Trans Indian Inst Met
Metallurgy
https://doi.org/10.1007/s12666-023-03045-6
ORIGINAL ARTICLE
Evaluation of Corrosion Resistance of as‑Sprayed WC–Co–Cr
on DH‑36 Steel with Addition of 3% GNPs
Shreyansh Shrivastava1 · Rajeev Verma1 ·
Vijay Kumar1 · Rahul Soni1 · Gaurav Saini2
Received: 18 April 2023 / Accepted: 3 July 2023
© The Indian Institute of Metals - IIM 2023
Abstract DH 36 is a naval grade steel that is widely used
in shipbuilding components and offshore due to its high
strength, durability, and usability. However, it suffers from
corrosion and slit erosion in acidic and service environments
such as sea applications. To address the above concern, a
tungsten carbide coating with and without the addition of 3%
grapheme nano-platelets is applied to DH 36 steel using the
high-velocity oxy-fuel deposition technique. After a coat-
ing has been applied, its corrosion resistance was tested by
exposing it to a 3.5% Nacl environment for 56 h at environ-
mental temperature of 35 °C and salt mist temperature of
47 °C, as per ASTM B-117, to ensure its integrity. Scanning
electron microscopy is used to investigate coating morpholo-
gies. After 8 h of corrosion study, it was determined that the
coated substrates had no corrosion sign while the DH-36
steel substrate had noticeable pits. The corrosion products
were analyzed using the XRD pattern and it was observed
that various oxides like ­WO4, ­WO3, CoO, ­W18O49, and
­FE3O4 were formed after corrosion. This reported coating
promises to outperform the pristine substrate in terms of
corrosion resistance.
Keywords DH 36 · HVOF · Tungsten carbide · Graphene
nano-particles · Corrosion
* Rajeev Verma
vermar@nitj.ac.in
1
Department of Industrial and Production Engineering, Dr
B R Ambedkar National Institute of Technology, Jalandhar,
Punjab 144027, India
2
Department of Mechanical Engineering, UIET,
Panjab University SSG Regional Centre, Hoshiarpur,
Punjab 146023, India
Materials Engineering
1 Introduction
Ships are extremely important to the global economy as
90% of all trade is conducted on the sea water [1]. Since the
maritime sector contributes so significantly to the global
economy, the materials employed in shipbuilding and related
fields are of paramount importance. In marine application,
the saline media presents a risk of corrosion; hence, the
materials used in ship construction or other marine-related
uses must be resilient enough to withstand the corrosive air
and water. Nonetheless, the necessity for the ultimate safety
and dependability makes materials in these extremely severe
marine climates and settings quite demanding. High strength
low alloy (HSLA) steels are the most common type of struc-
tural steel used for building ships, offshore structures, and
structures on land [2]. The hull and other structural parts of
ships are usually constructed from DH-36 HSLA steel [3].
Because of its properties like high strength, durability, and
capacity to tolerate sub-zero temperatures without cracking,
DH-36 steel seems an extensive application as ship construc-
tion steel [4, 5]. However, DH-36 is severely affected by
corrosion in a saline environment [6], which severely limits
its application. To enhance corrosion-resistant properties of
DH-36 steel, researchers have tried many techniques such as
applying a layer of corrosion-resistant material like AISI 308
and 304, on the exposed surface through welding or clad-
ding [7]; however, these techniques have a repercussion of
making the units heavier than necessary. The application of
cermet coatings on the exposed surface is an effective means
of preventing this unnecessary weight gain.
From past few decade, tungsten carbide (WC) coatings
are frequently used for abrasion and erosion wear resist-
ance in aerospace, automobile and other industries [8, 9].
Cobalt (Co) is used as binder in the WC coating, which also
improve its hot hardness and wear resistance [10]. Due to
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the favorable outcomes attained by WC–Co coating, they are Table 1  Operational
parameters used for HVOF Spray distance 150 mm
widely popular in industries. However, Co, the most promi-
coating deposition Powder feed rate 45 gm/min
nent binder used in WC coatings, does not improve the coat-
Oxygen Pressure 9 kg/cm2
ing’s resistance to corrosion [11]. So, to improve the cermet
Oxygen flow rate 225 slpm
coating’s corrosion resistance without having to compromise
Air pressure 5 kg/cm2
its wear qualities, various researchers have incorporated
Air flow rate 500 slpm
Cr with Co to form Co–Cr binder for WC coating so as to
LPG pressure 5 kg/cm2
increase cohesive strength of the coating and because of
LPG flow rate 45 slpm
its corrosion resistance properties [12]. The combination of
Co and Cr binders gives better corrosion resistance in harsh
condition. In view of corrosion performance of chromium,
salt spray test was carried out and result reveals that the Table 2  Specimen configuration used for experimentation
addition of Cr improves the coating’s resistance to corro- Sample Id Coating configuration
sion. Further, wear resistance of coatings is being improved
by some researchers by incorporating graphene nano-parti- Pristine DH-36 (uncoated)
cles (GNPs) and from various results it has been observed C1 WC–10Co–4Cr
that because of its particle size and high corrosion-resistant C2 WC–10Co–4Cr + 3% GNP
properties, GNPs can significantly enhance the corrosion
resistance of material [13]. Consequently, the addition of
GNP should be a better alloy to further increase corrosion 2 Experimentation
resistance in cermet coatings. Therefore, the incorporation
of GNP into cermet coatings should be beneficial to further 2.1 Materials
enhance corrosion resistance.
Thermal spray methods are commonly used coating The DH-36 HSLA steel used in this work was acquired from
technique for depositing aforesaid cermet coatings. Due to a vendor at a local market in Jalandhar, India, and the chemi-
greater particle velocities and optimum flame temperatures cal compositions of this procured DH-36 steel are 0.166% C,
produced by detonation spray coating (DSC) and high-veloc- 0.0825% Si, 0.848% Mn, 0.0521% P, 0.0170% S, 0.0122%
ity oxy-fuel spray (HVOF), these two thermal spray coating Cr and balance Fe. The sectioning of steel plate in dimen-
procedures are most commonly used for ceramic powders sion of 100 mm × 100 mm was done for coating purpose.
[14]. Out of above two coating techniques, HVOF thermal WC–10Co–4Cr powder (particle size 45 ± 15 μ) was pur-
spraying is one of the most effective technique to deposit a chased from Metallizing Equipment Co. (MEC) Pvt. Ltd in
ceramic and metallic coating because it results in a dense Jodhpur, India, and the industrial grade graphene powder
and highly adherent film with minimal porosity and oxide (diameter 5–10 μ, thickness 5–10 nm, and purity > 99%) was
content [15]. The hypersonic particle velocity in HVOF procured from shilpent, Nagpur, India.
reduces the coating time the particle spends interacting with
the atmosphere. The high kinetic energy of spray particles
in HVOF coating techniques improves the cohesiveness of 2.2 Specimen Preparation
deposited layers, which in turn reduces porosity to a mini-
mum. Further the use of LPG, a low carbon fuel, in the Before coating deposition, one face of substrate was ground
HVOF technique makes the process environment friendly. using magnetic grinding machine for removing the oxide
Based on the review of previous researches, a corrosion- layer formed on surface and for obtaining a referential flat
resistant material layer is often applied to the substrate using surface; then, the workpiece was shot blasted using alumina
welding or cladding, which includes additional weight. grit blasting particle size 80 to provide surface roughness
There are also very few studies on DH-36 that show coatings that would enhance coating adhesion. Before coating dep-
can improve a material’s corrosion resistance. Hence in this osition, WC–10Co–4Cr and 3%GNP coating powder was
experimental work, coatings of WC–10Co–4Cr are created mixed using ball milling for 30 min to obtain a homogene-
on a DH 36 steel substrate by employing the HVOF deposi- ous mixture; subsequently, powder was fed into feeder of
tion process, with and without the addition of GNPs. Fur- HVOF system. Then, coating was applied using the HVOF
ther, the corrosion resistance of deposited coatings has been method on the shot-blasted surface as parameter shown in
investigated in NaCl solution using a salt spray technique for Table 1. The specimen configuration is given in Table 2.
an extended period of time. Field emission scanning electron Field emission scanning electron microscopy (FESEM) at
microscopy (FESEM) is used to relate the coating charac- Institute Instrumentation Centre (IIC), NIT Jalandhar, was
terization and surface morphology. used to examine the coating’s morphologies.

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Trans Indian Inst Met
2.3 Micro‑hardness Test
The micro-hardness of the coated and uncoated specimens
was evaluated by Vickers micro-hardness indenter. The
hardness was measured in accordance to standard, ASTM
E384, at an applied load of 30N and dwell period of 10 s.
A minimum of three readings at substrate, coating, and
interface were taken and average of these readings has
been reported (Table 3) (Fig. 1).
2.4 Salt Spray Test
The specimen of dimensions 10 mm × 10 mm for the salt
spray test was cut from the coated sample using wire elec-
tron discharge machining (WEDM) to avoid any thermal
damage to the coating structures. Further the specimens
were polished using emery paper up to P1000. The un-
scribed specimen was then exposed to saline environment
of 3.5 wt% NaCl salt water in a salt spray testing machine
available at NIT Jalandhar (Fig. 1). Corrosion resistance
was evaluated by conducting two tests on the specimens.
Firstly by continuously exposing the specimens to salt mist
in accordance with the ASTM B-117 standard [16], the
testing environment was set at a temperature of 35 °C and
the salt mist temperature was 47 °C and specimens were
exposed to the testing environment for 56 h. Secondly by
performing cyclic salt spray test in accordance to Jiang
et al. [17] for understanding the corrosion mechanism; this
test comprises of three process wiz. wetting, drying and
transition. The cycle performed is shown in Fig. 2. This
cycle of 8 h was repeated 7 times. The weight of specimen
was measured at interval of 8 h during test 1 and after each
cycle for test 2 (Table 3).
Exhaust pipe
Compressor Salt brine inlet
Test chamber
Control panel
Pressure adjustment valve
Fig. 1  Salt spray chamber
Fig. 2  Test conditions for cyclic salt spray test
3 Results and Discussions
In this work, barrier coating of WC–10Co–4Cr and
WC–10Co–4Cr + 3%GNPs with coating thickness ranging
between 190 and 210 μm was deposited successfully on
DH-36 substrate using HVOF coating deposition technique.
The motive behind using 3% GNP for WC–10Co–4Cr coat-
ing is that experiments in past, with varying weight percent-
ages of the GNPs in WC–10Co–4Cr coating, have shown
that the coating surface has a significant amount of porosi-
ties if less than 3 wt% of GNPs are added, whereas the cohe-
sive strength of the coating decreases if more than 3 wt% of
GNPs are added; hence, 3 wt% would be optimal amount of
GNP to be used in WC–10Co–4Cr coating [13]. Figure 3
illustrates cross-sectional SEM image of WC–10Co–4Cr
coating (sample id: C1), the SEM image shows that the
thickness of deposited coating is around 204 μm with proper
interfacial bonding between coating and substrate and no
visible voids or cracks are present on the deposited coating.
The coating’s corrosion resistance was assessed by exposing
it to a saline environment in a salt spray test rig. The findings
were then analyzed using SEM images and XRD pattern.
3.1 Coating Morphologies
The SEM images of as-sprayed coatings of WC–10Co–4Cr
and WC–10Co–4Cr + 3% GNPs are shown in Fig. 4. Partially
melted splats of tungsten carbide have led to the formation
of protrusions on the surface. These partially melted splats
are formed due to the high melting point of tungsten carbide
Table 3  Micro-hardness values of uncoated and HVOF sprayed
WC + GNP specimens
Sample ID Surface Interface
Observations Average Observations Average
hardness hardness
­(HV30) ­(HV30)
Pristine 157, 145, 139 147 – –
C1 902, 849, 951.33 307, 289, 300 298.66
1103
C2 1068, 1194, 1186 303, 266, 356 308.33
1296
13

Fig. 3  Cross-sectional SEM image of WC–10Co–4Cr coating (Sam-
ple id: C1)
(WC) compared to the cobalt (Co) and chromium (Cr). Some
porosity can be seen in the coated surfaces which are formed
during the coating deposition. These porosities are the result
of difference in melting point of WC, Co, and Cr. As Cr and
Co have low melting point, at the time of solidification, they
flow down leaving gaps around the partially melted tungsten
particles. Porosity formation in WC–10Co–4Cr coating has
been reduced with GNPs reinforcement due to void filling by
GNPs, as illustrated in Fig. 4b. The reason for the reduction
in the porosity is that during solidification, Co and Cr flow
downwards and they try to pull C atoms due to the adhesive
action, due to which carbon acquires the pores and reduces
the porosity.
The protrusions on the surface will aid in the accumula-
tion of salt water sprayed on the surface during salt spray
testing. As a result, the corrosion rate will be high in areas
where salt water has accumulated, resulting in different cor-
rosion at different locations on the surface. To avoid these
issues, the coated surface was polished with emery paper
from grade P800 to grade P1200 on a rotating disk polishing
(a)
Pores
Partially melted
100 μm
splats caused
protrusions
Fig. 4  Surface morphology of as-sprayed a WC–10Co–4Cr and b WC–10Co–4Cr + 3%GNPs
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Trans Indian Inst Met
machine, resulting in a smooth surface free of pores and
protrusions, as shown in Fig. 5.
3.2 Micro‑hardness Test
The Vickers hardness value at the surface has been found to
be 147 ­HV30N for pristine substrate, 951.33 ­HV30N for C1,
and 1186 H ­ V30N for C2. In comparison to the hardness of
bare substrate, hardness of C1 and C2 are observed to be
6.47 and 8.06 times higher, respectively. The high hardness
value is attributed to the presence of harder phase of tung-
sten and carbide, additionally; the incorporation of GNPs
fills the porous structure during solidification resulting a
dense coating which increases the hardness. However, it is
observed that the hardness decreases gradually while mov-
ing toward the substrate. At the coating-substrate interface,
the micro-hardness value obtained is 298.66 ­HV30N and
308.33 ­HV30N for C1 and C2, respectively.
3.3 Salt Spray Test
3.3.1 Continuous Exposure Test
Visual inspection of the specimens was done at an inter-
val of 8 h during the testing. It has been seen that the red
rust on the base metals is observed at the first inspection,
i.e., after the 8 h of exposure in salt solution whereas for C1
(WC–10Co–4Cr) specimen, the red rust is visible after 40 h
and for C3 (WC–10Co–4Cr + 3% GNPs) specimen the rust is
visible after 56 h. Upon visual inspection, it is clear that the
WC–10Co–4Cr coating has delayed the start of corrosion and
WC–10Co–4Cr + 3% GNPs coating has delayed the corrosion
even more.
After 56 h of salt spray testing, corroded surface was ultra-
sonically cleaned with ethanol to remove loose particles cre-
ated by pitting corrosion. Subsequently, the specimens were
dried at 50 °C for 20 min to remove moisture. After drying, the
(b)
Pores
100μm
Trans Indian Inst Met

Fig. 5  Surface morphologies of polished specimens before salt spray testing a Uncoated surface, b WC–10Co–4Cr coating and c WC–10Co–
4Cr + 3%GNPs

SEM image of pristine (shown in Fig. 6) and coated surfaces
C1 & C2 (refer Fig. 7) were taken to view the pits formation
due to long time contact in corrosive environment, moreover
the weight loss of each specimen was obtained to calculate the
corrosion rate. The weight loss has been found to be 0.14031 g,
0.07990 g, and 0.03810 g for pristine (DH-36 steel), C1
(WC–10Co–4Cr coating), and C2 (WC–10Co–4Cr + 3% GNPs
coating), respectively. The corrosion rate in mm/year has been
calculated by using formula [18],

Pitting Corrosion Area 2

Area 1

Passivation Layer

Area 2
Area 1
200μm

Fig. 6  SEM image of base material DH-36 after 56 h of salt spray test and EDS plots

13

(a) Corrosion Pits
200μm
Fig. 7  SEM image of the coated surface at the end of 56 h of salt spray test a WC–10Co–4Cr and b WC–10Co–4Cr + 3%GNPs
mm cm3
CR = k × weight loss, g ×
year Alloy density, g
1 1
× 2
× coating, very fine oxide layer is formed and small pits are
exposed area, cm exposed time, h
Here, k is constant and attains value 8.76 × ­104 for cor-
rosion rate to be in mm/year. Upon calculation, the corro-
sion rate is found to be 27.96 mm/year, 8.95 mm/year, and
4.38 mm/year for pristine, C1, and C2, respectively. The
SEM image and corrosion product formation at different
locations of bare pristine substrate is shown in Fig. 6. From
the figure, it has been seen that an oxide layer is obtained
on the surface of material due to the reaction of salt water
with the metal. This layer is mainly containing ferrous oxide
which acts as the protective layer for material against fur-
ther degradation against salt water [19], and this layer is
known as passive layer. With time the thickness of this layer
increases, however, after a certain thickness of this ferrous
oxide layer, cracks are generated and start increasing with
testing time. As the cracks grow, the ferrous oxide layer
starts to break down; this disintegration of the passive layer
was given by Vetter and Strehblow [20]. Due to the break-
down of passive layer, base material which was protected
by ferrous oxide layer is exposed to the NaCl medium and
pits are formed on the exposed surface thus initiating pitting
corrosion (Fig. 6). The galvanic cell formed during corro-
sion compressive of pits formed act as anode and metal act
as cathode which leads to migration of anions toward pits
and results into local production of metal cations [21]. These
metal cations create excessive positive charge which attracts
chlorine ions and forms ferrous chloride which in turn reacts
with the moisture in environment to form HCl which accel-
erates the corrosion rate.
The SEM image of the cor roded surface of
WC–10Co–4Cr and WC–10Co–4Cr + 3%GNPs is depicted
in Fig. 7. The corrosion mechanism similar to that of pristine
13
Trans Indian Inst Met
(b)
Pits
200μm
steel is seen on the coated specimens also but due to the
presence of a coating on both specimens, the NaCl solu-
tion did not react with the base metal. In WC–10Co–4Cr
observed on the surface at the end of 56 h of testing; this
indicates that the corrosion of the metal has been delayed
by the deposition of WC–10Co–4Cr coating. Further on the
WC–10Co–4Cr + 3%GNP coated specimen, very minute pits
are observed compared to that formed on the WC–10Co–4Cr
coating. The literature says that due to presence of single
layer of carbon atoms linked together in a hexagonal struc-
ture and high surface area, graphene should have high cor-
rosion resistance [22]. The results obtained indicates that the
corrosion on DH-36 steel has been delayed by the deposition
of WC-based cermet coating, and the further addition of
GNPs in the cermet coating has shown positive results by
further increasing the corrosion-resistant properties of the
material.
3.3.2 Cyclic Corrosion Test
Corroded surfaces were ultrasonically cleaned with etha-
nol to remove corroded particles after salt spray testing
for 56 h (7 cycles). After that, moisture was removed from
the samples by drying them at 50 °C for 20 min. Figures 8
and 9 shows the SEM image of corroded surfaces of base
metal and coated samples (C1 andC2), respectively, at
the end of 7 cycles. From Fig. 8, it has been seen that the
ferrous oxide layer formed on the corroded surface is still
present on the surface but some cracks has formed on this
oxide layer which degrades the protective nature of the
layer, which indicates the film breaking mechanism of
pitting corrosion. On continuing the test, the salt water
will propagate into these cracks and will form a galvanic
cell at the interface of base metal and oxide layer thus
promoting the pitting corrosion which will eventually peel
Trans Indian Inst Met
Passivation Layer
Area 1
Area 2
Cracks
200μm
Fig. 8  SEM image of base material DH-36 after 56 h cyclic salt spray test and EDS plots
(a)
Corrosion Pits
200μm
Fig. 9  SEM image of the coated surface at the end of 56 h of cyclic salt spray test a WC–10Co–4Cr and b WC–10Co–4Cr + 3%GNPs
off the oxide layer and expose the fresh metal surface to
the saline environment.
Figure 9a shows the SEM image of WC–10Co–4Cr
coated surface after 56 h of the cyclic salt spray test. Few
corrosion pits are visible on the coated surface which indi-
cates the start of corrosion on the exposed surface. But these
pits are visible at few discrete spots and not much damage
due to corrosion is observed on the coated surface. Figure 9b
indicates the SEM image of WC–10Co–4Cr + 3%GNPs
coated specimen after 56 h of cyclic salt spray test, and no
evidence of corrosion is visible in the image. This test also
align with the literature that GNPs increase the corrosion
resistance of the material. From the cyclic salt spray test, we
can conclude that the WC–10Co–4Cr coating increase the
corrosion-resistant properties of the DH-36 steel and addi-
tion of GNPs further enhances this property.
Area 1
Area 2
(b)
200μm
3.4 XRD Analysis
The compounds formed on the corroded samples were
investigated using the PAnalytical Empyrean XRD and
the XRD patterns obtained were analyzed using High-
Score software. Figure 10 shows the XRD pattern of
bare substrate (pristine), and WC–10Co–4Cr (C1) and
WC–10Co–4Cr + 3%GNPs (C2) coatings before and after
the conduct of cyclic salt spray testing. The XRD pattern
shows that there is change in phase of the compounds after
the testing. The figure illustrates that for pristine sample
after the corrosion, a throughout peak of iron (II, III) oxide
­(Fe3O4) is present on the surface which is particularly due
to the formation of oxides in NaCl solution. The through-
out oxide peak is observed because oxide layer formed is
present intact on the surface of the base as seen from the
SEM image (Fig. 8). Whereas on coated specimens, due
to the high percentage of WC in feedstock powder, the
major phase observed is of WC and minor phase of CoCr.
During the coating deposition due to decarburization of
13

Fig. 10  XRD pattern of a C2 coating (WC–10Co–4Cr + 3% GNPs), b C1 coating (WC–10Co–4Cr) and c uncoated (DH-36 steel) specimens
WC or due to the disappearance of CoCr phase (as a result
of high cooling rate of semi-molted feedstock powder),
a new phase of W ­ 2C has formed [23]. In as-sprayed C1
coating, the observed phases are WC (hexagonal) and
­Co3Cr (cubic), while after the corrosion test, ­Co3Cr has
disappeared and instead ­WO4 (orthorhombic) and ­CoCr2
(cubic) phases has been identified. In as-sprayed C2 coat-
ing, WC (hexagonal), CoCr (tetragonal) and ­W2C (hex-
agonal) phases are observed, and after corrosion, W ­ O3
(tetragonal), ­Co2Cr3 (tetragonal) phases are formed. The
XRD pattern of corroded C2 sample shows that due to
the reinforcement of GNPs, very tiny peaks of oxides are
observed which shows that the corrosion rate in C2 speci-
men is reduced to a great extent. Further small traces of
various other oxides like CoO, ­CoCr2O4 and ­W18O49, are
also observed which may have formed as reaction product
of the corrosion test.
4 Conclusion
From the coating investigation on DH-36 steel, the following
conclusions has been drawn.
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• Very few micro-voids and corrosion pits have been
observed on WC-10C0-4Cr coating compared to bare
substrate.
• The corrosion resistance of WC–10Co–4Cr coating is
further increased by reinforcement of graphene nano-
platelets.
• From XRD patterns, it has been observed that various
oxides like W
­ O4, ­WO3, CoO, C ­ oCr2O4 and W
­ 18O49 have
been formed as the reaction product of the corrosion test
in coated specimens, while the corroded surface of the
base has an oxide layer of ­Fe3O4.
Declarations
Conflict of interest This research did not receive any specific grant
from funding agencies in the public, commercial, or not-for-profit sec-
tors.
Trans Indian Inst Met

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