Materials and Design 32 (2011) 5154–5158

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Materials and Design

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Technical Report

A case study of environmental assisted cracking in a low alloy steel under

simulated environment of pressurized water reactor
M. Shahzad ⇑, A.H. Qureshi, H. Waqas, N. Hussain
Materials Division, Pakistan Institute of Nuclear Science & Technology (PINSTECH), P.O. Nilore, Islamabad, Pakistan

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

Article history: The electromechanical behavior of a pressure vessel grade steel A516 has been investigated using poten-
Received 10 March 2011 tiodynamic polarization curves and slow strain rate test (SSRT) in simulated environment of pressurized
Accepted 20 May 2011 water reactor. The anodic polarization behavior shows that the steel remains active in the solution till
Available online 25 May 2011
localized attack (pitting) starts. The cracks initiated at the surface propagate in a trans-granular mode.
These cracks are initiated at the inclusion (MnS) sites and at the interfaces between local anode (ferrite)
and local cathode (pearlite). It seems that the ultimate fracture occurs when the propagating surface
cracks join the subsurface hydrogen induced cracks. The addition of oxygen in the testing chamber to
supersaturation levels shifts the corrosion potential to anodic side and significantly lowers the strength
and ductility. Compared to the room temperature properties, the UTS and tensile elongation in various
simulated conditions are reduced by 10–25% and 25–75%, respectively.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction
Steel is the most commonly used structural metal and has a
wide range of alloys for specific engineering applications. One of
the important applications of steels is in the fabrication of pressure
vessels. Because of the high pressures that these vessels retain, the
pressure vessel grade steels must meet the stringent requirements
of high notch toughness and strict low limits for allowable imper-
fections. One of the widely used pressure grade steel is A516 G-70
which contains Mn as principal alloying element. Manganese is
normally present in all commercial steels due to its multiple ben-
efits. It deoxidizes the melt and facilitates hot working of the steel
by reducing the susceptibility to hot shortness. Mn also contributes
in strength and hardness, and has a strong effect on the hardenabil-
ity of steel. A516 has the highest strength and ductility among
other pressure vessel steels (containing slightly lower levels of
Mn but relatively higher levels of S); moreover, it gives the longest
time to fracture in corrosive environments [1]. Recent studies on
this alloy show strong dependence of mechanical and corrosion
properties on morphology of ferrite [2,3].
The pressure vessel grade steel used in pressurized water reactor
(PWR) must meet an additional requirement of low susceptibility to
SCC and HIC in the working environment. The fracture toughness
(KIc) values drop significantly when the material under stress is also
exposed to the aqueous environment in which electro-chemical
reactions can take place. The water chemistry in such applications
is carefully maintained within the safe regimes to minimize the ef-
⇑ Corresponding author. Tel.: +92 51 2207 226; fax: +92 51 2207 374.
E-mail address: shahzad@pinstech.org.pk (M. Shahzad).
fects of corrosion and corrosion related phenomenon e.g. HIC and
SCC. One such controlling factor is the dissolved gaseous content
of the solution [4–7]. Corrosion is an electrochemical process and
proceeds with the formation of local anodes and cathodes at the sur-
face exposed to the corrosive medium. At equilibrium, the rate of
anodic reaction (oxidation) is equal to the rate of cathodic reaction
(reduction). In aqueous environments, the reduction reaction con-
sists of oxygen reduction reaction. An increase in the dissolved oxy-
gen contents increases the rate of reduction reaction (O2 +
2H2O + 4e ? 4OH ) and thereby the corrosion potential of the sys-
tem. Since, the corrosion potential is decided at the point where the
current produced by oxidation is totally used by the reduction reac-
tion; an increase in the dissolved oxygen contents increases the cor-
rosion potential, which is the driving force for the corrosion reaction.
Cáceres et al. observed the presence of a critical dissolved oxygen
content which separates the two distinct regions of high and low
corrosion rates. At this critical oxygen content, the corrosion current
density, corrosion potential and hydrogen evolution rate are signif-
icantly increased [8]. The dissolved oxygen contents also affect the
composition of the corrosion products that is formed [9]. In pearlitic
steels, depending upon the dissolved oxygen contents, the pseudo-
passive range may be replaced with the active or passive range
[10]. A removal of oxygen from the solution also lowers the suscep-
tibility to stress corrosion cracking (SCC) [11].
The air contains about 209 ppm volume oxygen in gaseous
form. Due to which, air readily oxidizes the elements in materials
which have strong thermodynamic affinity to form oxides. The oxi-
dation process is particularly enhanced at higher temperatures.
The amount of oxygen that is dissolved in water or any other liquid
depends upon the partial pressure of oxygen in equilibrium with

0261-3069/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2011.05.034
 M. Shahzad et al. / Materials and Design 32 (2011) 5154–5158
that liquid, as per the famous Henry’s law. At room temperature
and atmospheric pressure the saturated dissolved oxygen content
is about 8 ppm. The oxygen dissolution limit in water decreases
with a rise in temperature and increases with an increase in pres-
sure. Baranenko et al. have calculated the solubility limits of oxy-
gen in water at various temperatures and pressures [12]. It is
clear from their results that at reactor conditions (300 °C and
15 MPa), a small amount of dissolved oxygen is present in equilib-
rium with the water, and is readily available for the oxidation reac-
tion. Present study investigates the environmentally assisted
cracking (EAC) behavior of the alloy in simulated PWR condition
with particular emphasis on the influence of oxygen levels (satura-
tion to supersaturation) present in equilibrium with the water in a
closed testing chamber. The supersaturated levels of oxygen have
been achieved by purging the pure oxygen gas into the chamber
before heating.
2. Experimental procedure
The alloy A516 G-70 steel was received in the form of a sheet
having a 12 mm thickness. The electromechanical behavior of the
alloy in PWR simulated environment was studied using electro-
chemical corrosion testing and slow strain rate tests (SSRT) using
Reference 600 of Gamry Instruments and stress corrosion cracking
testing machine of CORTEST Inc., respectively. The pressure vessel
in PWR works at about 290–310 °C under a pressure of about
15 MPa. The room temperature pH of the coolant is 6.5–7. The
coolant contains Boric acid and LiOH, which are instantaneously
added into the coolant system as per requirement to control fission
reactivity and pH, respectively. These conditions were simulated in
the laboratory using demineralized water (DMW) having a room
temperature pH and conductivity of 6 and 2 lS cm 1. Boric acid
and LiOH were added to the DMW in amounts giving 100 ppm of
boron and 7 ppm of Li in the solution. The potentiodynamic polar-
ization (anodic polarization) behavior of the alloy was studied in
the simulated solution using electrochemical corrosion testing at
room temperature. Some additional electrochemical tests were
performed to study the effects of boron concentration on the cor-
rosion rate. All electrochemical corrosion tests were performed
on round shaped specimens having an exposed surface area of
0.785 cm2 in the PWR simulated coolant. The slow strain rate tests
(SSRT) were performed in air at room temperature and at 300 °C,
and in simulated solutions at 300 °C. All tests were performed at
an initial strain rate of 1E 6 s 1. The tensile samples (25 mm
gauge length, 6.25 mm gauge diameter) used in this study were
machined from the alloy A516 G-70 steel sheet such that their ten-
sile axis were parallel to the rolling direction. At 300 °C, the pres-
sure gauge showed a pressure of about 8.5 MPa in the testing
chamber, which is the equilibrium pressure between water and
its vapors at 300 °C in a closed chamber [13]. The oxygen contents
in the solution during SSRT were controlled by purging pure oxy-
gen at room temperature for a calculated time span which corre-
sponds to oxygen contents of 45 ppm and 95 ppm inside the
closed chamber containing the solution and the sample. The elec-
trochemical corrosion potential was measured using a CORTESTÒ
external reference electrode for all the SSRT preformed in solution.
The microstructural analysis of the secondary cracks and fracture
surface morphology were performed using Olympus BX51 optical
microscope and Phillips scanning electron microscopy (SEM). En-
ergy dispersive X-ray analysis was done on SEM to characterize
the MnS inclusions.
3. Results and discussion
The chemical composition of the steel is given in Table 1. The low
carbon steel contains Mn as a main alloying element. The optical
5155
Table 1
The chemical composition of the alloys used in study.
C Mn Si S P Fe
0.2 0.9 0.22 0.04 0.035 Balance
micrographs of this ferritic steel is presented in Fig. 1. The micro-
structure in as received conditions consists of ferrite and pearlite
which are elongated in the rolling direction. The average size of fer-
rite grains is 25 lm and their volume fraction is 72%. In addition to
their effects on mechanical properties, the ferrite grain size and
their volume fraction are important for their corrosion properties.
Since, ferrite is anodic to pearlite [14] the volume fraction of ferrite
plays an important role in electrochemical properties of the steel ex-
posed to a solution. In addition, the morphology of pearlite plays an
important role in corrosion properties; because, it affects the inter-
face areas between the local cathodes (pearlite) and anodes (ferrite).
In general, the free corrosion potential increases as the interface
area between the two phases increases [15].
The potentiodynamic polarization curve of the steel in PWR
simulated environment (Fig. 2a) shows that the steel remains ac-
tive in the exposed environment. The anodic polarization current
which is equivalent to the corrosion rate in such condition in-
creases constantly with an increase in the applied potential till
the localized attack or pitting starts at a voltage of about 1 V which
was also clearly evident on the specimen surface. Fig. 2b shows
that an increase in the boron concentration from 100 ppm to
1000 ppm levels does not affect the corrosion potential. However,
the anodic and cathodic polarization slopes are also changed. The
Icorr and corrosion rates in the three conditions are give in Table
2, which shows that the corrosion rate increases from 1.34 mpy
to 7.35 mpy (increased by 450%) when the boron concentration
is increased from 100 ppm to 1000 ppm level (increased by 900%).
The polarization curves shown in Fig. 2 show the interactions
between steel and PWR simulated coolant in the absence of any
external stress. In general, the Icorr values and thus the uniform
corrosion rates shown in Table 2 are low which indicate a good
control of water chemistry. However, the imperfections in the
material may lead to localized attacks on the steel which can sig-
nificantly affect the mechanical properties under stress by acting
as stress raisers. Earlier studies have shown that microcells formed
in the corrosion pits may have corrosion rates higher by an order of
magnitude than the uniform corrosion rate [16]. Fig. 2a shows the
indications the onset of some sort of passivation, which is only
short lived and successive cycles of film formation and breakage
follow. The value of the pitting potential is important because
the corrosion potential may shift during the service life depending
upon the chemical composition of the coolant, i.e. the concentra-
tion of ions and oxygen contents [17]. Boron is added to the coolant
system in form of boric acid. Natural boron contains 20% B-10
which has a high absorption cross-section for thermal electrons.
In addition to the boron rods, the concentration of boron in the pri-
mary loop of the PWR coolant is one of the basic variables to con-
trol the fission rate in reactor pressure vessel. Fig. 2b shows that an
increase in the boron concentration (in the range 100–1000 ppm)
increases the corrosion rate. The highest corrosion rate has been
observed at 1000 ppm B (200 ppm of B-10) levels. Some other
studies have also shown that low alloy is prone to boric acid corro-
sion [18] and the corrosion rate increases with an increase in the
boron to lithium concentration ratio [19].
The results of the SSRT are presented in Fig. 3 in terms of engi-
neering stress–strain curves. The steel exhibits a sharp yield point
when tested in air at room temperature. However, in PWR simu-
lated solutions contained under saturated and supersaturated oxy-
gen conditions at 300 °C, there are gradual transitions from elastic
5156 M. Shahzad et al. / Materials and Design 32 (2011) 5154–5158

Table 2
The corrosion potentials and corrosion rates (from tafel slopes) measured at room
temperature by electrochemical corrosion cell (i–iii); and the corrosion potentials
measured during slow strain rate tests at 300 °C using an external electrode (iv–vi).

Test condition Corrosion Icorr Corrosion

potential (mV) vs (A/m2) rate (mpy)
SCE
i Solution with 100 ppm B 638 2.94E 2 1.34
ii Solution with 200 ppm B 655 3.49E 2 1.60
iii Solution with 1000 ppm 669 1.61E 1 7.35
B
iv Solution (100 ppm B) 623 – –
with 8 ppm oxygen
v Solution (100 ppm B) 434 – –
Fig. 1. Optical micrograph of the steel in as-received condition. with 45 ppm oxygen
vi Solution (100 ppm B) 322 – –
with 90 ppm oxygen
to plastic range. The strain hardening rate is reduced when the
temperature is raised from room temperature to 300 °C (compare
curves 1 and 2 in Fig. 3). However, the same temperature raise does
not affect the strain hardening in the presence of PWR simulated 500
solution. Supersaturating the testing chamber with oxygen to 1
3
45 ppm and 90 ppm levels only slightly increases the strain hard- 400

Stress (MPa)
ening rate (curves 3–5 in Fig. 3). In comparison to room tempera- 4
ture properties, the UTS drops by almost 50 MPa (10% drop) and 5 2
300
strain to fracture is reduced to 0.1 (50% drop) under PWR simu- 1 Air, Room temp.
lated conditions. The UTS and elongation values are further 200 2 Air, 300OC
dropped if the testing container is supersaturated with oxygen to 3 Soln (8 ppm), 300OC
45 ppm or 90 ppm levels. In the latter case, the UTS is dropped 100 4 Soln (45 ppm), 300OC
by 175 MPa (35% drop) and strain to fracture is dropped to 0.05 5 Soln (90 ppm), 300OC
(75% drop). All relative drops in percentages are with respect to 0
room temperature properties in air. The corrosion potential mea- 0.0 0.1 0.2 0.3
sured at SSRT testing conditions using CORTESTÒ external refer- Strain
ence electrode show that oxygen purging shifts the potential to
Fig. 3. Stress strain curves of the slow strain rate tests conducted in air and solution
anodic side. The potential shifts from 623 mV to 434 mV and under slow strain rate conditions.
322 mV (all potentials against SCE), when the oxygen contents
are increased from saturated level (8 ppm) to 45 ppm and
90 ppm, respectively. exposed to the simulated environment, the rate of strain hardening
The sharp yield point is widely credited to the pinning of mov- at 300 °C is even higher than that of at the room temperature. This
ing dislocations by their environments usually the solute elements. is due to the additional hindrance to the moving dislocations by
An extra amount of stress is required for dislocations to break this the adsorption of H which is produced during cathodic part of
environmental barrier and once the plastic deformation starts the electrochemical corrosion reactions occurring at the surface
there is a little bit drop in stress. At 300 °C, the movements of dis- of the exposed sample [20]. Infact, strain-hardening and an homog-
locations require a lower critical resolved shear stress and the enous or localized strain rate are necessary for environmentally as-
environmental pinning is usually not that effective. Thus, under sisted cracks to initiate and propagate [21]. The addition of oxygen
PWR simulated conditions, the transition from elastic to plastic into the system increases the rate of cathodic reaction, thus pro-
range is a gradual one. Once the plastic deformation starts, the dis- ducing more hydrogen to be absorbed, which raises the rate of
locations pile up at the grain boundaries and further slip on these strain hardening with the increase in oxygen contents. Moreover,
planes requires a higher stress resulting in strain hardening. At the increased corrosion activity increases the rates of initiation
300 °C, the thermal energy allows the piled up dislocations to and propagation of surface crack by enhancing the dissolution of
move to other planes and allow further deformation at lower stress inclusions and other local anodic sites at surface, and the exposed
than that is required at room temperature. However, when surfaces of the propagating cracks, respectively [22,23].

(a) 2.0 (b) -0.25

1 100 ppm B
1.5 1 2 3
Potential (V, SCE)
Potential (V, SCE)

2 200 ppm B
3 1000 ppm B
1.0 -0.50
0.5

0.0
-0.75
-0.5

-1.0

-1.5 -1.00
1E-3 0.01 0.1 1 10 100 1E-5 1E-4 1E-3 0.01 0.1 1 10
Current density (A/m2) Current density (A/m2)

Fig. 2. The electrochemical behavior of the alloy in simulated PWR condition (a) anodic polarization behavior and (b) effect of boron concentration on tafel slope.
 M. Shahzad et al. / Materials and Design 32 (2011) 5154–5158 5157

Fig. 4. Secondary cracks analysis of the steel after SSRT test. (a) Optical micrograph showing the longest crack observed, (b) SEM image showing crack propagation along the
parallel ferrite–pearlite bands by connecting the pits formed in SSRT and (c) EDX analysis showing increased levels of Mn and S around the pits visible in SEM image.

Microstructure based models of stress corrosion cracking have re-

ing the several fine pits that are indicated by arrows on the micro-
vealed that ferrite constituents in pearlite act as local anodes and
graph. An EDX analysis of the adjacent regions (Fig. 4c) shows a high-
their dissolution causes the cracks initiation which act as stress
er concentration of Mn and S, indicating the presence of MnS
raisers [24]. Similar mechanism of crack initiation at ferrite has
inclusion which has probably been oxidized following a reaction
been observed in A516 alloy [25] which grow into pearlite upon
MnS + 2H ? H2S + Mn2 [22].
prolonged exposure [26].
The SEM fractographs of the tested specimens are given in
One of the secondary cracks observed in solution containing
Fig. 5. The specimen tested in air (Fig. 5a) shows some dimples
90 ppm oxygen has been shown in the optical micrograph (Fig. 4).
on the fractured surface which is a peculiar feature of ductile frac-
The crack grows in almost a straight line perpendicular to the stress
ture. The fractographs of the specimens tested in environment
axis. The fracture morphology is transgranular. The blunt base of the
(Fig. 5b–d) show a predominant brittle fracture. There are multiple
secondary crack has a higher cross-section than the tip, which still
surface cracks visible in all three fractographs. In addition there are
appears to be sharp i.e. little impact of direct corrosion. The scanning
also many subsurface cracks (c.f. Fig. 5c in particular) and pits
electron microscope image in Fig. 4b shows the subsurface cracks
which resemble with the typical hydrogen induced cracks (HIC)
which are not connected to the outer surface of the specimen. These
observed in steels exposed to H+ ions containing environments.
cracks which are significantly smaller than the surface cracks grow
Therefore, the probable mode of fracture in these specimens is
along the ferrite–pearlite interface, and seem to propagate by join-
the initiation of surface cracks of the kind seen in Fig. 4a which

Fig. 5. The fractographs of the specimen tested in (a) air at room temperature, (b) solution saturated with oxygen (8 ppm) at 300 °C, (c) solution containing 45 ppm of purged
oxygen at 300 °C and (d) 90 ppm of purged oxygen at 300 °C.
5158 M. Shahzad et al. / Materials and Design 32 (2011) 5154–5158
propagate until they meet the internal (HIC) cracks. A comparison
of Fig. 5b–d shows that with the increase in oxygen concentration,
the depth of surface cracks and the severity of HIC increases.
4. Conclusions
(1) Electrochemical corrosion testing shows that A516 remains
electrochemically active in the simulated coolant till pitting
occurs at pitting potential. Moreover, the results show slight
increase in corrosion rate with the increase in boron
concentration.
(2) Although, the room temperature corrosion rate measured by
electrochemical corrosion testing in the simulated PWR
coolant is in general low, the SSRT results show a significant
loss of strength and ductility due to hydrogen induced
embrittlement which leads to environmentally assisted
cracking (EAC).
(3) Purging the testing chamber with oxygen shifts the corro-
sion potential to anodic sides by 300 mV in the tested oxy-
gen level range (8–90 ppm). The increased corrosion
activity at this potential produces more hydrogen during
cathodic reaction which causes increased strain hardening
and significant loss of ductility (25–75%) in the tested range.
In comparison, an increase in boron concentration (100–
1000 ppm) has relatively much smaller effect on the corro-
sion potential.
(4) The EAC proceeds with the crack initiation at micropits
formed at the specimen surface due to the oxidation of
MnS inclusions and localized corrosion at the ferrite–pearl-
ite interface. The surface cracks propagate in the transgran-
ular mode. The ultimate fracture occurs when the
propagating surface cracks meet the subsurface cracks
formed by the diffused hydrogen.
Acknowledgments
The authors acknowledge the support of IAEA in conducting this
study through TCP Project PAK/04/046. The authors gratefully
acknowledge Mr. Muhammad Akram for allowing experiments
on electrochemical corrosion testing instrument. Authors are also
thankful to Mr. Mohammad Masood and Mr. Amir Alam for
performing SCC tests and metallography, respectively.
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