metals

Article
Effects of Small Ni Addition on the Microstructure
and Toughness of Coarse-Grained Heat-Affected
Zone of High-Strength Low-Alloy Steel
Gang Huang 1 , Xiangliang Wan 1, *, Kaiming Wu 1, *, Huazhong Zhao 2
and Raja Devesh Kumarmr Misra 3
1 The State Key Laboratory of Refractories and Metallurgy, Hubei Province Key Laboratory of Systems Science
in Metallurgical Process, International Research Institute for Steel Technology, Wuhan University of Science
and Technology, Wuhan 430081, China; huanggang@wust.edu.cn
2 Wuhan Anchor Welding consumables Co., Ltd., Wuhan 430081, China; hzzhao@163.com
3 Department of Metallurgical and Materials Engineering, University of Texas at El Paso,
El Paso, TX 79968, USA; dmisra2@utep.edu
* Correspondence: wanxiangliang@wust.edu.cn (X.W.); wukaiming@wust.edu.cn (K.W.);
Tel.: +86-27-68862772 (X.W. & K.W.); Fax: +86-27-68862606 (X.W. & K.W.)




Received: 14 August 2018; Accepted: 11 September 2018; Published: 13 September 2018


Abstract: The objective of the present study is to investigate the effects of nickel (Ni) on the
microstructure and impact toughness of coarse-grained heat-affected zone (CGHAZ) of high-strength
low-alloy steel. It was observed that the microstructure of CGHAZ predominantly consisted of
bainite and a small proportion of martensite-austenite (M-A) constituents and acicular ferrite
(AF). With increased Ni content, the percentage of M-A constituent decreased and AF increased;
consequently, the impact toughness of CGHAZ increased. The study revealed that a small addition of
nickel significantly affected the formation of M-A constituents and AF; however, no obvious influence
was observed on the bainitic microstructure of high-strength low-alloy steel.

Keywords: high-strength low-alloy steel; Ni; coarse-grained heat-affected zone; microstructure;

impact toughness

1. Introduction
High-strength low alloy steels (HSLA) are widely used in applications requiring welding because
of their high toughness, high strength, cold formability, and good weldability. In recent years, several
studies have been carried out using high heat input welding to reduce cost and improve welding
efficiency. However, the high heat input welding thermal cycle results in a coarse-grained heat-affected
zone (CGHAZ), as well as degradation in the toughness of steels [1]. Therefore, improvement in the
toughness of HAZ is an important aspect when high heat input is used.
The toughness of HAZ is strongly influenced by the microstructural features of steels [2].
Coarse bainite in the HAZ of HSLA steel contains parallel bainitic ferrite and martensite-austenite
(M-A) constituents [3]. Thus, it is difficult to obtain superior HAZ toughness because of the hard
M-A constituents and the low-angle grain boundary between parallel bainitic ferrite, which facilitates
nucleation and propagation of cracks. Previous studies have revealed that the microstructural features
of HAZ greatly depend on the alloying elements in HSLA steels [4]. Deoxidizing alloying elements,
such as titanium and zirconium, provide favorable nucleation sites at grain boundaries for AF during
the welding thermal cycle [5]. Some studies have also proposed that niobium, aluminum, and silicon
can modify the morphology of M-A constituents [6–8].

Metals 2018, 8, 718; doi:10.3390/met8090718 www.mdpi.com/journal/metals

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Nickel (Ni)
Nickel (Ni) is
is generally
generally present
present asas aa solid
solid solution
solution strengthening element in
strengthening element in ferrite
ferrite and
and increases
increases
the strength of steel by solid solution strengthening. Ni also has a strong influence on the
the strength of steel by solid solution strengthening. Ni also has a strong influence on the toughness
toughness of
of weld
weld metals.
metals. Previous
Previous studies
studies havehave indicated
indicated that
that withwith increasing
increasing Ni Ni content,
content, thethe microstructure
microstructure of
of the weld metal can be refined [9]. However, when Ni content exceeds a certain value, the toughness
the weld metal can be refined [9]. However, when Ni content exceeds a certain value, the toughness
of the
of the weld
weld metal
metal isis reduced
reduced because
because of of the
the formation
formation of of martensite
martensite [10].
[10]. Superior
Superior low-temperature
low-temperature
toughness in
toughness in high-Ni
high-Nisteelsteelcan
canbebeobtained
obtaineddue duetotothe
theretained
retained austenite,
austenite, which
which absorbs
absorbs high
high energy
energy by
by transformation of the retained austenite to strain-induced martensite during Charpy impact
transformation of the retained austenite to strain-induced martensite during Charpy impact testing [11].
testing [11].
However, an However,
understanding an understanding
of the effect of Ni of the effect of Ni ontransformation
on microstructural microstructural and transformation
impact toughnessand
impact toughness of CGHAZ of HSLA steels is relatively limited and requires in-depth study.
of CGHAZ of HSLA steels is relatively limited and requires in-depth study.
In the
In the present
present study,
study, the
the effect
effect of
of NiNi on
on microstructural
microstructural transformation
transformation during
during thethe welding
welding
thermal cycles
thermal cycles ofof HSLA
HSLA steels
steels was
was studied,
studied, and and the
the underlying
underlying toughening
toughening mechanism
mechanism of of CGHAZ
CGHAZ
was also
was also explored.
explored.

2. Experimental Procedure
2. Experimental Procedure
Three
Three steel
steel samples,
samples, Ni-free,
Ni-free, 0.23% Ni, and
0.23% Ni, and 0.43%
0.43% Ni
Ni steel, were prepared
steel, were prepared inin aa 10
10 kg
kg vacuum
vacuum
melt induction furnace (Jinzhou North Electric Furnace Factory, Jinzhou, Liaoning,
melt induction furnace (Jinzhou North Electric Furnace Factory, Jinzhou, Liaoning, China) (Table China) (Table 1).
1).
◦
The
The cylindrical
cylindrical ingots,
ingots, 120120 mm
mm inin diameter
diameterandand100
100mmmmin inlength,
length,were
werereheated 1250±± 20
reheatedtoto1250 20 °CC and
and
forged into rectangular billets with cross-sections 30 mm × 30 mm. The samples were
forged into rectangular billets with cross-sections 30 mm × 30 mm. The samples were then machined then machined
into
into dimensions
dimensions of of 11 mm ×
11 mm × 11 mm ×
11 mm 100 mm.
× 100 mm. The
The simulation
simulation ofof CGHAZ
CGHAZ was was carried
carried out
out using
using aa
Gleeble
Gleeble 3800
3800 (Dynamic
(Dynamic Systems
Systems Inc.,
Inc., Austin,
Austin, TX,
TX, USA).
USA). A A schematic
schematic diagram
diagram ofof simulated
simulated thermal
thermal
cycles
cycles is presented in Figure 1.The peak temperature, heating rate, and holding time for
is presented in Figure 1.The peak temperature, heating rate, and holding time for thermal
thermal cycle
cycle
simulation were 1350 ◦ C, 300 ◦ C/s, and 3 s, respectively. The cooling times from 800 ◦ C to 500 ◦ C (t )
simulation were 1350 °C, 300 °C/s, and 3 s, respectively. The cooling times from 800 °C to 500 °C (t8/5 8/5)
were
were 10.6
10.6 ss and
and 52.8
52.8 s,
s, respectively,
respectively,which
whichwere
wereapproximately
approximatelyequivalent
equivalenttotoheat
heatinputs
inputsofof20
20kJ/cm
kJ/cm
and 100 kJ/cm, respectively
and 100 kJ/cm, respectively [12,13].[12,13].

Table 1. The chemical composition of the investigated steels (wt.%).

Table 1. The chemical composition of the investigated steels (wt.%).
Sample
Sample CC SiSi Mn
Mn Nb
Nb Ni
Ni Ti
Ti Mo
Mo Al
Al Fe
Fe
Ni-free
Ni-free 0.054
0.054 0.19
0.19 1.56
1.56 0.038
0.038 -- 0.012
0.012 0.020
0.020 0.022
0.022 Bal.
Bal.
0.23%
0.23%NiNi 0.056
0.056 0.20
0.20 1.58
1.58 0.036
0.036 0.23
0.23 0.015
0.015 0.019
0.019 0.025
0.025 Bal.
Bal.
0.43% Ni
0.43% Ni 0.052
0.052 0.22
0.22 1.55
1.55 0.037
0.037 0.43
0.43 0.014
0.014 0.018
0.018 0.024
0.024 Bal.
Bal.

Figure 1.
Figure 1. Schematic
Schematic illustration of simulated
illustration of simulated thermal
thermal cycles
cycles of
of the
the CGHAZ.
CGHAZ.

After the simulation, standard Charpy v-notch specimens of dimensions 10 mm × 10 mm × 55 mm

were machined for Charpy impact test at −20 ◦ C. The microstructure and fracture surface of the
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Metals 2018, 8, 718 3 of 12
After the simulation, standard Charpy v-notch specimens of dimensions 10 mm × 10 mm × 55
mm were machined for Charpy impact test at −20 °C. The microstructure and fracture surface of the
samples werestudied
samples were studiedbyby optical
optical microscope
microscope (OM,(OM, Olympus
Olympus Corporation,
Corporation, Tokyo, and
Tokyo, Japan.) Japan.) and
scanning
scanning electron microscope (SEM, FEI, Boston, MA, USA). The crystallographic grain size and
electron microscope (SEM, FEI, Boston, MA, USA). The crystallographic grain size and the the
grain
grain boundary misorientation were analyzed by electron backscattered diffraction (EBSD, EDAX,
boundary misorientation were analyzed by electron backscattered diffraction (EBSD, EDAX, New
New
York, York,
NJ, USA)NJ, technique.
USA) technique.
The M-A Theconstituents
M-A constituents
and AF and AFingrains
grains in the
the digital digital
images of images
simulatedof
simulated CGHAZ were selected and painted black using Adobe Photoshop (version 6.0, CA,
CGHAZ were selected and painted black using Adobe Photoshop (version 6.0, San, Jose, San, USA)
Jose,
CA, USA)
(Figure 2). (Figure 2). The
The length, length,
width, width,
density, anddensity, and area of
area percentage percentage of M-A constituents
M-A constituents and AF grains andwere
AF
grains were estimated using Image-Pro Plus (version 6.0, MEDIA, Rockville, MD, USA). Thirty digital
estimated using Image-Pro Plus (version 6.0, MEDIA, Rockville, MD, USA). Thirty digital images were
images
analyzedwere analyzed
to obtain to obtainvalue
an average an average value parameters
of the above of the above[12,13].
parameters [12,13].

Figure
Figure 2.
2.(a)
(a)Optical
Opticalandand(c)
(c)SEM
SEMimages
imagesshowing
showingrepresentative
representativeacicular
acicularferrite
ferriteand
andM-A
M-Aconstituents,
constituents,
respectively, inthe
respectively, in thesimulated
simulatedCGHAZ
CGHAZ of of Ni-free
Ni-free steel
steel withwith
100 100 kJ/cm
kJ/cm heatheat
inputinput welding
welding thermal
thermal cycle.
cycle. (b,d)
(b,d) are are processed
processed imagesimages ofrespectively,
of (a,c), (a,c), respectively, using Adobe
using Adobe Photoshop.
Photoshop.

3.
3. Results
Results

3.1. Microstructural Characteristics of Simulated CGHAZ

3.1.Microstructural Characteristics of Simulated CGHAZ
Figure 3 shows the optical micrographs of simulated CGHAZ for three steel samples. It was
Figure 3 shows the optical micrographs of simulated CGHAZ for three steel samples. It was
observed that the prior austenite grains became coarse in all the samples. The microstructure of all
observed that the prior austenite grains became coarse in all the samples. The microstructure of all
the samples predominantly consisted of bainite and a small percentage of AF and M-A constituents.
the samples predominantly consisted of bainite and a small percentage of AF and M-A constituents.
The AF grains were scattered among prior austenite grains, and some of them were also associated
The AF grains were scattered among prior austenite grains, and some of them were also associated
with inclusions. The bainitic ferrite sheaves nucleated at the grain boundaries and grew into the
with inclusions. The bainitic ferrite sheaves nucleated at the grain boundaries and grew into the
interior of the grain. Furthermore, the M-A constituents were observed in bainite packets, as well as
interior of the grain. Furthermore, the M-A constituents were observed in bainite packets, as well as
between the boundaries of bainite packets.
between the boundaries of bainite packets.
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Figure
Figure3. 3.
Optical micrographs
Optical micrographsof of
simulated
simulated CGHAZ
CGHAZ in in
specimens
specimens(a,b) Ni-free,
(a,b) (c,d)
Ni-free, 0.23%
(c,d) Ni,Ni,
0.23% andand
(e,f) 0.43% Ni,with heat input of (a,c,e) 20 kJ/cm, and (b,d,f) 100 kJ/cm, respectively.
(e,f) 0.43% Ni, with heat input of (a,c,e) 20 kJ/cm, and (b,d,f) 100 kJ/cm, respectively.

3.2. Quantitative
3.2. Analysis
Quantitative of Microstructure
Analysis of of
of Microstructure Simulated CGHAZ
Simulated CGHAZ

Prior austenite
Prior austenitegrain size
grain is crucial
size forfor
is crucial microstructural
microstructuralevolution
evolution [14]. The
[14]. Thesize of of
size prior austenite
prior austenite
grains
grainswaswasmeasured
measured bybyaveraging
averaging the
thelong
longand
andshort
shortaxes
axesofofthe
thegrains.
grains.TheThe mean
mean equivalent
equivalent
diameters
diameters and
andstandard
standard deviation
deviation of of
prior austenite
prior austenitegrains (taken
grains from
(taken fromabout
about2020optical
opticalmicrographs
micrographs
at at
500×
500magnification)
× magnification) areare
presented
presented in Figure 4a.4a.
in Figure The equivalent
The equivalentdiameters
diameters of of
prior austenite
prior austenitegrains
grains
were
wereininthe
therange
rangeofof 55–60 μm at
55–60 µm at20
20kJ/cm
kJ/cmheat
heatinput
inputwelding,
welding, and
and increased
increased to 70–80
to 70–80 μm100
µm for forkJ/cm.
100
kJ/cm. However,
However, no significant
no significant changechange was noticed
was noticed with with increased
increased Ni content
Ni content (Figure
(Figure 4a). 4a).
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Figure 4. (a) Prior austenite grain size and (b) mean length, (c) width, and (d) area percentage of
Figure 4.
Figure 4. (a)
(a) Prior
Prior austenite
austenitegrain
grainsize
sizeandand(b)
(b)mean
mean length, (c) (c)
length, width, andand
width, (d) (d)
areaarea
percentage of of
percentage
acicular ferrite in samples subjected to different heat inputs.
acicular ferrite
acicular ferrite in
in samples
samples subjected
subjectedtotodifferent
differentheat
heatinputs.
inputs.

AFAFis one
AF isis one
oneof of
the most
of the
the most
most important
important
important constituents
constituents
constituents for
for improving
forimproving
improving the
thethetoughness
toughness
toughness of CGHAZ
of CGHAZ
of CGHAZ ofofHSLA
HSLA
of HSLA
steels [3].[3].
steels
steels TheThe
[3]. mean
The meanlength,
length,
length,width,
width,
width, and and area
and areapercentage
areapercentage
percentage of
ofAFAFAF
of was
waswasmeasured
measured
measured (Figure
(Figure 4b–d).
4b–d).
(Figure TheThe
The
4b–d). mean
mean mean
length and width of AF increased with increased Ni content (Figure
length and width AF increased with increased Ni content (Figure 4b,c). The area percentage of AF AF
length and width of AF increased with increased Ni content (Figure4b,c). The
4b,c). area
The percentage
area percentageof AF
of
also increased
also
also increased
increased with increased
with
with increased
increased NiNicontent
Ni content
content and
and
andheat
heat
heatinput
input
input (Figure
(Figure
(Figure4d).
4d).
4d).
Figure
Figure
Figure 5 shows
55 shows
shows thetheSEM
the SEM
SEMimages
images
images ofofof
block-like
block-like
block-like and
and
and film-like
film-like
film-likeM-A
M-AM-A constituents
constituents
constituents inthe
in thethe
in simulated
simulated
simulated
CGHAZ.
CGHAZ. It is
It noted
is noted that the
that thesize,
size, density,
density, and
and area
area percentage
percentage
CGHAZ. It is noted that the size, density, and area percentage of M-A constituents varied of
of M-A constituents
constituents varied
varied with
with with
increased
increased
increased Ni Ni content
Ni contentandand
content andheatheat
input
heat input (Figure
input (Figure 6). The
(Figure6). 6).mean
The mean
The meanlengthlength
length of M-Aofconstituents
of M-A constituents decreased
decreased
M-A constituents with
with
decreased
increased
increased
with Ni Ni
increased content
content
Ni content (Figure
(Figure 6a);however,
6a);
(Figure however,
6a); thedensity
the
however, density
the density of M-A
of M-A constituents
constituents
of M-A constituentsdid not
did did change
notnot
change with
changewith
with
increased
increased Ni Ni content
content (Figure
(Figure 6b).
6b). It It
waswas observed
observed that
that the
the area
area percentage
percentage
increased Ni content (Figure 6b). It was observed that the area percentage of M-A constituents also of
of M-A
M-A constituents
constituents also
also
decreased
decreased
decreased with with
with increased
increased
increased Ni Ni
Ni content(Figure
content
content (Figure6c).
(Figure 6c).Previous
6c). Previousstudies
Previous studiesreported
studies reportedthat
reported that M-A
thatM-A
M-A constituents
constituents
constituents with
withwith
large large
large length
length length
(>2(>2 (>2
µmμm μm
and and and small
small
small length/width
length/width
length/width ratio
ratio
ratio (<4)
(<4)were
(<4) were regarded
wereregarded as
regardedasasblock block
blockM-AM-A constituents,
M-Aconstituents,
constituents, and
and and
werewere detrimental
detrimental to to impact
impact toughness[15].
toughness [15].ItItisisevident
evidentfrom from Figure
Figure 6d 6d that
that the
the area
area percentage
percentage
were detrimental to impact toughness [15]. It is evident from Figure 6d that the area percentage of
of block M-A
of block constituents decreased withincreased
increasedNi Nicontent.
content.
block M-A
M-A constituents
constituents decreased
decreased with with increased Ni content.

Figure 5. Cont.
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Figure
Figure
Figure 5.5. SEM
5. SEM SEM images
images
images of the
of the
of the simulated
simulated
simulated CGHAZ
CGHAZ
CGHAZ in (a,b)
in (a,b)
in (a,b) Ni-free,
Ni-free, (c,d)
Ni-free, (c,d)
0.23%
(c,d) 0.23% Ni,
Ni,Ni,
0.23% and
andand (e,f)
(e,f) 0.43%
(e,f) 0.43% Ni
Ni Ni
0.43%
steels
steels
steels subjected
subjected
subjected tothe
to the
to the
heatheat
input
heat input of(a,c,e)
of of
input (a,c,e)
(a,c,e) 20kJ/cm
20 20 kJ/cm
kJ/cm and
andand (b,d,f)
(b,d,f) 100
100100
(b,d,f) kJ/cm.
kJ/cm.
kJ/cm.

Figure
Figure
Figure 6.6.Effect
Effect
6. Effect ofnickel
of of nickel
nickel content
content
content andand
and simulated
simulated
simulated heat
heat
heat input
input
input on
on (a)
on (a)
(a) meanmean
mean length,
length,
length, (b) (b) density,
(b)density,
density,and
and and
(c) (c)
area
(c)
area percentage
percentage of M-A of M-A constituent,
constituent, and
and (d) (d)
area area percentage
percentage of
of block block
M-A inM-A
the in
area percentage of M-A constituent, and (d) area percentage of block M-A in the CGHAZ. the
CGHAZ.CGHAZ.
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3.3.
3.3. EBSD
EBSD Analysis
Analysis andand Grain
Grain Size
Size Determination
Determination of of Simulated
Simulated CGHAZ
CGHAZ
Figure
Figure 7 presents
7 presents thethe EBSD
EBSD analysis
analysis ofof simulated
simulated CGHAZ
CGHAZ forfor 100
100 kJ/cm
kJ/cm heat
heat input
input welding.
welding.
Figure 7a–c is the corresponding EBSD orientation image maps of Ni-free, 0.23% Ni, and 0.43% NiNi
Figure 7a–c is the corresponding EBSD orientation image maps of Ni-free, 0.23% Ni, and 0.43%
steel,
steel, respectively.
respectively. Different
Different bainite
bainite packets
packets areare represented
represented byby different
different colors
colors andand characterized
characterized byby
high-angle grain boundaries between the packets with large misorientations (50 ◦ –60◦ ). The bainitic
high-angle grain boundaries between the packets with large misorientations (50°–60°). The bainitic
ferrite
ferrite laths/plates
laths/plates (for(for low-angle
low-angle grain
grain boundaries)
boundaries) in in
thethe same
same bainite
bainite packet
packet areare represented
represented byby
similar
similar color.
color. However,
However, it was
it was observed
observed that
that AFAF grains
grains grew
grew in in
thethe interior
interior of of prior
prior austenite
austenite grains
grains
and had different orientations with the neighboring ferrite
and had different orientations with the neighboring ferrite plates. plates.

Figure
Figure7. Orientation maps
7. Orientation of of
maps bccbcc
phase of of
phase steel samples.
steel samples.(a) (a)
Ni-free, (b)(b)
Ni-free, 0.23% Ni,Ni,
0.23% and (c) (c)
and 0.43% Ni;Ni;
0.43%
and (d)(d)
and orientation color
orientation key.
color The
key. Thesimulated heat
simulated input
heat forfor
input allall
samples
samplesis is
100 kJ/cm.
100 kJ/cm.

Figure
Figure 8a,8a,
billustrates
billustratesthethe
distribution
distribution of of
grain boundary
grain boundary misorientation
misorientation angles
anglesbetween
between adjacent
adjacent
grains. TheThe
grains. frequency
frequency of high-angle
of high-angle grain boundaries
grain (45°–62°)
boundaries (45◦ –62for◦ )Ni-free steel steel
for Ni-free was smaller than for
was smaller than
0.23% Ni and
for 0.23% Ni 0.43% Ni steels
and 0.43% (Figure
Ni steels 8b). 8b).
(Figure In the present
In the study,
present study,thethe
high-angle
high-angle grain
grainboundary
boundary
threshold
threshold waswasestimated
estimated at at
15°;15hence, grain boundaries with a misorientation larger than 15° were
◦ ; hence, grain boundaries with a misorientation larger than 15◦ were

regarded
regarded asas thethe
boundary
boundary of of
twotwo grains.
grains.Grains
Grainswere
were assumed
assumed to to
bebespherical
spherical to to
facilitate grain
facilitate size
grain size
measurement.
measurement. Figure
Figure 8c 8c
displays
displays thethe
statistical distribution
statistical distribution of of
crystallographic
crystallographic grain
grainsize. The
size. mean
The mean
crystallographic
crystallographic grain
grainsizes in in
sizes CGHAZ
CGHAZ of of
Ni-free, 0.23%
Ni-free, 0.23%Ni,Ni,
andand0.43% NiNi
0.43% steels were
steels werecalculated
calculatedas as
9.49.4
μm,µm,4.94.9μm,µm,andand4.44.4
μm, respectively
µm, respectively (Figure
(Figure8d), and
8d), these
and thesevalues
values were
were significantly
significantly smaller than
smaller than
those
thoseforforthe
theprior
prioraustenite
austenitegrains
grains (73 μm, 78
(73 µm, 78µm,
μm,andand8080µmμm forfor Ni-free,
Ni-free, 0.23%
0.23% Ni,Ni,
andand 0.43%
0.43% Ni
Ni steels,
steels, respectively),
respectively), implying
implying grain grain refinement
refinement in Ni-containing
in Ni-containing steels. Thesteels. The percentages
percentages of grain
of grain refinement
refinement in prior austenite grains for 0.23% Ni, 0.43% Ni, and Ni-free steels were ~94% (15.9 times
finer), ~95% (18.6 times finer), and ~87% (7.7 times finer), respectively.
 Metals 2018, 8, 718 8 of 12

in prior austenite grains for 0.23% Ni, 0.43% Ni, and Ni-free steels were ~94% (15.9 times finer), ~95%
Metals
(18.6
Metals 8, x8,FOR
2018,
times
2018, x FOR
finer), PEER REVIEW
andREVIEW
PEER
~87% (7.7 times finer), respectively. 8 of
8 of 12 12

Figure8.
Figure
Figure 8.8.Statistical
Statistical
Statistical distribution
distribution
distribution of ofmisorientation
of (a,b) (a,b)misorientation
(a,b) misorientation between
betweenbetween
adjacent adjacent
adjacent
grains grains
grains
and (c) andand(c)(c)
crystallographic
crystallographic
crystallographic
grain size; and graingrain size; and (d) mean
size;crystallographic
(d) mean crystallographic
and (d) mean crystallographic grain size
grain size
grain size of simulated of simulated CGHAZ.
of simulated CGHAZ.
CGHAZ.

3.4.
3.4.
3.4. Impact
Impact
Impact Toughness
Toughness
Toughness in
inin the
the
the Simulated
Simulated
Simulated CGHAZ
CGHAZ
CGHAZ
TheCharpy
The
The Charpyv-notch
Charpy v-notchimpact
v-notch impacttoughness
impact toughnessofof
toughness ofCGHAZ
CGHAZforfor
CGHAZ forsamples
sampleswith
samples withvarying
with varyingheat
varying heatinputs
heat inputsis is
inputs is
presented
presented in Figure
presentedininFigure 9. It
Figure9.9.It It
was was
was observed
observed
observed that
that
that the
the
the average
average
average absorbed
absorbed
absorbed energy
energy
energy increased
increased
increased with
with
with increased
increased
increased Ni
NiNi
content
content for
for both
both heat
heat input
input welding
welding thermal
thermal cycles
cycles (20
(20 kJ/cm
kJ/cm and
and 100
100 kJ/cm).
kJ/cm).
content for both heat input welding thermal cycles (20 kJ/cm and 100 kJ/cm). The average absorbed The
The average
average absorbed
absorbed
energy
energy
energy for
for
for thethe
the 20
2020 kJ/cm
kJ/cm
kJ/cm thermal
thermal
thermal cycle
cycle
cycle increased
increased
increased gradually
gradually
gradually from
from
from 9494
94 JJ to
J to to 252
252
252 JJ and
J and and from
from
from 297
297
297 JJ for
J for for 0.23%
0.23%
0.23%
and
and
and 0.43%
0.43%
0.43% Ni
NiNi steels,
steels,
steels, respectively.
respectively.
respectively.

Figure 9. Effect of nickel content and simulated heat input on average impact energy at −20 ◦ C in the
Figure
Figure 9. 9. Effect
Effect of of nickel
nickel content
content andand simulated
simulated heat
heat input
input onon average
average impact
impact energy
energy at at
−20−20 in in
°C°C thethe
simulated CGHAZ.
simulated CGHAZ.
simulated CGHAZ.
Figure 10 displays the characteristics of impact fracture for all samples with varying Ni content and
Figure 10 displays thethe characteristics
ofof impact fractureforfor
allall samples with varying NiNi content
heatFigure
inputs. 10The
displays
fracture characteristics
surfaces of Ni-free impact
steel fracture
exhibited river samples
pattern with varying
characteristic content
of quasi-cleavage
and
and heat inputs.
heat inputs. The fracture surfaces of Ni-free steel exhibited river pattern characteristic of quasi-
fracture (Figure The fracture
10a,b). surfaces
In contrast, theof Ni-free
impact steel exhibited
fracture surface of river
0.23%pattern
Ni and characteristic
0.43% Ni steelsofconsisted
quasi-
cleavage fracture (Figure 10a,b). In contrast, the impact fracture surface of 0.23% Ni and 0.43% NiNi
cleavage fracture (Figure 10a,b). In contrast, the impact fracture surface of 0.23% Ni and 0.43%
steelsconsisted
steels consistedofofdimples
dimples(Figure
(Figure10c–f).
10c–f).Therefore,
Therefore,thethedifference
differenceininthethenature
natureofofthethefracture
fracture
surface can be attributed to transition in the fracture mechanism from quasi-cleavage
surface can be attributed to transition in the fracture mechanism from quasi-cleavage to dimple to dimple
fracture
fracture [16].
[16].
 Metals 2018, 8, 718 9 of 12

of dimples (Figure 10c–f). Therefore, the difference in the nature of the fracture surface can be attributed
to transition
Metals inPEER
2018, 8, x FOR the fracture
REVIEW mechanism from quasi-cleavage to dimple fracture [16]. 9 of 12

Figure 10.10.
Figure SEM images
SEM imagesof of
impact fracture
impact fracturesurface
surfaceofofsimulated
simulatedspecimens.
specimens.(a,b)
(a,b)Ni-free,
Ni-free, (c,d)
(c,d) 0.23%
0.23% Ni
Ni and
and (e,f)
(e,f) 0.43%
0.43% Ni
Ni for
for heat
heat input
input of
of (a,c,e)
(a,c,e) 20
20 kJ/cm
kJ/cm and (b,d,f) 100 kJ/cm.
and (b,d,f) 100 kJ/cm.

4. Discussion
4. Discussion
4.1. The Effect of Ni Addition on AF Formation and Impact Toughness
4.1. The Effect of Ni Addition on AF Formation and Impact Toughness
AF, also known as intragranular bainite, is the predominant microstructure in the CGHAZ of
AF, also known as intragranular bainite, is the predominant microstructure in the CGHAZ of
HSLA steels [3]. The formation of AF is strongly affected by the chemical composition of steel,
HSLA steels [3]. The formation of AF is strongly affected by the chemical composition of steel,
inclusions, isothermal temperature, continuous cooling rate, and austenite grain size [4]. In the present
inclusions, isothermal temperature, continuous cooling rate, and austenite grain size [4]. In the
study, the inclusion content, cooling rate, and prior austenite grain size were similar for three steels.
present study, the inclusion content, cooling rate, and prior austenite grain size were similar for three
The frequencies of AF grains in 0.23% Ni and 0.43% Ni steels were relatively higher in comparison to
steels. The frequencies of AF grains in 0.23% Ni and 0.43% Ni steels were relatively higher in
Ni-free steel because of the different Ni content. Nickel can also decrease bainite start (Bs ) and bainite
comparison to Ni-free steel because of the different Ni content. Nickel can also decrease bainite start
finish (Bf ) transformation temperature in steel [4]. Figure 11a–c shows the continuous cooling curves
(Bs) and bainite finish (Bf) transformation temperature in steel [4]. Figure 11a–c shows the continuous
of three steels for different cooling rates, which were calculated using J-MatPro software. The Bs and
cooling curves of three steels for different cooling rates, which were calculated using J-MatPro
Bf temperatures for the samples cooled at a cooling rate of 6 ◦ C/s (similar to 100 kJ/cm heat input
software. The Bs and Bf temperatures for the samples cooled at a cooling rate of 6 °C/s (similar to 100
simulated welding) were selected (Figure 11d). It was discerned that B transformation temperature
kJ/cm heat input simulated welding) were selected (Figure 11d). Its was discerned that Bs
transformation temperature decreased from 596 °C to 589 °C with increased Ni content. Thus, the
higher degree of supercooling induced an increase in Gibbs free energy and nucleation efficiency of
AF. A previous study suggested that AF grains grow faster at lower temperatures [17]; hence, the
percentage of AF increased with increased Ni content.
 Metals 2018, 8, 718 10 of 12

decreased from 596 ◦ C to 589 ◦ C with increased Ni content. Thus, the higher degree of supercooling
induced an increase in Gibbs free energy and nucleation efficiency of AF. A previous study suggested
that AF grains grow faster at lower temperatures [17]; hence, the percentage of AF increased with
increased
Metals 2018, 8, x Ni
FORcontent.
PEER REVIEW 10 of 12

Figure 11. 11.

Figure Calculated
Calculated continuous
continuouscooling curves
cooling curves prepared
preparedby using J-MatPro
by using for for
J-MatPro (a) Ni-free, (b) 0.23%
(a) Ni-free, (b) 0.23%
Ni Ni
andand(c) (c)
0.43%0.43% NiNi steels,
steels,and (d)BBs sand
and(d) andBBf f temperatures
temperatures of three samples
of three sampleswith
withacooling
acoolingrate
rate
of of
6 ◦6C/s.
°C/s.
The FsF, sB, sB,s,BBf ,f,PPss,, P
The Pff,, and
and M Mssindicate
indicateferrite
ferritestart,
start,bainite
bainitestart, bainite
start, finish,
bainite pearlite
finish, start,
pearlite pearlite
start, pearlite
finish andand
finish martensite
martensite start transformation
start transformation temperature,
temperature, respectively.
respectively.

AFAFmicrostructure
microstructure with high-angle
with high-angle boundaries
boundaries cancan
enhance
enhancethethe
toughness
toughness of HSLA
of HSLA steels by by
steels
deflecting
deflectingthethepropagation
propagation of cleavage
of cleavagecrack [18].
crack In the
[18]. present
In the study,
present thethe
study, frequency
frequencyof AF grains
of AF in in
grains
0.23% Ni and 0.43% Ni steels was observed to be relatively higher than in Ni-free steel. Moreover, AF
0.23% Ni and 0.43% Ni steels was observed to be relatively higher than in Ni-free steel. Moreover,
effectively refinedrefined
AF effectively the prior
theaustenite grains grains
prior austenite in the CGHAZ. Thus, the
in the CGHAZ. formation
Thus, of high-density
the formation AF
of high-density
grains in 0.23%
AF grains Ni andNi0.43%
in 0.23% Ni steels
and 0.43% contributed
Ni steels to a higher
contributed percentage
to a higher of grain
percentage of refinement. In
grain refinement.
addition, the average diameter of crystallographic grains was lower in 0.23% Ni and 0.43% Ni steels Ni
In addition, the average diameter of crystallographic grains was lower in 0.23% Ni and 0.43%
than in Ni-free
steels than insteel.
Ni-freeFurthermore, because of
steel. Furthermore, the fine-grained
because microstructure
of the fine-grained of AF, the
microstructure ofcracks
AF, thewere
cracks
lesswere
mobilelessand theirand
mobile direction of propagation
their direction was able to
of propagation waschange during
able to changetheduring
Charpy v-notch
the Charpy impact
v-notch
testimpact
[18]. Ittest
can therefore
[18]. be inferred
It can therefore that 0.23%
be inferred Ni andNi0.43%
that 0.23% Ni steels
and 0.43% possessed
Ni steels higher
possessed impact
higher impact
toughness
toughness in comparison
in comparison to Ni-free steel.
to Ni-free steel.

4.2.4.2.
TheThe
Effect of Ni
Effect of Addition on M-A
Ni Addition Constituents
on M-A andand
Constituents Impact Toughness
Impact Toughness

M-A M-Aconstituents have

constituents a significant
have influence
a significant influenceon on
thethe
toughness
toughnessof of
HAZHAZ[15]. Carbon
[15]. diffuses
Carbon diffuses
into the untransformed austenite in CGHAZ, and these untransformed austenite areas become
into the untransformed austenite in CGHAZ, and these untransformed austenite areas become carbon
carbon enriched and are transformed into hard and brittle M-A constituents during continuous [4].
enriched and are transformed into hard and brittle M-A constituents during continuous cooling
cooling [4]. Subsequently,
Subsequently, microcracks microcracks are easily
are easily nucleated at thenucleated
boundariesatbetween
the boundaries between
M-A constituents andM-A
ferrite
constituents and ferrite matrix. These cracks further propagate into the matrix when the stressthe
matrix. These cracks further propagate into the matrix when the stress concentration exceeds
concentration exceeds the critical stress of M-A constituents [4]. In the present study, SEM analysis
revealed the presence of M-A constituents in bainite matrix (Figure 5). Moreover, the area percentage
of M-A constituents decreased with increased Ni content. This finding is not in agreement with the
previous result that showed an increase in M-A constituents with increased Ni content in high-
strength steel [4]. The calculation of continuous cooling transformation also demonstrated that the
Metals 2018, 8, 718 11 of 12

critical stress of M-A constituents [4]. In the present study, SEM analysis revealed the presence of M-A
constituents in bainite matrix (Figure 5). Moreover, the area percentage of M-A constituents decreased
with increased Ni content. This finding is not in agreement with the previous result that showed an
increase in M-A constituents with increased Ni content in high-strength steel [4]. The calculation of
continuous cooling transformation also demonstrated that the temperature gap between Bs and Bf
increased from 67 ◦ C to 77 ◦ C (from Ni-free to 0.43% Ni steel) (Figure 11d). Thus, more austenite was
transformed into bainitic ferrite and AF. Also, the amount of M-A constituents was lower in 0.23% Ni
and 0.43% Ni steels, and thereby contributed to high impact toughness in CGHAZ.

5. Conclusions
(1) The microstructure of simulated CGHAZ in the three steel samples with heat input of
20–100 kJ/cm predominantly consisted of bainite and a small proportion of AF and M-A
constituents. Although the small addition of Ni showed no significant effect on bainitic
microstructure, it significantly influenced the formation of AF and M-A constituents. The area
percentage of AF and M-A constituents in the simulated CGHAZ increased and decreased with
increased Ni content, respectively.
(2) The impact toughness of simulated CGHAZ at −20 ◦ C increased with increased Ni content
because of the fine-grained microstructure with more AF and fewer M-A constituents.

Author Contributions: K.W. conceived, X.W. and G.H. designed the experiments; G.H. performed the experiments
and wrote the manuscript; H.Z. supplied the raw materials and R.D.K.M. revised the grammar of the manuscript.
Funding: The Major Technology Innovation of Hubei Province under grant (No. 2016AAA022); the National
Natural Science Foundation of China (No. 51501134); China Postdoctoral Science Foundation (No. 2014M550414).
Acknowledgments: The authors gratefully acknowledge the financial support from the Major Technology
Innovation of Hubei Province under grant No. 2016AAA022 and the National Natural Science Foundation
of China (No. 51501134) and China Postdoctoral Science Foundation (No. 2014M550414).
Conflicts of Interest: The authors declare no conflict of interest.

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