Corrosion Science 74 (2013) 92–97

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Corrosion Science
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Potentiodynamic polarization behaviour of AISI type 316 stainless steel

in NaCl solution
Y. Yi a,⇑, P. Cho a,b, A. Al Zaabi a, Y. Addad a, C. Jang b
a
Department of Nuclear Engineering, Khalifa University, Abu Dhabi, United Arab Emirates
b
Nuclear and Quantum Engineering Department, Korea Advanced Institute of Science and Technology, Republic of Korea

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

Article history: Potentiodynamic polarization behaviour of AISI type 316 SS in NaCl solution was investigated in terms of
Received 6 October 2012 the potential scan rate effect. The critical pitting potential, Epit, of the stainless steel appeared to be
Accepted 9 April 2013 strongly dependent on the potential scan rate. A cumulative anodic electric charge density of the steel
Available online 22 April 2013
was defined as the total charge density from the open circuit potential, Eocp, and calculated using the
potentiodynamic polarization curves. It was found that, plotted as a function of the polarization time,
Keywords: the values of the cumulative charge density consisted of two lines with different slopes. It was confirmed
A. Stainless steel
that the deflection of the cumulative charge density vs. time plots corresponded to Epit and the values of
B. Polarization
C. Pitting corrosion
the cumulative charge density at the deflection were little dependent on the applied scan rate. The cumu-
lative charge density at the deflection was defined as a critical electric charge density for the stable pit-
ting. Also, it was suggested that this electric charge density should be associated with the critical
condition for the stable pitting and the critical electric charge for stable pitting should be a representative
parameter for the pitting resistance of a material.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction of Epit are obtained at different scan rates, it is questionable if Epit

Pitting is one of the localized forms of attack that results in rel-
atively rapid penetration at small discrete areas [1]. It is well-
known that chloride ions break down passivity or prevent its for-
mation in iron, chromium, nickel, cobalt, and the stainless steels,
which would result in pitting. The pitting susceptibility of materi-
als has been evaluated using the critical pitting potential, Epit. The
critical pitting potential is defined as a potential above which there
is a rapid increase in the current on a polarization curve, accompa-
nied by random formation of pits [2]. The pitting observed at the
potentials above Epit is known as the stable pitting which continues
to grow in a destructive fashion while the metastable pitting is de-
fined as the initiation and repassivation of micropits without stable
growth [3]. The critical pitting potential, Epit, of a material has been
determined by various electrochemical techniques such as poten-
tiodynamic, potentiostatic, and galvanostatic polarization tests
[4,5]. Man and Gabe have reported that, as a relatively simple
method, the potentiodynamic technique can give self consistent
data of pitting potentials with observed trends using pseudo-equi-
librium methods [6]. However, it has also been found that the pit-
ting potential determined by the potentiodynamic technique is
dependent on the potential scan rate [7,8]. Since different values
⇑ Corresponding author. Address: Abu Dhabi Campus, Khalifa University, PO
127788, Abu Dhabi, United Arab Emirates. Tel.: +971 2 401 8105.
E-mail address: yongsun.yi@kustar.ac.ae (Y. Yi).
could be a parameter representing pitting resistance of a material
in a given environment.
This study was aiming at finding another parameter as a pitting
resistance indicator which was not dependent on the polarization
conditions. Using AISI type 316 stainless steel potentiodynamic
polarization tests have been performed in a simulated sea water
condition. Changing the potential scan rate, its effect on the polar-
ization parameters of the stainless steel was investigated.
2. Experimental
2.1. Material and sample preparation
AISI type 316 SS (UNS S31600) was used in this study and its
chemical compositions are shown in Table 1. The samples
(10 mm  10 mm  3 mm) were cold-mounted in epoxy resin
with a wire connection and used as a working electrode. Sample
surfaces were abraded up to #2400 using SiC papers and ultrason-
ically cleaned and dried just before they were introduced into the
electrochemical set-up.
2.2. Potentiodynamic polarization testing
The tests were performed with the conventional three-elec-
trode set up. A graphite rod was used as a counter electrode and

0010-938X/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.corsci.2013.04.028
 Y. Yi et al. / Corrosion Science 74 (2013) 92–97
Table 1
Chemical Compositions of AISI type 316 SS (wt%).
Type C Fe Cr Ni Mo Cu Mn Si S P
316 SS 0.05 67.9 17.34 10.73 2.15 0.25 0.64 0.6 0.005
an SCE (saturated calomel electrode) as a reference electrode. Be-
fore the polarization, samples were cathodically conditioned at
500 mV vs. Eocp (open circuit potential) for 5 min to remove air-
formed surface oxide. Then, they were polarized from the cathodic
conditioning potential in the positive direction. To investigate the
effect of the potential scan rate on the polarization behaviours of
the stainless steel, the tests were performed at five scan rate con-
ditions of 0.01, 0.1, 1, 10, and 50 mV s1. The solution for these
tests was aerated 3.5% NaCl solution (800 ml). The tests were
interrupted at a certain current density after the samples had
shown the stable pitting indicated by the sudden increase in the
current density on the current density vs. potential plots. All the
tests were done at 25 ± 1 °C.
3. Results
3.1. Potentiodynamic polarization curves and critical pitting potential
(Epit)
The potentiodynamic polarization curves of type 316 SS mea-
sured in 25 °C, 3.5% NaCl solution at the scan rates from 0.01 to
50 mV s1 are shown in Fig. 1. Tested at the scan rates of 1, 0.1,
and 0.01 mV s1, type 316 SS showed a typical anodic polarization
behaviour of a stainless steel in a NaCl solution consisting of active
dissolution, passivity, and a rapid increase in the current density
due to pitting. This rapid increase in the current density indicates
the occurrence of the stable pitting in which the potential corre-
sponding to this current transient is known as a critical pitting po-
tential, Epit [1]. Fig. 2 is an optical microscope image of a test
sample at 1 mV s1 scan rate showing stable pits grown during
the polarization. In Fig. 1 some current density spikes are observed
at potentials below Epit. These spikes are due to the occurrence of
metastable pits and are explained by the consecutive formation
and repassivation of microsize pits [9,10]. Comparing the three
curves together, the frequency and magnitudes of the spikes ap-
pear to increase with the potential.
Fig. 1. Potentiodynamic polarization curves of type 316 stainless steel in 3.5% NaCl
solution at different scan rates.
93
0.02
Fig. 2. Pits formed on the 316 SS sample during the potentiodynamic polarization
at 1 mV s1.
On the other hand, the samples tested at higher scan rates, 10
and 50 mV s1, did not show a clear indication of the stable pitting
until the transpassive potential region at a potential around 1.2 V
(vs. SCE). This transpassive dissolution of type 316 SS is due to
the oxidative dissolution of Cr oxide, which is observed in solutions
with no chloride ions [11]. The values of Epit determined for the
polarization curves are listed in Table 2, which are increasing with
the scan rate as expected in literature. Various analyses on the
polarization curves have been performed. Among the parameters
analyzed here, a cumulative anodic electric charge density showed
interesting characteristics, which will be discussed in the following
sections.
3.2. Cumulative anodic electric charge density
A cumulative anodic electric charge density, which was defined
as a total charge density from Eocp, was calculated for the anodic
polarization curves shown in Fig. 1. The cumulative anodic electric
charge density was calculated by converting the potential values in
the polarization curves to the anodic polarization time from Eocp
and integrating the polarization curves with respect to the time:
Z t
QðtÞ ¼ jðtÞ dt ð1Þ
0
where Q(t) is the cumulative electric charge density. The time t and
the potential E are correlated by the following equation:
E  103
t¼ ð2Þ
v
where E (V) is the potential (vs. SCE) and v (mV s1) is the scan rate.
The cumulative electric charge density was plotted as functions
of the applied potential and the anodic polarization time in Fig. 3.
On the cumulative charge density vs. the applied potential (Fig. 3a),
there was not anything noticeable. However, as shown in Fig. 3b it
is worth being noted that, plotted against the polarization time, the
cumulative charge density curve at every scan rate consists of two
lines having different slopes and they are deflected at similar Q val-
ues. Here, the values of Q at the deflection are defined as a ‘critical
electric charge density’. From this figure two parameters were
determined: (i) critical electric charge density and (ii) the poten-
tials at the deflection. The deflection potentials were determined
by converting the polarization times at the deflection using Eq. (2).
Table 2 summarizes the critical electric charge densities and the
potentials at the deflections together with Epit determined from the
polarization curves in Fig. 1 for comparison. As stated in the previous
94 Y. Yi et al. / Corrosion Science 74 (2013) 92–97

Table 2
Cumulative electric charge densities and critical pitting potentials of type 316 SS (wt%).

Scan rate (mV s1) 0.01 0.1 1 10 50

2
Critical electric charge density (mC cm ) 0.56 ± 0.29 1.19 ± 0.23 1.03 ± 0.10 1.22 ± 0.27 1.18 ± 0.28
Ecorr (V vs. SCE) 0.094 ± 0.006 0.152 ± 0.040 0.292 ± 0.045 0.432 ± 0.046 0.564 ± 0.031
Edeflect (V vs. SCE) 0.032 ± 0.030 0.377 ± 0.069 0.435 ± 0.014 0.515 ± 0.059 0.678 ± 0.066
a a
Epit (V vs. SCE) 0.032 ± 0.031 0.389 ± 0.086 0.463 ± 0.043
a
NOT determined.

section, the values of Epit for the polarization curves at 10 and

50 mV s1 could not be determined since they did not show the clear
indication of the steep increase in the current density. From Table 2,
it can be judged that the potentials at the deflections in Fig. 2b coin-
cide with the values of Epit from the polarization curves. These
deflection potentials will be referred to Epit , which increases with
the scan rate as shown in Fig. 4. In Fig 5 the values of the critical elec-
tric charge density are plotted against the scan rate, which are close
each other except for the scan rate condition of 0.01 mV s1.

4. Discussion

4.1. Critical parameter for pitting

The pitting potential, Epit, has generally been accepted as an

indicator for pitting resistance. Even though it is known as a critical

Fig. 4. Dependence of pitting potential on scan rate.

value indicating pitting tendency, there seem to be still some ques-

Fig. 3. Cumulated electric charge densities as functions of (a) the applied potential
and (b) anodic polarization time.
tions on its practical meaning [12,13]. To determine this critical
pitting potential, electrochemical potentiodynamic, potentiostatic,
and galvanostatic methods have been widely used. In the potentio-
dynamic method [7,14], the potential applied to a sample is contin-
uously changed and the resulting current densities are measured.
During the polarization materials that are susceptible to pitting
in a given environment suffer from a sudden increase in the cur-
rent density. The potential where this increase in the current den-
sity is observed is determined as Epit. However, this Epit determined
from the potentiodynamic method is known to be strongly depen-
dent on the potential scan rate. Broli and Holtan [7] observed that
Epit of unalloyed aluminium in deaerated 3% NaCl solution in-
creased as the scan rate increases over the range between 1 and
100 mV min1, which is very similar to the results in this study.
Concerning this scan rate dependence of Epit, they explained that
it might be related with time to reach equilibrium since longer
time would be necessary in higher scan rate polarization. Zhang
et al. [8] investigated the scan rate dependence of Epit of type 403
SS in chloride-containing borate buffer solution. In their study they
found a linear relationship between Epit and a square root of the
scan rate (v1/2), which was explained in terms of the critical cation
vacancy concentration using the PDM (point defect model). No
matter what the mechanism of this behaviour of Epit, it seems to
be obvious that Epit determined using the potentiodynamic tests
should be used limitedly. Pointing out this limitation, Broli and
Holtan [7] suggested that the stationary potentiodynamic method
should be used to get the most correct values for Epit. The station-
ary method is defined as a stepwise change of potential where each
potential is kept until a constant current is established. The exact-
ness of the pitting potential values determined using electrochem-
ical experiments will be discussed with the critical condition of the
stable pitting in a subsequent section.
 Y. Yi et al. / Corrosion Science 74 (2013) 92–97
Fig. 5. Critical electric charge densities determined at different scan rates.
The potentiodynamic tests on type 316 SS in this study showed
similar polarization behaviours to those found in literature, which
is typical for localized corrosion of stainless steel [15]. A new
parameter that has not been reported previously is the critical
electric charge density, Qc. Since the values of Qc were not depen-
dent on the scan rate and close each other over the wide range of
the scan rate, Qc may be a parameter representing the pitting resis-
tance of a material in the test condition.
4.2. Effect of scan rate on polarization behaviour
Even though a lot of work has been extensively performed on
pitting for various materials, there are only a few papers that have
reported the scan rate effect on the polarization behaviours associ-
ated with pitting [7,8,16]. Furthermore, in literature there are little
data sets that are available for the determination of Qc at different
scan rates. Therefore, Qc was resolved into two components and
the scan rate dependence of each component is discussed sepa-
rately. Since, as shown in Fig. 1, the anodic dissolution peaks are
not significant in neutral solutions such as neutral NaCl solutions,
ipass can be considered to be a representative current density value.
Then, the critical charge density calculated by Eq. (1) can be
approximately expressed as follows:
Q c  ipass  Dt p
where ipass the passive current density and Dtp is the anodic polar-
ization time duration until the stable pitting.
4.2.1. Effect of scan rate on ipass
In this subsection the scan rate dependence of the passive cur-
rent density, ipass, is discussed. First, data of the passive current
density of various materials available in literature were collected
and plotted as a function of the scan rate (v). The current density
values were averaged over the passive range in the polarization
curves and used as the values of ipass. The analysis showed that
log(v) and log(ipass) had a linear relationship in each data set.
Fig. 6 shows the data sets plotted using the following equation:
logðipass Þ ¼ logðC 1 Þ þ n1 logðv Þ or ipass ¼ C 1  v n1
where C1 and n1 are constants. The values of the exponent, n1, are
summarized in Table 3. It has been known that the potential change
during polarization affects the metallic dissolution and passive film
growth kinetics [17,18], which results in the changes in ipass. The
95
Fig. 6. Dependence of passive current density, ipass, on scan rate: (1) this study, (2)
Ref. [38], (3) Ref. [39], (4) Ref. [38], (5) Ref. [40], and (6) Ref. [41].
values of the exponent, n1, determined using the linear regression
ranged from 0.73 to 0.96 with very high values of R2.
4.2.2. Effect of scan rate on Dtp
The second term in Eq. (3) is defined as the time duration for the
anodic polarization before the stable pitting. Eq. (2) gives the rela-
tionship between Dtp and DEp that is defined as |Epit  Eocp|. Leckie
[16] and Broli and Holtan [7] have reported that Epit increases as
the scan rate increases for 304 stainless steel in 0.1 M NaCl and alu-
minium in 3% NaCl, respectively, which is in agreement with this
study (Fig. 4). However, no literature dealing with Dtp and DEp de-
fined in this study is available. Therefore, an analysis using only the
test results in this study was carried out in the same manner as the
analysis of ipass. As shown in Fig. 7, Dtp is linearly correlated with
the scan rate in a log–log plot. In the following relationship, the
second exponent, n2, was determined to be 0.77 (R2 = 0.99):
logðDt p Þ ¼ logðC 2 Þ þ n2 logðv Þ or Dt p ¼ C 2  v n2 ð5Þ
4.2.3. Scan rate dependency of Qc
Since the ipass and Dtp showed linear relationships in log–log
plots, from Eq. (3) Qc is expressed as follows:
Q c  C 1 C 2 v ðn1 þn2 Þ ð6Þ
ð3Þ
Also, the scan rate dependency of Qc is expressed the sum of n1
and n2. The analysis in the previous subsections shows that the
absolute values of n1 and n2 are very close each other
(|n1| = 0.73–0.96 and |n2| = 0.78). Therefore the sum of n1 and n2
is close to zero or much smaller value than 1, which implies that
the scan rate has little effect on the critical cumulative charge den-
sity. This analysis on the scan rate dependency of Qc was per-
formed using some data available from literature. Even though
this is not directly related to the determination of Qc, it is consid-
ered that these analysis results could support partially the concept
of Qc defined in this study.
4.3. Critical charge for stable pitting
ð4Þ The elementary pitting process can be divided into three stages
[19]: (i) pit nucleation, (ii) the development of a metastable pit,
and (iii) the stable pit growth. The nucleation stage simply involves
breakdown of the passive film at electrochemically active site, but
the propagation stage of pits is associated with complicated pro-
cesses. Many researchers seem to agree that there is a critical con-
96 Y. Yi et al. / Corrosion Science 74 (2013) 92–97

Table 3 According to Laycock and Newman [27] in general Epit will be

Values of the exponent, n1, from the linear relationship between log(v) and log(ipass). the lowest transition potential, ET, which is the transition potential
This [38] [39] [38] [40] [41] between diffusion controlled and activation/ohmic controlled
study growth. The transition potential, ET, is defined for a particular lim-
Materials 316 SS 304 SS CR 304 Ti Ti Ti iting current density. Hoar et al. [33] suggested the pitting poten-
SS tial (breakdown potential) as a critical potential value under which
Solutions 3.5% 1N 10 N 1N 0.9% 0.1 M the aggressive anion such as Cl could penetrate the surface film.
NaCl H2SO4 H2SO4 H2SO4 NaCl H2SO4
n1 0.82 0.83 0.73 0.77 0.75 0.96
Similarly, Leckie and Uhlig [34] explained that passivity was de-
R2 0.999 1.000 0.988 0.990 0.961 0.999 stroyed at the sufficient concentration corresponding to the critical
potential. Galvele [36] expressed the pitting potential as a function
CR: cold rolled.
of a polarization (g) needed to reach the critical x  i value where x
is the pit depth and i is the current density circulating in the pit.
These lead to a conclusion that the pitting potential should be re-
lated to a critical condition which depends on the water chemistry
inside pits and their geometry. Even though a number of works
have confirmed the existence of the pitting potential experimen-
tally as well as theoretically it is questionable that the exact values
of the pitting potential for materials can be experimentally mea-
sured. When the pitting potential is measured using the electro-
chemical techniques, it is not expected that the same or similar
water chemistry inside pits could be achieved with different test
conditions such as different scan rates in potentiodynamic polari-
zation, different applied potentials and currents in potentiostatic
and galvanostatic polarization, respectively. It is more likely that
in a practical sense the measured pitting potential could depend
strongly on the test conditions.
The values of Qc determined in this study appeared to be little
dependent of the scan rate. The cumulative anodic charge density
corresponds to the total amount of all the reactions occurring on
the material surface from Eocp. After repassivattion, the inner sur-
face conditions of the pits nucleated and developed in the metasta-
Fig. 7. Dependence of polarization time duration, Dtp on scan rate. ble manner are expected to be the same as that in the bulk. Also,
therefore, the current densities would also be the same in both
the pit and bulk surfaces. If during the polarization, all the pits
dition to determine whether an initiated pit grows in a stable man- are assumed to be fully occluded, the Qc inside the pits will contrib-
ner (stable pitting) or it is repassivated (metastable pitting). Pit sta- ute to accumulation of ions produced by the reactions on the pit
bility depends upon the maintenance of pit electrolyte surface. According to Scheiner and Hellmich, transition from meta-
composition and pit bottom potential that are at least severe en- stable pitting stage to stable pitting stage can be explained by phe-
ough to prevent repassivation [20]. Both the factors can be associ- nomena taking place at the anode: metal ions released from the
ated with a ‘‘salt film’’. It has been generally accepted [9,21–23] solid electrode combine with chlorides in the solution, forming
that a corrosion product ‘salt film’ is formed at the bottom of a metal chloride salt. The more ions released, the more salt is
growing pit, which was confirmed experimentally [24]. The main formed, until the saturation concentration of the salt is reached
role of this salt film is to block repassivation of the surfaces within [37]. Therefore, the Qc may be interpreted as a critical cumulative
a pit. Luo et al. [24] suggested a critical pit depth for salt film for- charge density condition inside occluded pits which causes the
mation which ensures the maintenance of the necessary local crit- critical chemistry for the salt film formation. However, the rela-
ical solution chemistry. This implies that there is a critical tionship between the cumulative electric charge density suggested
chemistry within pits for the stable pitting. On the other hand, in this study and the other critical conditions in literature should
Pistorius and Burstein [25,26] had developed a criterion for stable be investigated and verified as a further study.
pit growth in terms of the product of current density and pit depth.
And for stainless steel in chloride solution it was determined to be
3 mA cm1. Others have determined the criterion in terms of the
critical concentration of metal ions in pits. Laycock and Newman 5. Conclusion
reported [27] that solutions greater than about 80% saturated in
metal ions were necessary to prevent passivation. Using an elec- The pitting properties of AISI type 316 SS in NaCl solutions were
trode of 18Cr–12Ni–2Mo–Ti anodically polarized, Mankowski and investigated using the potentiodynamic polarization technique.
Szklarska-Smialowska measured the concentration of Cl ions in The results showed that the critical pitting potential (Epit) strongly
the pits grown for different time periods and found that the Cl depends on the scan rate. In the analysis of the results, a new
concentration inside the pits was much higher than that in the bulk parameter, the cumulative electric charge density (Qc), was defined
[28]. These previous reports suggest that there should be a critical and determined for the stainless steel using polarization curves
condition of the solution chemistry within pits for the stable pit- measured in 3.5% NaCl solution at the scan rates from 0.01 to
ting, which is also applied to the critical pitting temperature 50 mV s1. The values of Qc were 1.05 mC cm2 on average, show-
(CPT) [29–32]. Such critical conditions could be associated the pit- ing little dependency on the scan rate. Based on these results, it is
ting induction time. The induction time can be interpreted as a suggested that the cumulative electric charge density (Qc) should
time period required for Cl penetration or adsorption [33,34]. This be a parameter representing the pitting resistance of a material
is supported by an analysis by Sayed and Shayeb [35] that the when it is determined using the potentiodynamic polarization
induction time varies with aggressive ion concentrations. method.
 Y. Yi et al. / Corrosion Science 74 (2013) 92–97
In this study, the electrochemical meaning of Qc or its relation-
ship with the stable pitting was simply discussed in terms of the
critical chemistry condition inside pits. It will be further investi-
gated in future work.
Acknowledgements
The authors are grateful for the financial support and test facil-
ities provided Khalifa University. Also, the authors would like to
express thanks for Dr. Hasna El-Masri’s help and assistance on
the experiments.
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