3.4 5.

Article

On the Post-Printing Heat

Treatment of a Wire Arc Additively
Manufactured ER70S Part

Alireza Vahedi Nemani, Mahya Ghaffari and Ali Nasiri

https://doi.org/10.3390/ma13122795
 materials
Article
On the Post-Printing Heat Treatment of a Wire Arc
Additively Manufactured ER70S Part
Alireza Vahedi Nemani *, Mahya Ghaffari and Ali Nasiri
Faculty of Engineering and Applied Science, Memorial University of Newfoundland,
St. John’s, NL A1B 3X5, Canada; [email protected] (M.G.); [email protected] (A.N.)
* Correspondence: [email protected]




Received: 24 May 2020; Accepted: 18 June 2020; Published: 21 June 2020


Abstract: Wire arc additive manufacturing (WAAM) is known to induce a considerable microstructural
inhomogeneity and anisotropy in mechanical properties, which can potentially be minimized by
adopting appropriate post-printing heat treatment. In this paper, the effects of two heat treatment
cycles, including hardening and normalizing on the microstructure and mechanical properties of
a WAAM-fabricated low-carbon low-alloy steel (ER70S-6) are studied. The microstructure in the
melt pools of the as-printed sample was found to contain a low volume fraction of lamellar pearlite
formed along the grain boundaries of polygonal ferrite as the predominant micro-constituents.
The grain coarsening in the heat affected zone (HAZ) was also detected at the periphery of each melt
pool boundary, leading to a noticeable microstructural inhomogeneity in the as-fabricated sample.
In order to modify the nonuniformity of the microstructure, a normalizing treatment was employed
to promote a homogenous microstructure with uniform grain size throughout the melt pools and
HAZs. Differently, the hardening treatment contributed to the formation of two non-equilibrium
micro-constituents, i.e., acicular ferrite and bainite, primarily adjacent to the lamellar pearlite phase.
The results of microhardness testing revealed that the normalizing treatment slightly decreases the
microhardness of the sample; however, the formation of non-equilibrium phases during hardening
process significantly increased the microhardness of the component. Tensile testing of the as-printed
part in the building and deposition directions revealed an anisotropic ductility. Although normalizing
treatment did not contribute to the tensile strength improvement of the component, it suppressed the
observed anisotropy in ductility. On the contrary, the hardening treatment raised the tensile strength,
but further intensified the anisotropic behavior of the component.

Keywords: wire arc additive manufacturing; ER70S-6; anisotropic mechanical properties; microstructure;
heat treatment

1. Introduction
Wire arc additive manufacturing (WAAM) is a novel technology capable of producing metallic
components utilizing an arc welding process to additively fabricate engineering parts [1], with various
applications such as impeller blades [2], bridge structures [3], shipbuilding plates [4], and wing ribs in
the aerospace industry [5]. Different from the metal powder-based additive manufacturing processes,
such as direct metal laser sintering (DMLS) and selective laser melting (SLM), wire arc additive
manufacturing uses a consumable metallic wire as the feedstock material [6]. In WAAM, the entire
consumable wire is continuously fed into an adopted electric arc or plasma, leading to an extremely
high deposition rate as compared to that of the powder-based AM systems [7]. Therefore, wire-based
systems are generally suitable for producing large-scale components with less complexity in geometry
and design, in contrast to the powder-bed systems, which typically fabricate small and high-definition
parts [8]. From another perspective, powder-bed additive manufacturing techniques are limited to a

Materials 2020, 13, 2795; doi:10.3390/ma13122795 www.mdpi.com/journal/materials

Materials 2020, 13, 2795 2 of 13

build envelope, but in wire-based systems, the torch is usually mounted on a robotic arm having more
freedom of movement, implying that the component’s size is not confined by a chamber.
During wire arc additive manufacturing process, the feedstock material is melted and deposited
in the form of weld beads layer by layer on the previously solidified tracks. As the consecutive
layers fuse into the previous ones, the material is built up until the near-net-shape component is
completed [9]. Since the process is involved with sequential melting and solidification, each region
of the component is subjected to periodic fast heating and cooling cycles by the deposition of upper
layers. Such complex localized thermal cycles lead to heterogeneous microstructure and anisotropic
mechanical properties in the AM-fabricated components [1,10,11]. This is one of the main drawbacks of
the WAAM technique as compared to the conventional methods of manufacturing. Sridharan et al. [12]
studied the microstructure and mechanical properties of low-carbon low-alloy steel (ER70S) built
through additive manufacturing and reported anisotropic elongation percentages in different directions.
They concluded that the anisotropy in mechanical properties is related to the inhomogeneous and
localized microstructure [12]. Haden et al. [13] also investigated wire arc additive manufacturing of
304 stainless steel and reported graded wear and hardness properties in both deposition and building
directions. Their findings showed that this anisotropy is due to the fluctuation in localized thermal
histories, consequently leading to the formation of a variety of microstructures, from austenitic to
solidification structures owning mixed ferrite morphology with abrupt texture changes at different
regions of the sample [13].
In addition to the microstructural inhomogeneity, the formation of internal defects between the
deposited layers as a result of high heat removal capacity from the inter-pass regions may deteriorate
the mechanical properties of the additively manufactured components [6,12,14,15]. The inter-pass
defects being formed in the fusion boundaries commonly include entrapped gas, porosities, and lack of
fusion [16,17]. The presence of the mentioned discontinuities acting as a stress riser in the structure can
potentially make crack initiation sites leading to premature brittle fracture under tension, which has
been extensively investigated in a previous authors’ publication [14].
Interestingly, the heterogeneous microstructure and anisotropic mechanical properties in a
WAAM-fabricated part can be minimized by applying tailored post-printing heat treatment cycles [4].
For instance, Wang et al. [18] studied the effect of heat treatment on the anisotropic mechanical
properties of a WAAM-fabricated H13 steel. They reported that the homogeneous microstructure
achieved by annealing heat treatment for four hours at 830 ◦ C led to diminishing the anisotropic
mechanical properties of the part. Xu et al. [19] also successfully minimized the microstructural
inhomogeneity of a wire arc additive manufactured maraging steel part by performing a post-process
heat treatment i.e., solutionizing and aging, which resulted in a significant improvement in mechanical
properties of the WAAM-fabricated component. Although applying a post-fabrication heat treatment
has been previously reported by different studies [18–20], to the best of the authors’ knowledge,
heat treatment of WAAM ER70S-6 has not been investigated heretofore, except for one of the authors’
previous studies [4], in which the impacts of a different heat treatment cycle (inter-critical austenitizing
temperature) on the WAAM ER70S-6 microstructure and mechanical properties were investigated.
In this study, with the aim of homogenizing the microstructure and diminishing the induced
anisotropy in an as-printed WAAM-ER70S-6 low-carbon low-alloy steel part, two heat treatment
cycles, including normalizing (austenitizing followed by still-air cooling) and hardening (austenitizing
followed by water quenching) from an upper-critical austenitizing temperature, were conducted on
the as-printed samples. Microstructural and mechanical property characterizations were carried out
on both as-printed and heat-treated samples in different orientations, including deposition (horizontal)
and building (vertical) directions.
STT can further contribute to reducing the surface irregularities and spattering during the building
process [21]. In order to smoothly feed the wire to the melt pool, the stand-off distance was held
constant at 3 mm between the tip of the filler wire and the surface of the previous layer. Figure 1
schematically represents the set-up of the WAAM process.
Table 1 shows the nominal chemical composition of the ER70S-6 feedstock solid wire with 0.9
Materials 2020, 13, 2795 3 of 13
mm diameter manufactured by Lincoln Electric. The selected WAAM process parameters yielding
the optimum bead quality and appearance with minimum spattering are listed in Table 2. ASTM A36
mild steel with
2. Materials and a thickness
Methods of 12 mm was used as the substrate, which was attentively wire brushed
and then cleaned by acetone to prevent contamination of the melt pools and the formation of gas
pores during Fabrication
2.1. Material, the solidification
Process, process. The whole Heat
and Post-Fabrication part Treatment
contained 50 consecutive layers, and each
layer Inwas comprised of six beads with a length of 135 mm and a 3 mm
the present study, a wall of low-carbon low-alloy steel (ER70S-6) wascenter-to-center
fabricated using overlap,
the wire
resulting
arc additivein amanufacturing
wall with a total
methodwidth of 22 amm
utilizing and Electric
Lincoln a heightGMA
of 150 mm. Employing
machine (Cleveland,aOH,
Thermo-
USA)
Scientific
with a torch Lindberg
mounted furnace, two Fanuc
on a 6-axis heat treatment cycles
robot as the were
power applied
source. to the as-printed
To minimize the heatcomponent,
input of the
including (i) normalizing (austenitizing followed by still-air cooling), and (ii) hardening
WAAM process and be able to adjust the heat independent of the wire feed speed, an advanced current
(austenitizing followed by water quenching). For initial austenitizing in both cycles, the samples were
controlled surface tension transfer (STT) process was employed for fabrication. Utilizing the STT can
heated up to 900 °C for 1 h. The purpose of the normalizing process was to homogenize the
further contribute to reducing the surface irregularities and spattering during the building process [21].
microstructure by producing a uniform grain size along the melt pools, fusion boundaries, and heat
In order to smoothly feed the wire to the melt pool, the stand-off distance was held constant at 3 mm
affected zones. The intention of the hardening heat treatment was also to increase the hardness and
between the tip of the filler wire and the surface of the previous layer. Figure 1 schematically represents
tensile strength of the component.
the set-up of the WAAM process.

Figure
Figure 1.
1. Schematic
Schematicillustration
illustrationof
ofthe
the wire
wire arc
arc additive
additive manufacturing
manufacturing (WAAM)
(WAAM) wall
wall and
and tensile
tensile
sample
sample selection.
selection.

Table 1 shows the

Table 1. nominal
The nominalchemical
chemicalcomposition of the
composition of theER70S-6
ER70S-6feedstock
feedstock solid
wire wire with 0.9 mm
(wt.%).
diameter manufactured by Lincoln Electric. The selected WAAM process parameters yielding the
optimum bead CqualityMn Si
and appearance S
withPminimum
Cr Ni Mo
spattering are VlistedCu Fe
in Table 2. ASTM A36
0.06– 1.40– 0.80– 0.04 0.03 0.15 0.15 0.15 0.03 0.5
mild steel with0.15
a thickness Bal.
1.85 of 12
1.15mm was
max used
maxas the
maxsubstrate,
max max whichmax
was attentively
max wire brushed
and then cleaned by acetone to prevent contamination of the melt pools and the formation of gas
pores during the solidification process. The whole part contained 50 consecutive layers, and each
layer was comprised of six beads with a length of 135 mm and a 3 mm center-to-center overlap,
resulting in a wall with a total width of 22 mm and a height of 150 mm. Employing a Thermo-Scientific
Lindberg furnace, two heat treatment cycles were applied to the as-printed component, including
(i) normalizing (austenitizing followed by still-air cooling), and (ii) hardening (austenitizing followed
by water quenching). For initial austenitizing in both cycles, the samples were heated up to 900 ◦ C for
1 h. The purpose of the normalizing process was to homogenize the microstructure by producing a
uniform grain size along the melt pools, fusion boundaries, and heat affected zones. The intention of
the hardening heat treatment was also to increase the hardness and tensile strength of the component.

Table 1. The nominal chemical composition of the ER70S-6 feedstock wire (wt.%).

C Mn Si S P Cr Ni Mo V Cu Fe
0.06–0.15 1.40–1.85 0.80–1.15 0.04 max 0.03 max 0.15 max 0.15 max 0.15 max 0.03 max 0.5 max Bal.
Materials 2020, 13, 2795 4 of 13

Table 2. The processing parameters used for the wire arc additive manufacturing of the low-carbon
low-alloy steel (ER70S-6).

Average Arc Wire Feeding Scanning Argon Flow

Arc Voltage Heat Input
Current Rate Rate Rate
135 A 28 V 104 mm/s 5 mm/s 20 L/min 7.56 kJ/cm

2.2. Microstructural Characterization

To prepare the samples for microstructural characterizations, a Tegramin-30 Struers auto-grinder/
polisher (Cleveland, OH, USA) was employed, then the samples were etched chemically using a 5 vol.%
Nital reagent for 15–20 s [22]. The microstructure of the fabricated component was characterized
at different regions from the bottom to the top of the wall to detect any microstructural changes
throughout the whole part. To perform the microstructural characterization at different magnifications,
an optical microscope (Nikon Eclipse 50i, Shinagawa, Tokyo, Japan) and a field emission scanning
electron microscope (FEI MLA 650F, Hillsboro, OR, USA) were employed.

2.3. Mechanical Properties Evaluation

Microhardness distribution was measured and plotted along a line covering five successive
layers through the building (vertical) direction on different zones including the center of the melt
pools, fusion boundaries, and heat affected zones (HAZs), using a Buehler Micromet hardness test
machine (Lake Bluff, IL, USA) with the applied load of 300 g and an indentation time of 45 s. It should
be noted that the reported data of microhardness are the average of five different measurements.
The indentations were done on the polished and etched surfaces in order to distinguish the position of
each indentation relative to the melt pool’s geometry. Moreover, microhardness profiles were produced
by subsequent indentations with 300 µm intervals (approximately five times more than the diagonal of
each indent) to avoid the work hardening effect.
Tensile test specimens from the as-printed and heat-treated samples were machined parallel and
perpendicular to the building directions based on the ASTM E8m-04 standard sub-size specimen
(West Conshohocken, PA, USA) [23] with dimensions of 100 mm × 25 mm × 5 mm. The room
temperature uniaxial tensile tests were carried out using an Instron load frame (Norwood, MA, USA)
equipped with an extensometer at the crosshead speed of 8 mm/min. Each tensile test was repeated
five times under the same conditions to obtain a reliable average value.

3. Results and Discussion

3.1. Microstructural Characterization

Figure 2a illustrates a low magnification OM micrograph of the as-printed sample showing the
transition from the center of the melt pool to the melt pool boundary and then the heat affected
zone. The dominant microstructure in the center of the melt pool consists of a low volume fraction of
lamellar pearlite (P) primarily formed at the grain boundaries of polygonal ferrite (PF) (Figure 2b).
Figure 2c depicts the SEM micrograph taken from the melt pool boundary region (denoted as the
fusion boundary shown in Figure 2a) at higher magnification, revealing the formation of acicular
ferrite (AF) and bainite (B) due to the faster cooling rate along the boundaries of each deposited bead
as compared to its center. The aforementioned transition in the microstructure during 3D-printing
of ER70S wire is also reported by Haselhuhn et al. [24]. In another investigation, Lee et al. [25] also
studied the microstructure of the welded low-carbon low-alloy AH36 steel and similarly reported the
formation of acicular ferrite and bainite near the fusion line.
the HAZ can potentially lead to a remarkable softening in this area, consequently resulting in a
reduced localized strength and hardness in a sample that accommodates this region [29]. The
formation of such microstructural inhomogeneity from the center of the melt pool to its boundaries
and to HAZ is attributed to the overlapping scanning strategy associated with the multi-layer
deposition
Materials 2020,nature
13, 2795of the WAAM process. Consequently, this process evokes various thermal cycles
5 of 13
in different regions of the sample [30].

Figure
Figure2.2.(a)
(a)Low
Lowmagnification
magnificationoptical
opticalmicrograph
micrographofofthe
theas-printed
as-printedsample,
sample,(b)
(b)higher
highermagnification
magnification
SEM
SEMmicrograph
micrographof ofthe
themelt
meltpool
poolcenter,
center, and
and (c)
(c) fusion
fusion boundary
boundary (PF:
(PF: polygonal
polygonal ferrite,
ferrite, P:
P: lamellar
lamellar
pearlite,
pearlite, B:
B: bainite,
bainite, AF:
AF: acicular
acicular ferrite).
ferrite).

Post
It is printing heat treatment
well established that is
thecommonly
presenceused to modify
of acicular the microstructure
ferrite and, consequently
and bainite constituents in the
the mechanical properties
microstructure of steels canofpromote
an additively manufactured
the mechanical component
properties of the [4,20]. FigureThis
component. 3a–disdepict the
primarily
microstructure of the WAAM-ER70S-6 wall after applying different heat treatment cycles, including
resulted from the finer structure of both phases, a more uniform distribution of carbide and higher
normalizing (Figureand
dislocation density 3a,b) and hardening
internal stresses in (Figure 3c,d)
the bainite at different
phase, magnifications.
contributing According to the
to a higher hardness/strength
thermodynamically
and ductility in the simulated continuous
alloy [26–28]. However, cooling transformation
it should be noted that(CCT) diagram
since for thefraction
the volume ER70S-6 of
wire [31], moderate cooling rates in the range of 10–100 °C/s results in a ferritic–pearlitic
acicular ferrite and bainite constituents are negligible as compared to the dominant ferritic and pearlitic
microstructure,
microstructure while of the severe cooling
alloy, the rates in
presence of the rangeferrite
acicular of 0.1–1
and °C/s leadscannot
bainite to the formation of non-
have a significant
equilibrium
contributionphases such as bainite.
to the mechanical As indicated
properties in Figure 3a,b,sample.
of the WAAM-ER70S the normalizing heat hand,
On the other treatment with
according
moderate cooling rate from the austenitizing temperature of 900 °C, has not altered the pre-existing
to Figure 2a, the microstructure of the HAZ consists of coarser grains of polygonal ferrite in comparison
constituents of the
with the interior of microstructure
the melt pool, asofthethethermal
as-printed
cyclesample. However,
associated with each thedepositing
grain sizetrack
became more
facilitates
uniform and homogenous from the center of each melt pool toward the heat affected zone in to
the grain growth in the previous bead. The grain coarsening in the HAZ can potentially lead thea
adjacent
remarkable track. In other
softening in words, the
this area, grain coarsening
consequently in the
resulting in aheat affected
reduced zone strength
localized was eliminated after
and hardness
normalizing
in a sample thatheataccommodates
treatment. this region [29]. The formation of such microstructural inhomogeneity
from the center of the melt pool to its boundaries and to HAZ is attributed to the overlapping scanning
strategy associated with the multi-layer deposition nature of the WAAM process. Consequently,
this process evokes various thermal cycles in different regions of the sample [30].
Post printing heat treatment is commonly used to modify the microstructure and, consequently
the mechanical properties of an additively manufactured component [4,20]. Figure 3a–d depict the
microstructure of the WAAM-ER70S-6 wall after applying different heat treatment cycles, including
normalizing (Figure 3a,b) and hardening (Figure 3c,d) at different magnifications. According to the
thermodynamically simulated continuous cooling transformation (CCT) diagram for the ER70S-6
wire [31], moderate cooling rates in the range of 10–100 ◦ C/s results in a ferritic–pearlitic microstructure,
while severe cooling rates in the range of 0.1–1 ◦ C/s leads to the formation of non-equilibrium phases
such as bainite. As indicated in Figure 3a,b, the normalizing heat treatment with moderate cooling
as-received material. Figure 3c,d illustrate the microstructure after hardening heat treatment, which
is a mixture of pearlite, bainite and acicular ferrite. In the case of hardening heat treatment cycle, the
sample was exposed to an extremely high cooling rate (water quenching), resulting in the formation
of the meta-stable bainite and acicular ferrite phases besides the lamellar pearlite phase. It should be
Materials 2020, 13, 2795 6 of 13
mentioned that similar to the scenario of the normalizing heat treatment, the hardening heat
treatment also resulted in the formation of a homogeneous microstructure with a uniform grain size
throughout
rate from thethesample from the
austenitizing bottom toofthe
temperature 900top of the WAAM-fabricated wall. The formation of
◦ C, has not altered the pre-existing constituents of

the acicular ferrite and bainite phases by quenching of the

the microstructure of the as-printed sample. However, thesample at higher
grain size becamecooling rates from
more uniform and the
austenite stabilityfrom
homogenous region
thehas alsoofbeen
center eachreported
melt poolintoward
other low-carbon low-alloy
the heat affected steels,
zone in such astrack.
the adjacent API X70
In other words, the grain coarsening in the heat affected zone was eliminated after normalizing
and X80 [26,27,35].
heat treatment.

Figure 3. The microstructure of the normalized sample (a,b), and hardened (water-quenched) sample
Figure 3. The microstructure of the normalized sample (a and b), and hardened (water-quenched)
(c,d) at different magnifications.
sample (c and d) at different magnifications.
For the initial austenitizing step, the sample was heated up to 900 ◦ C, where γ is the only stable
phase since the Ac3 temperature of the alloy was calculated to be at ~883 ◦ C, using a reported empirical
equation that predicts austenite formation temperatures, i.e., Ac1 and Ac3 , for the low-alloy steels
with less than 0.6 wt.% C [32]. Subsequently, uniformly distributed austenite grains nucleate and
grow evenly in any region of the material during austenitization. Following the full austenitization
of the microstructure, the sample is subjected to a relatively slow cooling by exposing the sample to
room temperature. The slow cooling rate associated with the normalizing heat treatment hinders the
formation of unstable or metastable phases, such as bainite or martensite, during the normalizing
heat treatment. Therefore, the microstructure of the sample in terms of the formed constituents was
analogous to the dominant microstructure of the as-printed sample containing polygonal ferrite,
pearlite and precipitation of tertiary cementite, whilst the grains obtained a more homogeneous and
uniform distribution after the normalizing heat treatment. The precipitation of the tertiary cementite in
the ferrite grain boundaries, as a high energy site for nucleation of a new phase, has been also reported
in other grades of low-carbon steels family [33,34]. Natividad et al. [35] also performed the normalizing
heat treatment on Grade X70 pipeline steel and reported the formation of polygonal ferrite and pearlite
areas with more homogenous and uniform microstructure in comparison with the as-received material.
Figure 3c,d illustrate the microstructure after hardening heat treatment, which is a mixture of pearlite,
Materials 2020, 13, 2795 7 of 13

bainite and acicular ferrite. In the case of hardening heat treatment cycle, the sample was exposed to
an extremely high cooling rate (water quenching), resulting in the formation of the meta-stable bainite
and acicular ferrite phases besides the lamellar pearlite phase. It should be mentioned that similar
to the scenario of the normalizing heat treatment, the hardening heat treatment also resulted in the
formation of a homogeneous microstructure with a uniform grain size throughout the sample from
the bottom to the top of the WAAM-fabricated wall. The formation of the acicular ferrite and bainite
phases by quenching of the sample at higher cooling rates from the austenite stability region has also
Materials
been 2020, 13,in
reported x FOR PEER
other REVIEW low-alloy steels, such as API X70 and X80 [26,27,35].
low-carbon 7 of 13

3.2. Mechanical
3.2. Mechanical Properties
Properties Evaluation
Evaluation
Figure 44 shows
Figure shows the themicrohardness
microhardnessprofile profileofofthe as-printed
the as-printedand andheat-treated
heat-treatedsamples along
samples alonga line
a
covering
line five five
covering consecutive
consecutive layers
layersthrough
through thethebuilding
building(vertical)
(vertical)direction
direction onon different zones,
different zones,
including the center of the melt pools, fusion boundaries, and heat affected zones (HAZs). The overall
including the center of the melt pools, fusion boundaries, and heat affected zones (HAZs). The overall
microhardness of
microhardness of the
the as-printed
as-printed sample
sample was was 160
160 ±± 77 HV,HV, which
which showed
showed aa relatively
relatively significant
significant
fluctuation from
fluctuation from aa minimum
minimum of of 150
150 ± ± 11 HV
HV toto 160
160 ± ± 22 HV, and then
HV, and then to to the
the maximum
maximum of of 175
175 ±± 22 HV.
HV.
The observed fluctuation was ascribed to the presence of different phases along the melt pool center,
The observed fluctuation was ascribed to the presence of different phases along the melt pool center,
the fusion
the fusion boundary,
boundary, and and the
theheat
heataffected
affectedzone.
zone. In In particular,
particular,the
thelowest
lowestamount
amount of ofmicrohardness
microhardness
(150 ± 1 HV) corresponded to the HAZ containing coarser polygonal ferrite grains than the
(150 ± 1 HV) corresponded to the HAZ containing coarser polygonal ferrite grains than the rest
rest of
of the
the
fusion zone, and the maximum microhardness (175 ± 2 HV) was correlated to the fusion boundaries,
fusion zone, and the maximum microhardness (175 ± 2 HV) was correlated to the fusion boundaries,
whereacicular
where acicularferrite
ferriteand
andbainite
bainiteconstituents
constituentsexist.
exist.TheThecenter
centerofof the
the melt
melt pool,
pool, owning
owning thethe dominant
dominant
microstructure of the component (lamellar pearlite and polygonal ferrite), revealed the
microstructure of the component (lamellar pearlite and polygonal ferrite), revealed the microhardness
microhardness
of 160 ± 2 HV. The of 160 ± 2 HV. The
fluctuations fluctuations
in the microhardnessin thevalues
microhardness values were
were considerably lowerconsiderably lower
in both hardened
in both hardenedand
(water-quenched) (water-quenched)
normalized samples and normalized
as comparedsamples as compared
to the as-printed to the due
component as-printed
to the
component due
homogeneity to the
of the homogeneityinofthe
microstructure theheat-treated
microstructure in the heat-treated samples.
samples.

Figure 4. Vickers microhardness profile of the as-printed and heat-treated samples along a line covering
Figure
five 4. Vickers
successive microhardness
layers profile of
through the building the as-printed
(vertical) direction.and heat-treated samples along a line
covering five successive layers through the building (vertical) direction.

The normalized sample with a microstructure analogous to the dominant microstructure of the
as-printed sample showed the microhardness of 154 ± 1 HV, comparable to that of the center of the
melt pools in the as-printed sample. It is also worth noting that the microhardness of the normalized
sample was slightly decreased after the heat treatment, primarily due to (i) the stress relieving
Materials 2020, 13, 2795 8 of 13

The normalized sample with a microstructure analogous to the dominant microstructure of the
as-printed sample showed the microhardness of 154 ± 1 HV, comparable to that of the center of the
melt pools in the as-printed sample. It is also worth noting that the microhardness of the normalized
sample was slightly decreased after the heat treatment, primarily due to (i) the stress relieving occurred
during heating to austenitizing temperature, (ii) diminishing of lattice defects formed during the
rapid solidification associated with the WAAM, (iii) potential growth of primary austenite grains [36],
and (iv) omitting the acicular ferrite and bainite phases from the microstructure of the fusion boundaries.
Contrarily, the microhardness of the hardened (water-quenched) sample was 260 ± 3 HV, drastically
higher than the other samples, a phenomena ascribed to its microstructure, including pearlite, bainite,
and acicular ferrite as the predominant micro-constituents in its structure. It has been reported that the
presence of bainite, along with a finer microstructure, can increase the microhardness of low-carbon
steels [36]. However, it should also be noted that a higher microhardness is not always beneficial to the
overall mechanical performance of the material since the ductility and toughness of the alloy could
potentially be degraded. The adverse effect of existing hard micro-constituents can be more crucial
particularly in the case of samples manufactured by a welding process, which are usually prone to the
presence of welding defects, discontinuities, and residual stresses. Such discontinuities can readily
propagate into a brittle microstructure and form internal micro-cracks during the tensile loading of
the sample.
Figure 5 shows the engineering tensile stress–strain curves for the as-printed and heat-treated
WAAM-ER70S-6 samples in the building (vertical) and deposition (horizontal) directions. In the
as-printed component, the vertical and horizontal tensile strengths were approximately similar
(~500 MPa). However, the ductility (elongation percentage) of the vertical sample only reached to
12 ± 3%, whereas the horizontal sample showed a significantly higher ductility at 35 ± 2%, indicating
a large plastic deformation prior to the fracture with an obvious necking phenomenon. Therefore,
the results of tensile testing of the as-printed part revealed anisotropy in ductility. Wang et al. [37]
investigated the anisotropy in the mechanical properties of the additively manufactured 304L stainless
steel parts, and reported that the elongation percentage in the transverse direction was higher compared
to the longitudinal direction, while the tensile strength was fairly isotropic. The substantial lower
ductility of the vertical samples as compared to the horizontal ones herein can be justified by (i) the
existence of solidification imperfections and flaws, such as inter-pass lack of fusion (LOF) and (ii) the
HAZ softening as a result of grain coarsening. Since the long axis of the inter-pass lack of fusions is
perpendicular to the loading direction in the vertical samples, the sharp edges of these defects can serve
as stress concentration sites, causing the propagation of the discontinuity in the vertical samples during
uniaxial tensile loading, but not in the horizontal ones [14]. A similar observation was also reported
by Wang et al. [38]. In another study, Lopez et al. [16] demonstrated the formation of manufacturing
defects in the wire arc additive manufacturing of ER70S-6 using different nondestructive examination
methods including radiographic testing (X-ray), liquid penetrant inspection (LPI), and ultrasonic
testing (UT), and reported the presence of the LOF defect between the deposited layers.
The anisotropy in the mechanical properties has been reported as a common issue in various
metals and alloys produced by additive manufacturing processes [39–41], which can be minimized by
applying proper post-printing heat treatment cycles [4,20]. Hardening treatment could increase the
tensile strength of the WAAM-ER70S steel from ~ 500 MPa for the as-printed sample to 640 ± 14 MPa
and 624 ± 13 MPa in vertical and horizontal heat-treated samples, respectively. This improvement
in the tensile strength of the hardened alloy is attributed to its bainitic, acicular ferritic, and pearlitic
microstructure with ~62% higher microhardness compared to the as-printed sample. However, the
ductility of the hardened samples was reduced by 4% and 7% for the vertical and horizontal samples,
respectively. Although, the horizontal sample with the ultimate tensile strength (UTS) value of
624 ± 13 MPa and elongation of 28 ± 2% plausibly satisfies the mechanical integrity requirement for
the service conditions of this alloy, the anisotropic mechanical behavior of the component cannot be
diminished since the sample revealed a severe brittle fracture in the vertical direction with only 8 ± 1%
plastic deformation prior to the fracture with an obvious necking phenomenon. Therefore, the results
of tensile testing of the as-printed part revealed anisotropy in ductility. Wang et al. [37] investigated
the anisotropy in the mechanical properties of the additively manufactured 304L stainless steel parts,
and reported that the elongation percentage in the transverse direction was higher compared to the
longitudinal direction, while the tensile strength was fairly isotropic. The substantial lower ductility
Materials 2020, 13, 2795 9 of 13
of the vertical samples as compared to the horizontal ones herein can be justified by (i) the existence
of solidification imperfections and flaws, such as inter-pass lack of fusion (LOF) and (ii) the HAZ
softening
elongation.asItashould
result beof mentioned
grain coarsening. Since
that in the casethe long
of the axis of the
as-printed inter-pass
vertical sample,lack
the of fusions of
formation is
perpendicular
some defects, flaws,to theand
loading directionweak
also possible in the vertical samples,
metallurgical bondingthebetween
sharp edges of these
the layers (lackdefects can
of fusion)
serve as stress concentration
can potentially reduce the degreesites, of
causing
plasticthe propagation
deformation thatofthe
the material
discontinuity in the verticalbefore
can accommodate samples its
during
failure. uniaxial tensilecan
This scenario loading, but not when
be intensified in the the
horizontal ones [14].
microhardness A similar
increases observation
from 160 ± 7 HV was foralso
the
reported
as-printedby Wangtoet260
sample al.±[38].
3 HVInfor another study, sample.
the hardened Lopez etConsequently,
al. [16] demonstrated
as a resultthe formation
of the hardening of
manufacturing
cycle, the ultimate defects
tensilein the wire
strength arc additive
increased manufacturing
at the expense of in
of a reduction ER70S-6
ductility.using different
Overall, it can
nondestructive
be inferred that the examination
hardening methods including
heat treatment radiographic
exhibited testing
a positive effect on(X-ray), liquid properties
the mechanical penetrant
inspection (LPI), and
in the horizontal ultrasonic
direction testing
but was (UT), and
not found reported
beneficial the vertical
to the presencesample,
of the LOF
leadingdefect between
to its brittle
the deposited
fracture during layers.
the uniaxial tensile loading.

Figure 5. The stress–strain curves for the as-printed and heat-treated samples in the building (vertical)
Figure 5. The stress–strain curves for the as-printed and heat-treated samples in the building (vertical)
and deposition (horizontal) directions.
and deposition (horizontal) directions.

On the other hand, the normalizing process that contributed to the formation of a homogenized
microstructure, characterized by a uniform grain size along the center of the melt pool, fusion boundary,
and the heat affected zone could increase the tensile strength neither in horizontal nor in the vertical
samples. Similar to the slight reduction in the microhardness of the normalized sample, its tensile
strength was expected to be slightly lower (~465 MPa) than the as-printed sample (~500 MPa). Moreover,
a closer look at the stress–strain curves of the normalized samples revealed that there is not a huge
difference between the elongation of the component in the vertical (29 ± 2%) and horizontal (34 ± 3%)
directions. It should be mentioned that the purpose of the normalizing cycle was to eliminate the
inhomogeneous microstructure that resulted from the complex thermal cycles associated with the
layer-by-layer deposition nature of the wire arc additive manufacturing process. As a consequence of
heating the sample up to a temperature above the upper critical temperature (Ac3 ), and formation
of new austenite grains, the inhomogeneous microstructure including coarse grains of HAZ was
totally eliminated. Accordingly, during the cooling process in still-air, the whole part experiences a
similar cooling rate leading to a uniform microstructure at different zones of the sample. Therefore,
the anisotropy in the elongation can be eliminated or weaken through modifying the microstructure
from an inhomogeneous one to a homogenized microstructure with a uniform grain size.
Materials 2020, 13, 2795 10 of 13

Figure 6 demonstrates the reduction in area (RA) for the as-printed and heat-treated samples in
both vertical and horizontal directions. The stereomicroscope images of the fractured surfaces are also
attached to each point of the plot in order to clarify the brittle or ductile nature of the fracture in different
samples. The results of fractography investigations revealed that horizontal samples experienced an
entire ductile fracture, while the vertical specimens showed a mixed mode of ductile-brittle fracture,
which is consistent with the results obtained from the uniaxial tensile testing (see Figure 5). As clearly
shown in Figure 6, there is a considerable difference between the RA values of the horizontal and
vertical tensile samples in both as-printed and hardened conditions, implying a significant anisotropy
in ductility of the component. However, the RA values of the normalized sample in the vertical
and horizontal directions are relatively close to each other, indicating a negligible anisotropy in
ductility. Therefore, normalizing treatment can be utilized as a post-printing cycle to minimize the
anisotropic behavior of the wire arc additively manufactured low-carbon low-alloy steel (ER70S-6) by
homogenizing the grain size and eliminating the inhomogeneous microstructure through the melt
pool center,
Materials fusion
2020, 13, x FORboundary, and the heat affected zone.
PEER REVIEW 10 of 13

Figure
Figure 6.
6. The
The reduction
reduction in
in area
area (RA)
(RA) for
for the
the as-printed
as-printed and
and heat-treated
heat-treated samples
samples in
in both
both vertical
vertical and
and
horizontal
horizontal directions.
directions.

4. Conclusions
4. Conclusions
This study aimed to investigate the effect of two post-printing heat treatment cycles, including
This study aimed to investigate the effect of two post-printing heat treatment cycles, including
normalizing and hardening, on the microstructure and mechanical properties of a wire arc additively
normalizing and hardening, on the microstructure and mechanical properties of a wire arc additively
manufactured low-carbon low-alloy steel (ER70S-6). The following are the key conclusions of the study:
manufactured low-carbon low-alloy steel (ER70S-6). The following are the key conclusions of the
study:
1. The dominant microstructure of the as-printed WAAM-ER70S-6 component consisted of polygonal
1. ferrite
The grains along
dominant with a smallof
microstructure volume fraction ofWAAM-ER70S-6
the as-printed lamellar pearlite formed
component at theconsisted
ferrite grain
of
boundaries. In addition, the formation of acicular ferrite and bainite constituents
polygonal ferrite grains along with a small volume fraction of lamellar pearlite formed were detected as
at the
the primary
ferrite grain phases alongIn
boundaries. theaddition,
melt pooltheboundaries.
formationFurthermore, a heatand
of acicular ferrite affected zone
bainite comprised
constituents
of coarser polygonal ferrite grains adjacent to each deposited track
were detected as the primary phases along the melt pool boundaries. Furthermore, in the previously solidified
a heat
affected zone comprised of coarser polygonal ferrite grains adjacent to each depositedinducing
bead also formed, associated with the layer-by-layer deposition nature of the process, track in
multiple
the heating
previously cycles on
solidified each
bead deposited
also formed,track.
associated with the layer-by-layer deposition nature
2. of the process, inducing multiple heating cycles
Normalizing heat treatment eliminated on each deposited
the meta-stable track.i.e., acicular ferrite and
constituents,
bainite, from the as-printed microstructure, leading to a more uniform and homogeneous
2. Normalizing heatmicrostructure
ferritic/pearlitic treatment eliminated
within thethemelt
meta-stable constituents,
pool center, i.e., acicularand
fusion boundaries, ferrite and
the heat
bainite, from the as-printed microstructure, leading to a more uniform and
affected zone. On the contrary, the hardening heat treatment altered the microstructure of the homogeneous
ferritic/pearlitic
as-printed part to microstructure
a combinationwithin the melt
of pearlite, pool
bainite, andcenter, fusion
acicular boundaries, and the heat
ferrite.
affected zone. On the contrary, the hardening heat treatment altered the microstructure of the
as-printed part to a combination of pearlite, bainite, and acicular ferrite.
3. Microhardness of the as-printed sample slightly decreased from 160 ± 7 HV to 154 ± 1 HV after
the normalizing heat treatment, while the hardening treatment could increase the microhardness
to 260 ± 3 HV.
Materials 2020, 13, 2795 11 of 13

3. Microhardness of the as-printed sample slightly decreased from 160 ± 7 HV to 154 ± 1 HV after
the normalizing heat treatment, while the hardening treatment could increase the microhardness
to 260 ± 3 HV.
4. Uniaxial tensile testing of the as-printed samples indicated a comparable tensile strength in
horizontal and vertical samples, while a considerable anisotropy in the ductility with 35 ± 2%
and 12 ± 3% of elongation, in horizontal and vertical directions, respectively, was apparent.
5. Although the hardening heat treatment could increase the tensile strength of the component by
around 20%, it intensified the anisotropy in the ductility of vertical and horizontal samples.
6. The anisotropy in ductility was minimized by normalizing heat treatment due to the removal
of the coarse grain regions in the HAZ and the resultant uniformity and homogeneity of
the microstructure.

Author Contributions: Conceptualization, A.V.N.; Funding acquisition, A.N.; Investigation, A.V.N. and M.G.;
Methodology, M.G.; Supervision, A.N.; Validation, M.G.; Visualization, A.V.N.; Writing—Original draft, A.V.N.;
Writing—Review and editing, M.G. and A.N. All authors have read and agreed to the published version of
the manuscript.
Funding: This research was funded by [Natural Sciences and Engineering Research Council of Canada (NSERC)]
grant number [RGPIN-2017-04368] and [Memorial University of Newfoundland].
Acknowledgments: The authors gratefully acknowledge the support of Natural Sciences and Engineering Research
Council of Canada (NSERC) [grant number RGPIN-2017-04368] and Memorial University of Newfoundland for
sponsoring this work.
Conflicts of Interest: The authors declare no conflict of interest.

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