An Industrial Perspective on Environmentally Assisted Cracking of Some Commercially Used Carbon Steels and Corrosion-Resistant Alloys
An Industrial Perspective on Environmentally Assisted Cracking of Some Commercially Used Carbon Steels and Corrosion- Resistant Alloys
Commercial metals and alloys like carbon steels, stainless steels, and nickelbased super alloys frequently encounter the problem of environmentally assisted cracking (EAC) and resulting failure in engineering components. This article aims to provide a perspective on three critical industrial applications having EAC issues: (1) corrosion and cracking of carbon steels in automotive applications, (2) EAC of iron- and nickel-based alloys in salt production and processing, and (3) EAC of iron- and nickel-based alloys in supercritical water. The review focuses on current industrial-level understanding with respect to corrosion fatigue, hydrogen-assisted cracking, or stress corrosion cracking, as well as the dominant factors affecting crack initiation and propagation. Furthermore, some ongoing industrial studies and directions of future research are also discussed.
YUGO ASHIDA,1,3 YUZO DAIGO,2,4 and KATSUO SUGAHARA2,5
Environmentally assisted cracking (EAC) is one of
the most common causes of failure in structures and
components. For decades, the mechanisms of EAC
have been intensively and extensively studied in
chemical processing, in the oil and gas industry, and
in nuclear power generation.1,2 Having a better
understanding of EAC is vital for product life design
or life extension across industry sectors. This article
discusses on the EAC problem of some commercially
used metals and alloys. It is especially focused on
lowcost carbon steels (CS) and low-alloy steels (LAS) used
for the automotive industry, and corrosion-resistant
Fe-Cr-Ni alloys, such as stainless steels and Ni-based
alloys used in a salt production environment and in a
supercritical water environment. The purpose of this
review is to prevent or mitigate the risk of EAC by
raising awareness of the failure mode and the
susceptible regime in these industrial applications.
Table I shows the EAC problems of each
industrial application described in this article.
The information includes materials, the working
environment, the corrosion type/cracking mode, the
current industrial-level understanding of the root
cause, controlling factors affecting the susceptibility
to cracking, experimental approaches, and research
efforts within each industry. In the following, we
describe the EAC phenomena in the aforementioned
industrial applications in three topical themes
(categorized by application area).
CORROSION AND CRACKING OF CARBON
STEELS IN AUTOMOTIVE APPLICATIONS
Low-cost carbon steels are used for automotive
components, construction structures, bridges, and
many other structures associated with daily life. A
World Steel Association estimate shows that the
automotive sector consumes roughly 12% of the
overall steels in the world.3 On average, 900 kg of
steel is used per vehicle, including 12% of
highstrength carbon steels in the suspension.4 The
corrosion of carbon steels caused by road salts and
emissions was a serious problem during the early
years of automotive development.5 In recent years,
the corrosion and cracking problem was
significantly improved through the advancement of
coating technologies.5 Nevertheless, problems of
localized corrosion, corrosion fatigue, and
LC localized corrosion, CF corrosion fatigue, HAC hydrogen assisted cracking, SCC stress corrosion cracking, SST salt spray test, CCT
cyclic corrosion test.aTypical industry sectors as described in this article.bIndustrial metals prices and charts (https://www.quandl.com/
collections/markets/industrial-metals, accessed on 10-28-2016).
hydrogen-assisted cracking in automotive
components remain unsolved. The following section shows
the typical case of automotive suspension coil
Coating and Coating Damage Caused
Corrosion and Cracking of Coil Springs
Carbon steels or low-alloy steels with
pretreatment and resin powder coatings are being used for
the production of coil springs, taking into account
the balance between mechanical properties and the
cost of materials and manufacturing. As shown in
Fig. 1, the cross section of a coil spring wire consists
of a metal substrate, a shot peened surface layer, a
zinc phosphate (ZnP) pretreatment layer, and an
organic coating layer. There is a transition zone of
mechanical properties between the metal substrate
and the shot peened layer. The chemical
composition is not changed in the metal transition zone.
Nevertheless, the interface between metal and ZnP
and the interface between ZnP and the coating
provide favorable sites for corrosion when the
bonding condition is an issue, and a crevice is easily
formed in a moist/humid environment. Leidheiser6
systematically summarized the problem of corrosion
on coating protected metals and pointed out that
many problems remain unsolved. Ashida7,8 reported
significant occurrence of localized corrosion from
coating-damaged locations on coil springs.
It is important to understand localized corrosion
under imperfect or damaged coatings. Localized
corrosion has been studied for decades, and the
current understanding of the mechanisms and
critical factors has been reported.9–15 In the case
of resin powder-coated carbon steels, susceptibility
to corrosion is correlated to the properties of each
protective layer, and the bonding conditions
between different layers, as shown in Fig. 1. The
main purpose of the shot-peened layer is to provide
compressive stress on the surface to mitigate the
initiation of fatigue cracks. In addition, the
beneficial effect of compressive stress on localized
corrosion is reported by Liu et al.16 and Peyre et al.17 The
surface condition of shot-peened carbon steel affects
the formation and adhesion of the ZnP layer and the
organic coatings. Zinc phosphate crystals protect
the metal surface from corrosion and provide a
suitable interface for bonding with top coatings.18
The multiple chemical processes of forming the ZnP
layer determines the composition/shape of particles,
the surface coverage, and the layer thickness. The
outermost layer of a single- or dual-powder coating
provides a barrier on top, to prevent diffusion
processes and the occurrence of chemical and
electrochemical reactions on the metal surface.
Imperfect or damaged coating can cause corrosion and
subsequent crack initiation from the corroded site.
Figure 1 shows a schematic overview of corrosion
and cracking that originated from coating damage.
The process of localized corrosion (i.e., pitting or
crevice corrosion) involves the formation of coating
damage, partial or complete penetration through
coating and pretreatment, dissolution of the
exposed substrate (i.e., the carbon steel substrate
corrodes when no protective layers are provided),
crack initiation at the bottom of a corrosion pit, and
hydrogen-assisted crack propagation that leads to
final failure. In addition, crevice corrosion occurs
when adhesion is lost at the interfaces. Kendig and
Mansfeld19,20 reported that penetration of the
coating did not by itself cause failure of the coated
metal. Nevertheless, loss of adhesion between the
coating and the surface, as well as cohesive failure,
was the major driving force causing final failure.
Root Cause of Fatigue and Corrosion Fatigue
Fatigue cracking initiates in both dry and wet
environments under cyclic loading. In most cases of
field failure, the root cause of cracking is related to
metallurgical, physical, or corrosion defects on the
surface, such as surface or subsurface inclusions,
mechanical scratches or improper shot peening, or
pitting and possibly crevice corrosion. Dry fatigue
commonly starts from a metallurgical or physical
defect. In the case of corrosion fatigue, inclusions
and physical defects (e.g., a damaged coating) also
provide favorite sites for the initiation of corrosion
pits. Starting from these imperfect surfaces, small
cracks form at the early stage of cracking. The
formation of small cracks could represent a
significant fraction of the life of a component.21
Subsequently, both aqueous environments and the
mechanical driving force promote the propagation
of corrosion fatigue.
Hydrogen-Assisted Cracking of High-Strength
Hydrogen-delayed fracture or hydrogen-assisted
cracking (HAC) of high- and ultrahigh-strength
carbon steels have been studied for decades.
According to Gangloff,22 hydrogen degradation of the crack
propagation resistance of this type of alloy is
categorized as either internal hydrogen-assisted
cracking (IHAC) or hydrogen environment-assisted
cracking (HEAC). As shown in Fig. 1, the effect of
hydrogen is localized to the crack tip, regardless of
the source of the hydrogen (i.e., introduced by
manufacturing processes or through environmental
exposure). In the case of suspension coil springs, the
influences of tensile strength, hydrogen
concentration, and applying stress mode (tension or torsion)
on delayed fracture behavior have been
experimentally investigated using SAE9254 steel with a
tensile strength in the range between 1700 and
2000 MPa.23 It was found that the delayed fracture
strength tends to decrease with the increment of
diffusible hydrogen concentration, which is
especially significant when the amount of hydrogen is
less than 1 ppm. To ensure design integrity, these
findings on hydrogen cracking are important to
aPRE = [Cr, wt.%] + 3.3([Mo, wt.%] + 0.5[W, wt.%]).
ENVIRONMENTALLY ASSISTED CRACKING
OF IRON- AND NICKEL-BASED ALLOYS IN
SALT PRODUCTION AND PROCESSING
Stress corrosion cracking of stainless steels in
chloride containing environments is the most
common failure mode of vessels and pipes in chemical
processing and in the petrochemical industry. The
mechanism and controlling factors affecting chloride
stress corrosion cracking (CLSCC) have been
systematically summarized in well-known corrosion
textbooks.24,25 According to the empirical rule as
shown in the Copson curve,24 the susceptibility of
CLSCC increases with the nickel content from 0% to
approximately 10%. Nickel content from 8 to 10% is
the typical range of traditional AISI 304 and 316
steels, that are in the range of maximum
susceptibility. Nickel as an alloy element is said to have a
beneficial effect on stress-corrosion cracking in
chloride-laden environments in the case of nickel content
being more than approximately 10%. The CLSCC
susceptibility decreases for lower nickel content (i.e.,
duplex stainless steels) or higher content than this
range, as in the case of super-austenitic stainless
steels or nickel alloys. Alloys containing more than 42
wt.% nickel become immune to CLSCC. This article
focuses particularly on the application of stainless
steels and Ni-based alloys in extremely concentrated
In the Japanese salt manufacturing process,
highsalinity water is obtained using an ion exchange
membrane and distillation from sea water. The highest
chloride concentration is around 35 wt.%,26 and the
highest process temperature is around 130 C.27 Type
316L SS (S31600) is used in the standard structural
material of salt manufacturing plants. Although there
is extensive research about SCC in water containing
chloride, only a few studies have been conducted under
salt manufacturing conditions.28
Tsugawa et al.29 evaluated CLSCC susceptibilities
of alloys S31600, S31254, S32053, N08354, and
N06022 by U-bend tests under simulated salt
manufacturing conditions. The alloys S31254, S32053,
and N08354 are classified as super austenitic
stainless steels, and alloy N06022 is classified as a
nickelbased, corrosion-resistant alloy. They reported that
alloys with pitting resistance equivalent (PRE)
numbers over 50, such as alloys N08354 and N06022, were
proper structural materials for salt manufacturing
plants with high chloride concentrations. The
CLSCC susceptibilities of alloys S31600, S31254,
and S32053, especially in a bittern are very high. The
likely reason is that the high MgCl2 proportion of the
chlorides in a bittern brings about low pH and a low
pH buffer capacity; that is, low pH makes passivation
films of the alloys unstable, and the low pH buffer
capacity forms a low pH region locally.
Sugahara30 evaluated CLSCC susceptibilities of
iron-based and nickel-based alloys by carrying out
U-bend tests in a boiling 45 wt.% MgCl2 solution as
shown in Table II.
Although all of the alloys containing less than
39% nickel cracked within a short time, all of the
alloys containing around 60% nickel did not crack
even after being held for 1000 h. The results are in
good agreement with the Copson curve.
ENVIRONMENTALLY ASSISTED CRACKING
OF IRON- AND NICKEL-BASED ALLOYS IN
THE APPLICATION OF SUPERCRITICAL
The fourth state of water, supercritical water
(SCW), is water at a higher pressure and a higher
temperature than the critical point of water
(374.0 C and 22.1 MPa). Supercritical water
oxidation (SCWO),31–35 organic synthesis,36–44 hydrogen
production and upgrading of heavy crude oil,45–48
and supercritical water reactor49,50 have been
proposed as SCW applications. As SCW applications
tend to be under extremely high corrosive
conditions (e.g., high temperature and high pressure,
high or low pH, oxidizing or reducing environment,
existence of chloride ion, etc.), it is easy to cause the
SCC problem. Rebak51 found that N06625 and
N102276 are susceptible to intergranular stress
corrosion cracking (IGSCC) under SCWO conditions
by conducting slow strain rate testing (SSRT). In
this article, the results of testing under conditions of
SCWO and reducing (including acidic and alkaline)
are summarized on several more iron- and
nickelbased alloys after Rebak’s51 report.
Corrosion and SCC in SCWO
Harmful waste, such as chemical weapons and
polychlorinated biphenyl (PCB), can be decomposed
under SCWO conditions. It is possible to generate
chloride and sulfuric ions in the process of
decomposition. It is important to develop iron- and
nickelbased alloys further with high performance of
resistance to corrosion and SCC in SCWO.
Accordingly, the effects of alloying elements on corrosion
and cracking behavior of conventional and new
alloys were investigated. Yakuwa et al. conducted
corrosion tests of the Ni-(20–50 wt.%)Cr-(0–
10 wt.%)Mo alloy in SCW containing several anions
(Cl = 17,000 mg/L, SO42 = 120 mg/L, etc.) and
cations (Ca+ = 7,180 mg/L, K+ = 5,800 mg/L, etc.)
at 600 C and 25 MPa. They reported that alloys
with chromium content of more than 35 wt.%
showed higher corrosion resistance than those with
chromium content of less than 35 wt.%, and that
molybdenum improved corrosion resistance of the
alloys.52 Hara et al. conducted corrosion tests of
nickel-based and iron-based alloys in SCW
containing 0.001 mol/kg-HCl + 0.3 mol/kg-O2 at 500 C
29.4 MPa. They reported that the corrosion
resistance of tested alloys strongly depended on
chromium content, and that nickel-based alloys with
chromium content of more than 20 wt.% and
ironbased alloys with chromium content of more than 30
wt.% became more corroded because of
trans-passivation.53 Schorer et al. conducted corrosion tests of
Ni-(20–40 wt.%)Cr alloys in SCW containing
0.12 mol/kg-HCl + 0.06 mol/kg-O2 at 410 C and
400 bar. They reported that Ni-30wt.%Cr showed
excellent corrosion, and that tungsten improved the
corrosion resistance of the alloys.54 Watanabe et al.
conducted corrosion tests on several types of
nickelbased alloys and iron-based alloys in SCW
containing sulfuric acid. They reported that chromium was
a key element that improved the corrosion
resistance of the alloys, and that iron also improved
corrosion resistance of these alloys under oxidizing
conditions.55 They also reported that corrosion
conditions of subcritical water and high-pressure
SCW are more severe than lower pressure SCW
because density and dielectric constant of water of
those conditions are higher than those of lower
pressure SCW. Higher density and the electric
constant of water enhanced electrochemical
reactions.55 Fujisawa et al. conducted SSRT on S31603,
N10276, N06625, and N06044 in SCW containing
0.001 and 0.01 mol/kg-HCl at 400 C 25 MPa. They
reported that IGSCC susceptibility of tested alloys
in 0.01 mol/kg-HCl was higher than in 0.001 mol/
kg-HCl. They also reported that the susceptibility to
IGSCC-containing higher chromium showed lower
IGSCC susceptibility.56 In summary, the chromium
content of the alloys is one of the key factors
affecting corrosion and cracking behavior in SCWO.
In addition, Watanabe et al. evaluated SCC
susceptibility of S31603 in the subcritical and
SCW containing 0.01 mol/kg H2SO4 and reported
that SCC susceptibility of S31603 was higher in
SCW than in the subcritical.57 In SCW, the sulfate
concentration did not affect SCC susceptibility of
S31603 in the range of 0.0001–0.01 mol/kg at 400 C
and 25 MPa.58 Nevertheless, it was found that a
thick oxidized film formed along grain boundaries in
a sulfate-containing environment. Water density
was another factor affecting SCC susceptibility.
Crack initiation in low-density water occurred more
often than in high-density water.58
Corrosion and SCC in Reducing (Acidic and
Adding hydrogen to SCW (i.e., reducing SCW) can
be used for refining coal and oil sand at high pH and
for hydrothermal synthesis at low pH.
Experimental data of SSRT on stainless steels and nickel-based
alloys in reducing SCW were first reported by
Nishida and Fujisawa et al.59,60 They evaluated
the corrosion resistance of S31600, N10276,
N06625, N06210, and N06044 under reducing
0.01-mol/kg-HCl and 0.05–0.5-mol/l-NaOH
conditions.59,60 It was found that the corrosion resistance
of nickel-based alloys showed better corrosion
resistance over S31600 in all tested conditions, and that
the corrosion rates of tested alloys tended to
increase with increasing hydrogen partial pressure
in SCW at low pH at 400 C and 25 MPa. They also
showed that the Ni-Cr-Mo alloy demonstrated
better corrosion resistance than a N06044 alloy that
contains 44 wt.% of chromium. Fujisawa et al. also
showed that alloy N06210 demonstrated the best
corrosion resistance in those alloys, and that
chromium and molybdenum improved corrosion
resistance of these alloys under the tested
conditions. At high pH, a similar corrosion behavior was
observed. Regarding SCC susceptibility, Fujisawa
et al.56 found that the IGSCC susceptibility of
S31600 and N10276 decreased when H2 partial
pressure was higher than 0.48 MPa. IGSCC
susceptibility of S31600, N10276, N06625, N06210, and
N06044 increased with increasing NaOH
concentration at 400 C and 25 MPa. The SCC
susceptibility of the tested alloy also decreased with increasing
chromium content. In summary, as in SCWO,
adding chromium to these alloys improved
resistance to corrosion and SCC in reducing SCW.
Molybdenum was also an effective element to
increase corrosion and cracking resistance.
Temperature : 300
Pressure : 25MPa 550 60MPa
Oxygen Partial Pressure (MPa)
P : HC P : HC
Figure 2 shows applicable conditions of iron- and
nickel-based alloys in SCW. Figure 2a and b
comprise the SCC maps of S31600 and N10276,
respectively, which generated from experimental data.
The SCC susceptible region is larger under
oxidizing conditions than under reducing conditions for
the two alloys. Both S31600 and N10276 are
immune to SCC in the pH range between 3 and 11
in reducing SCW. The two alloys can be used for the
application of hydrogen production from biomass,
which is in the pH range of 3.5–7.0 and the
hydrogen partial pressure range of 0.01–3.00 MPa
in reducing SCW.
AND FUTURE DIRECTIONS
For industrial applications, it is essential to
identify root causes and key factors affecting the
initiation and propagation of EAC. This article
shows a typical range of variation in material–
environment combination. In the case of a high
corrosion rate (‡10 lA cm 2) material, such as
carbon steel, exposure to a mild aqueous
environment can cause localized corrosion to accelerate the
initiation of fatigue or corrosion fatigue
significantly. For corrosion-resistant alloys with
passivation behavior, the PRE number works as an
indicator of the passive film broken down.
Increasing the number of PRE delays the occurrence of
pitting and effectively prevents SCC starting from
pitting corrosion. In addition, mapping of a
potential SCC susceptible region becomes more important
for proactive design under extreme environments
such as SCWO and reducing SCW. In general, to
mitigate EAC in commercially used materials and
structures, the research from industry includes
developing new steels and alloys to improve EAC
resistance, developing new testing technologies to
identify the EAC regime, and increasing integrity
and reliability to extend the life of components and
structures. The future direction of industry-directed
research will need to continuously focus on these
areas to meet the requirements of next-generation
production and applications.
Regarding new steel grades for coil spring
manufacturing, Nakayama et al.62–65 proposed a method
to improve corrosion fatigue resistance of
ultrahighstrength steel by rust control and hydrogen
trapping. In the development of UHS1900 steel designed
with high strength and excellent corrosion fatigue
resistance, rust composition control was achieved by
the addition of copper, nickel, and chromium.
Hydrogen trapping sites were introduced by the
addition of titanium. In addition, Yoneguchi et al.66
reported the effectiveness of adding boron, niobium,
and nickel for the improvement of corrosion fatigue
strength and delayed fracture strength of coil spring
steels. The development of the N06210 alloy
previously described for application in highly
concentrated chloride solutions and SCW environments is
another example of improving EAC resistance. It’s
important to develop iron- and nickel-based alloys
further with a high performance of resistance to
corrosion and SCC in the SCW environment.
Industries are interested in developing new
methodologies for testing corrosion and cracking.
For automotive applications, Ashida et al.67 showed
the effectiveness of using coupled multielectrode
array sensor (CMAS) technology to evaluate localized
corrosion on ZnP pretreatment and powder coatings.
Otake et al.68 used a compact neutron source for the
nondestructive visualization of corrosion under
coating films. The new technologies help to better
understand the mechanism of corrosion and cracking under
coatings, or at a damaged coating site. For testing in
the SCW environment, it is important to enhance the
capability of testing EAC, as well as to generate
reliable data in the environment up to 30 MPa of
pressure and 600 C.31–50
To achieve both high performance and extended
component life for industrial applications, it is
crucial to evaluate EAC resistance along with
material development, component design, and
manufacture processing. The root cause of failure and
the key factors affecting the engineering life of
components must be identified by testing not only
small specimens but also component-level
performance. These concepts apply in the development of
2000-MPa grade, advanced high-strength spring
steel for the suspension component of lightweight
vehicles.66,69 In the meantime, surface condition
control before coating (including the control of
soluble salt contamination70) is important for the
management of the coating life cycle, which largely
affects the initiation of localized corrosion and EAC
in high-strength carbon and low-alloy steels.
The authors would like to thank Dr. Shinichi
Nishizawa of NHK International Corporation and
Mr. Toru Kobayashi of Hitachi Metals MMC
Superalloy, Ltd. for their support in the preparation
of this article. We thank Dr. Srujan Rokkam, the
SCC Subject Editor, and the four anonymous
reviewers for their comments.
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