Materials Today: Proceedings 49 (2022) 2000–2006

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Tensile behavior of pre-stress corroded and post hydrogen embrittled

spring steel
Basukumar H.K. a,⇑, Arun K.V. b
a
Depatment of Mechanical Engineering, KLE Institute of Technology, Hubballi 580027, Karnataka, India
b
Department of Mechanical Engineering, Government College of Engineering, Haveri 581110, Karnataka, India

a r t i c l e i n f o a b s t r a c t

Article history: Stress Corrosion Cracking (SCC) and Hydrogen Embrittlement (HE) are two major degradation phenom-
Received 13 June 2021 ena experienced by spring steel. The consequences of these phenomena have an impact both on the
Received in revised form 15 August 2021 mechanic response, sufficiency, and life of the mechanical system. The susceptibility to premature failure
Accepted 19 August 2021
is never the same and is unique for different environment combinations. There will be a combined effect
Available online 31 August 2021
of these phenomena. Here in this experimental investigation, an attempt is made to understand the ten-
sile behavior of combined treatment. The pre-stressed specimens were corroded and post-treated with
Keywords:
the HE process. Traditional tensile testing was used to investigate the combined effect of corrosion and
Tensile loading
SCC
post-treated HE. From the test results, it can interfere that the post hydrogen charged specimen exhibits
HE ductility loss, but recover in the ultimate strength, and increase in yield strength. The dominance of
Anodic dissolution recovery was also shown by an increase in fracture strength and toughness. The scanning electron micro-
Crack closure scope was used to assess the mechanism and to characterize it.
Fractography Ó 2021 Elsevier Ltd. All rights reserved.
Selection and Peer-review under responsibility of the scientific committee of the Global Conference on
Recent Advances in Sustainable Materials 2021.

1. Introduction works have been carried out to understand the failure mecha-
nisms. The various mechanism by which Environmental assisted
Corrosion of steel is one of the main degradation problems in cracking occurs like anodic dissolution, film rupture during general
the industrialized world. In many service conditions, where the corrosion, hydrogen influenced hydrogen enhanced assisted crack-
prevailing stresses are combined with a corrosive environment, ing or adsorption-induced dislocation is still debated in engineer-
the degradation phenomena intensify. There is considerable inter- ing alloys, particularly for different material and service
est in material degradation at present, which is partly responsible environment combinations [3–5]. The deleterious interaction of
for failures and shortening of the service life of the mechanical sys- the operating environment and mechanical loads influences the
tem. Material degradation affects the performance of many indus- performance and life of engineering alloys. Even though structural
trial engineering steel components due to exposure to in-service steel alloys were selected and intended for long-term use, they fail
conditions. Material degradation affects the performance of many due to various factors such as overuse, overloading, an unfavorable
industrial engineering steel components due to exposure to in- oxidative, corrosive environment, residual strains, and poor main-
service conditions such as overloading, overutilization, corrosive tenance. The components, which are subjected to deleterious aque-
environment, and improper maintenance. The consequences of ous conditions, lead to corrosion and subsequently decrease the
these in-service conditions lead to fatigue, corrosion, and wear life and load capacity. Spring steel is one of the widely used carbon
damage, are of considerable technological significance. Materials steel in the industrial world because of its properties such as
degradation problems are in particular important in naval, petro- toughness, strength & hardness. Under extreme service conditions,
chemical; energy generation, and conversion industries, including EN47 spring steel will undergo two major phenomena Stress corro-
nuclear [1,2]. In response to these challenges, extensive research sion cracking (SCC) and hydrogen embrittlement (HE). This con-
ceptualization raises the scope for the investigation of the failure
behavior of spring steel. The integrity of the material relies on
⇑ Corresponding author. the material behavior under complex service conditions such as a
E-mail address: [email protected] (H.K. Basukumar). high rate of loading, environmental conditions, and material. The

https://doi.org/10.1016/j.matpr.2021.08.156
2214-7853/Ó 2021 Elsevier Ltd. All rights reserved.
Selection and Peer-review under responsibility of the scientific committee of the Global Conference on Recent Advances in Sustainable Materials 2021.
H.K. Basukumar and K.V. Arun Materials Today: Proceedings 49 (2022) 2000–2006

Table 1
Chemical composition of test specimen material EN47/SAE6510.

Composition % Carbon Silicon Manganese Phosphorous Sulphur Chromium Vanadium

0.451 0.247 0.660 0.018 0.010 1.0 0.155

consequence of conjunction action of the escorts environmentally utes exposure. The nitric acid exhibits the most aggressive corro-
induced crack initiation and propagation results in impulsive fail- sive nature in most of the metal, especially in steel. Therefore,
ure [6–8]. nitric acid is considered for the simulated laboratory condition.
A comparative study of tensile behavior of EN47 spring steel, The nitric acid with 20–22% concentration is used for passivation
over the corrosion environments, has been examined. The conjoint below and beyond which acts as a corrosive media. This typical
action of loading rate, corrosive environment, and material leads to solution exhibits corrosion behavior by anodic dissolution, which
a sudden and catastrophic failure. The term SCC is used to describe is one of the mechanisms for SCC, a cracking phenomenon caused
service failures in engineering materials that occur under the influ- by the combined effect of tensile stress and a corrosive environ-
ence of slow environmentally induced crack and its propagation as ment. In the laboratory experiment, stress-corrosion cracking of
a consequence of the working stress. This can lead to unexpected low-carbon steels occurs in specimens, which experience some
sudden failure of normally in ductile material subjected to tensile plastic deformation due to applied working stresses. As a necessary
stress. SCC is selective and specific to a certain chemical environ- condition, an initial plastic deformation was induced (about 70
ment. The specific environments along with very small concentra- percent of the ultimate stress) by pre-stressing the samples. In a
tions of certain highly active chemicals are needed to produce simulated corrosion environment, these pre-stressed specimens
stress corrosion cracking, often leading to devastating and unex- were subjected to general corrosion before being put through a
pected failure [9,10]. Hydrogen damages are one of the most com- tensile test until the final fracture. Defects caused by corrosion spe-
plex occurrences as material failure compares to the other type of cies will act as stress raisers and cause catastrophic failure when
failure in the hydrogen nonexistence. This type of material degra- combined with the applied working load.
dation is the result of various unknown physical and chemical
kinetics. Hence the study of HE of steels is a particularly significant
issue in many industrial applications, since a fully developed and 2.2.2. Post hydrogen embrittlement
practically applicable predictive physical mechanism-model, still The specimens were submerged in a 35 percent aqueous solu-
does not exist [11,12]. HE is one of the common degradation pro- tion of ammonium thiocyanate at room temperature for 120 hours
cesses which can happen in a room or slightly above room temper- for hydrogen charging. The test solution was replaced with fresh
ature with or without applied stress. Unfortunately, just solution every 48 hours. The test solution for the immersion test
determining that a failure is due to HE or SCC is seldom lending was prepared by diluting with distilled water to concentration of
a hand to the customer unless that determination is put together 35%w/vol at room temperature. The laboratory immersion experi-
with references that provide some ways to avoid such damage in ments were carried out in compliance with ASTM guidelines. By
future applications [13]. The combined effect of corrosion caused immersing the pre-stressed corroded specimens in hydrogen, a tra-
by dissolution and embrittlement caused by a cathodic reaction ditional laboratory immersion approach was used to charge hydro-
can still cause the unexpected failure of relevant materials. The gen. The experimental study involves mechanical testing of stress
susceptibility of spring steel to stress corrosion and embrittlement
was studied simultaneously. The overall corrosion process in
spring steel under the influence of pre-stress condition, as well
as post-hydrogen embrittlement (SHE), were studied to investigate
the failure mechanism of spring steel.

2. Material and methods

2.1. Material

Spring steel is one of the major engineering materials used in

the automotive industries along with other engineering applica-
tions. One of spring steel designated as EN 47, is widely used in
the automobile, aviation, and aerospace industries. Applications
include gears, crankshafts, and other machine parts such as wash-
ers, saw blades, springs, and railway wheels and tracks. It is
medium-low alloy carbon steel (EN47/AISI 6150/SUP 10) which
is suitable for overall engineering applications with higher
strength. The compositions of the material procured have been
chemically analyzed and are listed in Table 1.

2.2. Methods

2.2.1. Stress corrosion cracking

General corrosion of the specimen was simulated in the labora-
tory by immersion technique. The specimens were corroded with
HNO3 of 35% concentration solution by immersion for about 5 min- Fig. 1. Typical Experimental setup for immersion test.

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H.K. Basukumar and K.V. Arun Materials Today: Proceedings 49 (2022) 2000–2006

of service load and environmental factors will affect crack growth

influencing impulsive failure. It is understood from various
research works, that the anodic dissolution changes the crack
shape and thus the crack tip radius. This may result in crack tip
blunting which can affect the SCC resistance of the material [14].
The general corrosion occurs due to anodic dissolution and HE
through cathodic reaction. Depending on the environment, cracks
from HE may also reveal corrosion products on a fracture surface
[15]. In hydrogen embrittlement, hydrogen is a by-product of the
cathodic reaction, the initial corrosion may occur but the rate of
corrosion is negligible as compared to the general corrosion pro-
Fig. 2. Tensile Specimen Dimensions. cess [12,16]. Cracks are caused by exposure to corrosive environ-
ments, and if they are allowed to propagate, they can cause
major and even catastrophic failures. In the case of stress-
corrosion, the toughness is likely due to initial hardening caused
by chemical interactions in the environment, which results in
delayed cracking and greater elongation. The susceptibility of SCC
and HE was discerned by the decrease in the mechanical properties
of treated test material as compared to untreated test specimens at
the same strain rate. The combined effect of pre-stress, chemical
damage due to corrosion, and the presence of the nonuniformities
in the metal structure, shallow wide mouth open dense cracks are
generated. During the embrittlement process, the wide mouth
cracks were squeezed out, some cracks were healed, and some
cracks were narrowed with a blunted crack tip. This hydrogen
environment embrittled process zone leads to damage that occurs
when the local stress exceeds the threshold level. Depending upon
the corrosion species present at the crack tip, the tip gets blunted
or sharpens. The blunting of the crack tip delays the crack growth
Fig. 3. Standard Tensile specimen; a) Untreated b) stress corroded c) pre stress resulting in the delayed fracture. The cracks which are susceptible
corroded, Post Hydrogen Embrittled. to the triaxial stresses lead to rapid crack growth leads to catas-
trophic failure. The chemical and electrochemical conditions at/
near the crack mouth and crack tip determine the crack initiation
corroded post hydrogen charged (SHE) and characterization of the and their growth. The anodic dissolution leads to the general cor-
SHE specimens at the micro- and macro-level using Scanning elec- rosion of metal. This corrosion forms a cluster of dense and wide
tron microscope observations of the failed specimen. Fig. 1 illus- cracks. These pre-SCC cracks when exposed to embrittle process
trates a typical test setup. by virtue of embrittlement, the crack fronts experience a pull,
and crack tip occludes. The blunt, wide cracks turn into narrow
2.3. Test specimens sharp cracks. The plastic zone at the crack tip leads to a delay in
the crack growth. The applied load will have to accommodate
Round cylindrical specimens (110 mm overall length, 30 mm and overcome from the plastic zone, before further crack growth
gauge length, and 6 mm diameter) were machined from bars of and final failure. This can be witnessed with the stress-strain curve
Alloy EN47 in such a way that the gage length to the diameter (l/ of a post-treated embrittled specimen. The mechanical properties
d) ratio of these specimens was maintained at 5 according to the were regained by this post-treatment justifying the above-
ASTM E8. All samples were machined to have the same dimen- mentioned statement, however, this needs further investigations.
sions. The test specimens used in tensile testing with the dimen- The prestressed surface affects the hydrogen uptake because they
sions are shown in Figs. 2 and 3. All the tensile testing has been offer lower energy sites in the surface and subsurface region. The
carried out in a universal testing machine (UTM) of 50kN capacity small addition of metal or oxide particles change the uptake kinet-
at room temperature. The crosshead velocity of 0.3 mm/min was ics [17].
maintained for all test specimens. Before the tests were carried The stress corrosion cracking behavior of the spring steel is
out, a metallographic finish was obtained by polishing the speci- influenced by crack tip blunting due to anodic dissolution. The
mens with 420 grit papers. The tensile tests are performed on stress corrosion-induced pits might act as a stress concentrator.
cylindrical specimens before and after being exposed to different HE and SCC differ by the interactions of the specimen. The SCC
chemical environments to experience general corrosion and HE. can be influenced by the cathodic reactions that influence the crack
In laboratory investigations, the specimens were pre-stressed growth mechanism [15]. The post hydrogen charging destabilizes
beyond their yield stress to experience a plastic deformation the passive film formed and hydrogen entry to blunt crack tip
(70% of rult). These pre-stressed specimens were subjected to gen- due to cathodic reaction [18]. As discussed in this Section, a tensile
eral corrosion and post hydrogen charging in a simulated aqueous load on a pre-stressed specimen causes crack opening. The crack
media. To study the behaviour of the treated material in tension, tip experiences plastic deformation. The corrosion species form
samples as shown in Fig. 3 were tested in a UTM till complete on the fractured surface as a result of environmental conditions,
failure. deposits on crack faces, which induces the compressive stress,
which will assist in crack closure under compression and a plastic
3. Results and discussion zone will form. Even though there’s small-scale yielding, the plastic
zone is plastically elongated and becomes longer than it had been
In most engineering industries, the effective life of the material before. Therefore, the zone experiences a compressive load due to
is recognized by yielding, not by fracture. The complex interaction embrittlement, and reversed plasticity occurs when the tensile
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H.K. Basukumar and K.V. Arun Materials Today: Proceedings 49 (2022) 2000–2006

load is applied. As a result, plasticity occurs ahead of the crack tip that the material was able to withstand a greater load before
and crack grows through the plastic zone during tensile load before deforming. The chemical reaction at the surface has caused work
final failure. hardening. The uniaxial tensile properties of the treated and
untreated EN 47 steel specimens were represented graphically in
Fig. 5a and 5b. As schematically illustrated in Fig. 5, the yield
3.1. Stress/strain behavior of treated and untreated material
strength was higher in both the treated specimens. Higher strength
means an increase in hardness and lesser deformation. The excep-
Fig. 4 depicts a typical tensile curve in terms of engineering
tion to this, in the stress-corroded specimen test, the yield and
stress–strain variations with engineering strain in a simulated cor-
elongation both increased indicating the formation of the shear
rosive environment at a nominal strain rate of 0.3 mm/minute. The
band. A higher strength means increase in the hardness and lesser
tensile properties such as the yield strength, ultimate strength
deformation. Exception to this, during stress corrosion process the
were obtained. The ductility parameters such as the percentage
yield and elongation both increased indicating towards intense
of elongation and the area reduction of treated EN47 samples were
shearing strain. After post hydrogen treatment, the yield strength
evaluated at ambient temperature. The engineering stress–strain
of the specimen increase with a decrease in the percentage elonga-
curves of the EN47 spring steel Untreated, stress corroded, Pre-
tion pointing towards the recovery of the material properties of an
stress corroded post HE (SHE) are presented in Fig. 4. Typically,
untreated specimen, the same can be substantiated in the stress–
the corrosive environment affects the engineering tensile curve.
strain curve behavior. The behavior of stress–strain curves reveals
The untreated specimen had yield strength of 385 MPa, a 26 per-
a certain work hardening has taken place in the SCC test specimen
cent elongation, and an ultimate strength of 650 MPa . The SCC
by virtue of process which can be depicted as a decrease in UTS.
behavior of the test specimen yields results of 416 MPa and ulti-
The increase in both yield strength and percentage elongation;
mate strength of 506 MPa. The yield strength (YS) and ultimate
decrease in ultimate strength substantiate chemical reaction and
tensile strength (UTS) of the SHE sample were found to be
failure due to stress corrosion cracking. Further, the increase in
434 MPa and 585 MPa, respectively. In comparison with the
yield strength and decrease in percentage elongation indicates loss
untreated specimen, the yield strength was increased by 13 per-
of ductility pointing towards the effect of HE. The curve of the post
cent and the UTS decreased by 10 percent. The elongation was
hydrogen charged material indicates that it had become harder,
increased by 37 percent in stress corroded specimens and 17 per-
revealing embrittlement; that is can withstand far higher loads
cent in post-HE specimens. The increase in yield strength indicates
before they deform. There is a small increment in the load-
carrying capacity which is indicated by an increase in the ultimate
strength of the SHE specimen compared to the SCC specimen. The
stress–strain curve in Fig. 4 corroborates the recovery process that
occurred due to the post-HE process. This further shows the recov-
ery of plastic deformation, leading to an increase in toughness.

3.2. Macro and micro-mechanism failure analysis

Initially, the fracture mechanisms are exemplified macroscopi-

cally by the surface morphology of the fracture. The scanning elec-
tron microscope was used to assess the failure mechanism and to
characterize it. The macroscopic observation of the fractured sur-
face revealed a preliminary failure mechanism.

3.2.1. Macro mechanism failure analysis

The tensile fracture surfaces of the untreated sample are shown
in Fig. 6(a). The fractured surface of the untreated specimen exhib-
ited a brittle failure with less plastic deformation. The shear band
formed due to the localized deformation was small that is the elas-
tic deformation of steel is relatively small. Fig. 6(a) depicts an
Fig. 4. Stress/strain behavior of untreated and treated specimen. untreated fracture surface, and the radial fanlike marks clearly

Fig. 5. Mechanical Properties of tensile test untreated SCC and SHE treated specimens of EN 47; (a) % elongation and yield strength, (b)) % elongation and Ultimate strength.

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H.K. Basukumar and K.V. Arun Materials Today: Proceedings 49 (2022) 2000–2006

show that the fracture origin is at the point indicated by the arrow. 3.2.2. Micro-mechanism failure analysis
The flat fracture surface indicates that the stress that caused the During slow strain rate tensile load failure, the formation of the
failure was tension, as there is no shear lip. The absence of a shear void, coalescence of voids, initiation of crack, crack, and rapid fail-
lip indicates that the fracture began at a free surface. The lack of ure has occurred in the untreated specimen. The formation of mul-
deformation indicates that the fracture is primarily brittle. The tiple cracks, at the circumference act as triggering site, will
radial lines are attributed to the direction of crack growth penetrate the material at a rapid speed; finally, fail as bulk shearing
upstream. The fracture surface is approximately normal to the of the material. The pre-crack originated by the virtue of the stress
applied tensile loading direction, and a shear lip is present around corrosion, are more and dense on the circumference of the material
the fracture. The fracture surface of the untreated specimen reveals as compare to untreated, but the depth of these dense cluster
a typical cup and cone morphology, which is reminiscent of glob- cracks are very less. The fracture facet of the untreated specimen
ally ductile failure; Macro brittle changing to macro ductile with (Fig. 6a) reveals elongated fracture whereas pre-stressed brittle
loss of constraint. This indicates a possible site for fracture initia- failure for treated specimen surfaces. Untreated specimens have
tion, as well as a bright central region and shear lips formed during a flat fracture surface with shallow radial marks associated with
the final stages of the fracture process. The fracture surfaces appear a cleavage mechanism, whereas the bright fibrous center region
brittle-ductile as a mixed-mode. There was a uniform distribution has dimples associated with a nucleation-growth-coalescence
of cracks around the circumference of the SCC specimen. These mechanism. The microstructure of the stress corroded specimen
were induced and originated by the virtue of the process. The uni- (Fig. 6b) shows pre-existing cracks that resulted in a mixed mode
form shear band formation can be seen on the fractured surface. of brittle and ductile cracking inferred by the presence of cleavage
There was a less and uneven distribution of cracks was observed and micro void coalescence at the microscale, as evidenced by the
on the circumference of the post-HE treated specimen as shown presence of shear lips. The macro and micrograph images show
in Fig. 7(a). Careful observation reveals of the gouge, possible crack that the central region is the result of void nucleation, their growth,
initiation site formed due to the corrosion phenomenon whereas and coalescence process; while the surface observed a formation of
closed crack on the surface formed due to embrittlement. Shiny the shear lip zone shows elongated dimples in the radial direction.
Fracture surface indicates cleavage likely failure whereas the rough Hence, it is presumed that, because of the decohesive process, a
matte surface stipulates ductile failure. quasi-brittle fracture failure occurred. This failure suggests that

Fig. 6. a) Macro and micrographs of Fractured Untreated Tensile Specimen; b) Macro and micrographs of Fractured stress corroded Tensile Specimen;

Fig. 7. Macro and micrographs of fractured pre-stress corroded post hydrogen embrittled Tensile Specimen; a) flat fractured surface b) Overall Micrograph of fractured
surface; c) Magnified image near the surface.

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H.K. Basukumar and K.V. Arun Materials Today: Proceedings 49 (2022) 2000–2006

the mechanism of plastic deformation localization induced by ano-  The SCC behaviour of the spring steel is influenced by crack tip
dic dissolution was dominant in the SCC. The SCC behavior of the blunting due to anodic dissolution and because of decohesive
spring steel is influenced by crack tip blunting due to anodic disso- process, a quasi-brittle fracture takes place, which indicates,
lution. Well-documented literature enumerate crack closure the mechanism of localized plastic deformation induced by ano-
mechanism have a significant effect on the threshold behavior, dic dissolution.
especially in fatigue failures. With reference to the available infor-  The effect of simulated chemical treatments of pre stress corro-
mation, the crack closure can be related to environmentally sion and post HE was noticed in-terms of change in yield
induced closure resulting from the corrosion product [19]. In this strength, ultimate strength and ductility under the influence
case, due to post hydrogen charging, the deposit also acts like a of tensile load. The stress-strain curve corroborate the recovery
trap allowing corrosive elements to enter but not to leave, leading process occurred due to post HE process. This further shows
to stationary propagation process of an external surface to the cre- recovery of plastic deformation, leading increase in toughness.
vice, anodic dissolution, internal cathodic reactions, and repassiva-  Although recovery in the mechanical properties, there is mate-
tion [8,20]. The fracture surface in Fig. 7 (a) presents a nearly flat, rial degradation phenomenon involving overall loss of material
identifying as a macroscopically brittle failure, however, the which will affect the service life.
appearance of the microstructure stays quasi-brittle (Fig. 7c).
Microstructural examination shows a course ridged pattern, with
a reduction in area and a fibrous zone. A ridge pattern is visible
Declaration of Competing Interest
on the fracture surface of a material that shows limited ductility
during fracture. The dotted circle represents the fibrous zone of
The authors declare that they have no known competing finan-
overload fracture; finally, in the treated specimen the ridge pattern
cial interests or personal relationships that could have appeared
has disappeared, the reduction in area is large, and the fracture
to influence the work reported in this paper.
surface consists of a central fibrous region and a smaller shear
zone. Fig. 7(b) depicts the fracture morphologies of specimens at
the failure area. On the fracture surface, there are signs of cleavage Acknowledgements
facets and ductile tearing. The distinctive fracture features, inter-
granular cracking characterized by cleavage and river pattern, All persons who have made substantial contributions to the
and microvoid coalescence during ductile failure were observed. work reported in the manuscript (e.g., technical help, writing and
Base on careful analysis of fracture surface images in Fig. 7c, the editing assistance, general support), but who do not meet the cri-
shear lips are indicated by the dark grey shaded area at the speci- teria for authorship, are named in the Acknowledgements and have
men’s extreme surface. By virtue of the applied load, in the mid- given us their written permission to be named. If we have not
region of the fracture surface, the treated specimen has ductile nat- included an Acknowledgements, then that indicates that we have
ure of failure with deep and uniformly distributed dimples as seen not received substantial contributions from non-authors.
in the typical untreated specimen. The increase in the yield
strength of the treated specimen maybe because of the solution
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