

As reported in previous studies [14,25–27], the preferred plane of crack

is the {001} plane for the body-centered cubic (bcc) structured steels. Figure

(a) (b) (c) (d) (e)

Figure 9. Schematic diagram
Figureof9. EBSD sampling
Schematic diagram location (a) andlocation
of EBSD sampling EBSD(a)analysis
and EBSDdiagrams with {001}
analysis diagrams with {001}
plane around the tip of delamination
plane around thecrack; (b) image crack;
tip of delamination quality plus grain
(b) image qualityboundary misorientation
plus grain boundary misorientation
map; (c) color-coded inverse pole figure plus grain boundary misorientation
map; (c) color-coded inverse pole figure plus grain boundary misorientation map (black line, >15°); map (black line, >15◦ );
(d) kernel average misorientation map; (e) distribution map of deformed grains, recrystallized grains
(d) kernel average misorientation map; (e) distribution map of deformed grains, recrystallized
and substructures.
grains and substructures.
A kernel average misorientation map (Figure 9d) shows that severe stress concentra-
A kernel average tion seems to appear
misorientation around
map the delamination
(Figure 9d) shows crack,
thatespecially at the turning
severe stress point of the
concentra-
delamination crack. In particular, there is more stress in AFs. Figure 9e shows the distribu-
tion seems to appear around the delamination crack, especially at the turning point of the
tion map of deformed grains, recrystallized grains and substructures, which are represented
delamination crack. Ininparticular,
red, blue andthere
yellowislines,
more stress inItAFs.
respectively. can beFigure
seen that9e shows
there the substructures
are more distri-
bution map of deformed and grains,
deformed recrystallized
grains around the grains and substructures,
delamination which arecontain
crack. The substructures repre-a high
sented in red, blue anddensity
yellowof dislocations, while the deformed
lines, respectively. grains
It can be show
seen a high
that therelevel of more
are strain. sub-
structures and deformed grains around the delamination crack. The substructures contain
a high density of dislocations, while the deformed grains show a high level of strain.

5. Conclusions
1. The BM of the pipe shows a low yield ratio of 0.83 and an excellent elongation of
more than 45%. The DWTT shear area of the steel plate reaches 87%, showing excel-
Metals 2022, 12, 716 11 of 12

5. Conclusions
1. The BM of the pipe shows a low yield ratio of 0.83 and an excellent elongation of more
than 45%. The DWTT shear area of the steel plate reaches 87%, showing excellent
low-temperature toughness. IC CGHAZ shows the highest hardness within the
reheated CGHAZ, with an average value of up to 262 HV. However, the concentrated
blocky/slender MA constituents along the prior austenite grain boundaries of IC
CGHAZ show a deteriorated impact toughness.
2. Under impact load, microcracks form from MA constituents. The Charpy impact
energy increases as the distance away from the FL increases and reaches a maximum
at the BM near HAZ due to the small size of MA constituents and grain, while that
of the FL zone is the lowest just below 50 J because of two distinct microstructures,
namely IAF in WM and coarse BF in CGHAZ, resulting in stress concentration in FL.
3. Delamination cracks only occurred in the midthickness of a steel plate with a small
opening width, which spread about 2.1 mm perpendicular to the DWTT fracture
surface. The delamination cracks were finally arrested at the AF clusters containing
a high density of HAGBs. Severe stress concentration appears around the delam-
ination cracks, and there are more substructures and deformed grains around the
delamination cracks.

Author Contributions: Conceptualization, X.Z., Y.D., D.L., L.H. and J.L.; Methodology, X.Z., Y.D.,
D.L., L.H. and J.L.; Software and Experimental Validation, Y.D., D.L. and L.H.; Formal Analysis
and Investigation, X.Z., Y.D., D.L., L.H. and J.L.; Resources, X.Z.; Data Curation, X.Z. and Y.D.;
Writing—Original Draft Preparation, Y.D.; Writing—Review and Editing, X.Z.; Supervision, X.Z.;
Project Administration, X.Z.; Funding Acquisition, X.Z. All authors have read and agreed to the
published version of the manuscript.
Funding: This research was funded by Henan Provincial Science and Technology Cooperation Project
China (grant no. 182106000016) and the Key R & D and Promotion Special Project of Henan Province
(no. 212102210444).
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Data are contained within the article.
Acknowledgments: The authors gratefully acknowledge the financial support provided by Nanjing
Iron & Steel Co., Ltd.
Conflicts of Interest: The authors declare no conflict of interest.

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