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DOI: 10.1007/s11665-017-2648-0 1059-9495/$19.00

Passive Film Properties and Electrochemical Behavior

of Co-Cr-Mo Stainless Steel in Chloride Solution
Hong Luo, Chaofang Dong, Kui Xiao, and Xiaogang Li

(Submitted March 15, 2016; in revised form March 8, 2017)

The electrochemical behavior and passive film properties of Co-Cr-Mo ultrahigh-strength stainless steel in
neutral and acidic chloride solution were evaluated by potentiodynamic polarization curves, electro-
chemical impedance spectroscopy and x-ray photoelectron spectroscopy. The results indicate that the steel
exhibited good passivation behavior in neutral NaCl solution. Both the film formation potential and the
applied potential time showed great effects on the open-circuit potential value and stability of the passive
film. Furthermore, the oxides and hydroxides of Fe, Co, Mo and Cr were the primary components of the
passive film, and the composition of the passive film was changed with a change of pH environment.

on stainless steel in test environments (Ref 8-14). On the other

Keywords corrosion and wear, failure analysis, stainless steel,
ultrahigh strength
1. Introduction
Currently, ultrahigh-strength stainless steel is widely used in
high-tech and military industries due to its good resistance to
fatigue, high strength and toughness (Ref 1, 2). The application
of ultrahigh-strength steel is one of the most popular and
powerful ways to make lighter products and reduce their cost.
However, when used in industry-polluted atmospheres or in
acid rain environments, ultrahigh-strength stainless steel can
undergo severe corrosion, which can even lead to cracks (Ref 3,
4). In addition, acid rain and industry-polluted atmospheres
have become an issue of widespread concern in Asia along with
the rapid development of its industry. It has been an increasing
problem over the last few decades in some areas of China.
Passivity is defined by a relatively inactive state, where the
metal displays more noble-like behavior than thermodynamic
conditions predict (Ref 5-7). Currently, it is well known that an
extremely thin passive film spontaneously forms on the surface
of stainless steel during exposure of the steel to an oxidizing
environment. The passive film can be changed with an applied
potential or by the environment. The dynamic properties of the
passive film provide the key to the high resistance of stainless
steel to corrosive attacks. Thus far, there are many methods to
evaluate the electrochemical and passive behavior of the
passive film formed on the surface of stainless steel. On one
hand, the electrochemical measurements, such as potentiody-
namic polarization curves, electrochemical impedance spec-
troscopy (EIS) and cyclic voltammetry (CV), have been used to
observe the passive and corrosion behavior of the passive film
Hong Luo, College of Mechanics and Materials, Hohai University,
Nanjing 210098, China; and Chaofang Dong, Kui Xiao, and
Xiaogang Li, Institute of Advanced Materials and Technology,
University of Science and Technology Beijing, Beijing 100083,
China. Contact e-mails: luohong2001@hotmail.com and cfdong@
ustb.edu.cn.
hand, the x-ray photoelectron spectroscopy (XPS), auger
electron spectroscopy (AES) and secondary ion mass spec-
trometry (SIMS) have been very suitable for observing the
structure, thickness and composition of the passive film.
Moreover, the semiconductor properties and growth mecha-
nism of the passive film have been interpreted by the Mott-
Schottky approach and point defect model (PDM) (Ref 15, 16).
In this paper, a new type of Co-Cr-Mo ultrahigh-strength
stainless steel was designed for aircraft and its relevant
components (Ref 17, 18), and it was expected to have excellent
combined mechanical properties and corrosion resistance.
Thus, it is necessary to understand its electrochemical behavior
to gain insight into its corrosion failure mechanism. Moreover,
there is still a lack of systematic knowledge about the passive
film structure of this material. Thus, the goal of the present
work was to clarify the passive behavior of the Co-Cr-Mo
ultrahigh-strength stainless steel in neutral and acidic environ-
ments, which can be used to simulate neutral or acid rain
environments. The electrochemical behavior was investigated
by potentiodynamic polarization and EIS measurements. The
chemical compositions of the passive films formed in different
conditions were observed by the XPS.
2. Experimental
2.1 Materials and Solutions
The specimens used in this paper were cut from a sheet of
ultrahigh-strength stainless steel. The detailed chemical com-
positions (wt.%) of the steel were as follows: C 0.26, Cr 14.1,
Mo 5.00, Ni 2.30, Co14, W 1.04, Fe balance. The size of the
samples was 1 cm 9 1 cm. The samples were ground sequen-
tially with 400-2000 grit SiC papers and polished with 0.1 lm
alumina polishing powder. After that, they were cleaned with
ethanol and deionized water and then dried with warm air.
2.2 Electrochemical Tests
Electrochemical measurements were taken in 1 wt.% NaCl
solution, which was prepared using double distilled water,
using a PAR 2273 electrochemical workstation at room

Journal of Materials Engineering and Performance

temperature. The pH values of solutions were adjusted by the
dilute H2SO4. A three-electrode system was used for testing. A
saturated calomel electrode (SCE) was connected to the cell
through Luggin capillary as a reference electrode (RE), a
platinum plate was used as the counter electrode (CE), and the
samples were used as the working electrode (WE). Argon gas
was vigorously bubbled through the solutions for 30 min
before the experiment and was maintained during the whole
test.
At the beginning of the electrochemical measurements, a
cathodic potential of 0.8 VSCE was applied to the samples for
30 min to reduce the pristine oxide formed in air and during the
immersion of samples in the test solution. Polarization curves
were recorded at a rate of 1.0 mV s1, and the potential
scanning range started from 0.7 VSCE to the anodic direction.
The electrochemical behavior of the passive film in the
simulated environments was observed by electrochemical
impedance spectrum (EIS). The EIS measurement was con-
ducted with a PAR 2273 workstation. Before all EIS experi-
ments, a reducing potential of 0.8 VSCE was applied for
30 min, and then, several film formation potentials were
applied for 1 h to form a stationary passive film. The potentials
were chosen in the passive region, according to the results of
the polarization curves. The frequency of the EIS measurement
was selected from 1 mHz up to 104 Hz, with an applied AC
amplitude of 10 mV. Zview 2.70 software was used to fit the
measured EIS data. The different electrochemical measure-
ments were repeated at least three times.
2.3 Surface Passive Film Characterization
XPS was used to observe the chemical composition of the
passive film formed in different environments. The radiation
source of XPS was monochromatic Al Ka with a pass energy of
approximately 25 eV. The XPS results were analyzed by the
commercial software Xpspeak (version 4.1) with the Shirley
background subtraction and Gaussian-Lorentzian tail function
to achieve better fittings.
3. Results and Discussion
3.1 The Potentiodynamic Polarization Curve Measurements
Figure 1 shows the potentiodynamic curves of Co-Cr-Mo
ultrahigh-strength stainless steel in the 1 wt.% NaCl solution at
pH 3 and pH 7. The typical characteristics of the electrochem-
ical behavior of the stainless steel can be observed on the
curves, such as the active region, active-passive transition
region, passive region and transpassive region, with an
increasing potential from the free-corrosion potential in the
anodic direction.
As seen from Fig. 1, the shapes of the potentiodynamic
curves obtained in neutral and acidic solutions show no
apparent difference, suggesting that the corrosion mechanism
of stainless steel in the chloride solution is not be affected by
the pH. Furthermore, both in pH 3 and pH 7 solutions, typical
passivation features with a broad passive region are displayed
in the anodic parts of the potentiodynamic curves. Some
important parameters of the electrochemical behavior, such as
the pitting potential (Ep) and passive current densities (ip), can
be obtained by fitting the curves. The Ep decreased, and ip
increased as the pH value decreased, indicating that the
2.0
pH=3
1.5 pH=7
1.0
E vs. SCE / V
0.5
0.0
-0.5
-1.0
-6 -5 -4 -3 -2 -1 0 1 2
-2
log (j/mA cm )
Fig. 1 Potentiodynamic polarization curve of Co-Cr-Mo ultrahigh-
strength stainless steel in 1 wt.% NaCl solution at different pH val-
ues (scan rate of 1 mV s1)
corrosion resistance decreased in low pH solution. This appears
to be in agreement with the results of previous studies on
ultrahigh-strength stainless steel (Ref 19), where the stability of
the passive film layer of the ultrahigh-strength stainless steel
was enhanced with an increase in pH from 3 to 7. Furthermore,
the decrease in ip may be attributed to the changes of the
composition and thickness of the passive film.
3.2 Electrochemical Behavior in Neutral NaCl Solution
3.2.1 The Effect of Potential on the Electrochemical
Behavior. Figure 2 displays the EIS spectra of ultrahigh-
strength stainless steel in neutral 1 wt.% NaCl solution
(pH = 7) at the open-circuit potential (OCP) after the passive
film formed at a different potential for 1 h. According to the
results of the potentiodynamic curves, several potentials in the
passive region and the transpassive region were chosen. The
potentials of 0, 0.2 and 0.5 VSCE were in the passive region,
and 1.1 VSCE was in the transpassive region. This indicates that
the potential has the greatest impact on the corrosion resistance
of the passive film. As seen in Fig. 2, for the Nyquist plots, at
applied potentials of 0, 0.2 and 0.5 VSCE, the radius of the
capacitive arc increased with an increase in the potential values.
However, when the applied potential was 1.1 VSCE in the
transpassive region, the radius of the capacitive arc slightly
decreased, indicating the low corrosion resistance of the passive
film formed in the transpassive region. For the Bode plots,
typical passive state shapes are displayed in the plots. The
medium frequencies by phase angles of approximately 80°
indicate that a stable passive film formed on the surface of the
electrodes (Ref 20, 21). In addition, the phase angle value of the
passive film formed at 1.1 VSCE is slightly lower than that
formed at the other potentials. The high impedance values
obtained were consistent with the passive film formed at a
different potential, and the decrease in impedance in the
transpassive region was due to the dissolution of the passive
film (Ref 22). Sometimes, dissolving Cr or other alloy elements
results in the breakdown of the passive film (Ref 23).
To interpret the effect of the potential on the EIS of stainless
steel in neutral 1 wt.% NaCl solution, the electrical equivalent
model was used to explain the results. There are several
Journal of Materials Engineering and Performance
electrical equivalents for interpreting the EIS results in chloride tively. The R2 and CPE2 stand for the passive film resistance
solutions (Ref 24, 25). Here, we choose the most commonly and the capacitance of the passive film. In this model, the
used electrical equivalent models to interpret the EIS results. constant phase element (CPE) is used to represent a shift from
As shown in Fig. 3, an electrical equivalent model was used an ideal capacitor (C) instead of using the capacitance itself. As
that consisted of the electrolyte resistance, Rs, and the R1 and noted in previous studies (Ref 26, 27), CPE can be used for
CPE1, which represent the charge transfer resistance and the modeling frequency dispersion behavior, especially for the
capacitance of the passive film/electrolyte interface, respec- passive film of stainless steel. The CPE is defined as follows:
ZðxÞ ¼ Z0  ðixÞn ðEq 1Þ
0V
12000
0.2 V where the factor n, defined as the CPE power, is an
0.5 V adjustable parameter that changes from 0 to 1. A value of
10000 1.1 V n = 0 represents an ideal resistor, a value of n = 1 represents
2

Fitting an ideal capacitor, and a value of n = 0.5 indicates a Warburg

cm

8000
impedance. However, a value of 0.5 < n < 1 indicates a fre-
quency dispersion of time constants due to local hetero-
-Z'' /

6000
geneities in the dielectric material (Ref 28, 29).
4000
The fitting results of all impedances are given in Table 1. In
Table 1, when the applied potential is in the passive region, the
2000 value of R1 increased significantly with an increasing potential.
This indicates that there are some reactions that occurred at the
0 passive film/electrolyte interface, indicating that the passive
0 2000 4000 6000 8000 10000 12000 film formed at higher applied potential (0.5 VSCE) is more
2
Z' / cm stable and protective than that formed at a lower potential
(0 VSCE). However, when the applied potential is 1.1 VSCE in
10000 100 the transpassive region, R1 and R2 decrease sharply, indicating
0V the worse protection of the passive films, and a porous film was
0.2 V formed at this potential. Furthermore, the CPE1 decreases
0.5 V 80
1000
1.1 V
significantly. This relates to the chromic oxide dissolution of
Fitting the passive film, and the onset of the passive film dissolution is
2

60
/ deg.

due to the following reaction:

100 þ
Cr2 O3 þ 5H2 O ! 2CrO2
4 þ 10H þ 6e ðEq 2Þ
40
As shown in the value of n1, n1 has a lower at 1.1 VSCE than
10 that in the passive region. This further supports that a porous
20
film is formed at high potentials in the transpassive region.
3.2.2 The Effect of the Passive Time on the Electro-
1 0 chemical Behavior. To observe the relationship between the
0.01 0.1 1 10 100 1000 10000 100000
f / Hz applied potential time and the stability of passive film, a sample
was potentiostatically formed at 0.2 VSCE (in the passive
regions) during exposure times of 0.5, 1.0, 1.5 and 2.0 h. EIS
Fig. 2 Nyquist and Bode plots in neutral 1 wt.% NaCl solution at
several film formation potentials (0, 0.2 and 0.5 VSCE within the and OCP were conducted in neutral NaCl solution after the
passive region, and 1.1 VSCE within the transpassive region) passive film was formed with different applied times. Figure 4
shows the Nyquist plots of the Co-Cr-Mo stainless steel of the
passive film formed with different times in neutral 1 wt.% NaCl
solution at the OCP. As seen in the plots, the radius of the
capacitive arc increases with an increase in the applied time.
This indicates that a more protective passive film was obtained
after a longer formation time.
Figure 5 shows the evolution of the OCP values after the
passive film was formed at 0.2 VSCE with different applied
times. According to the experimental results, the OCP values
changed from 0.2 to 0.15 VSCE in neutral 1 wt.% NaCl
Fig. 3 Equivalent electrical circuits of the impedance spectra solution. The OCP value was 0.2 VSCE when the passive film

Table 1 Equivalent circuit fitting parameters of the impedance spectra

Potential, VSCE Rs, X cm2 R2, X cm2 CPE2, lF21 cm22 n2 R1, X cm2 CPE1, lF21 cm22 n1

0 12.52 413.1 4.25 9 105 0.7845 2.03 9 104 7.72 9 105 0.8814
0.2 2.438 421.8 3.56 9 105 0.8853 6.93 9 104 5.30 9 105 0.7384
0.5 3.316 476.9 2.89 9 105 0.816 8.13 9 104 2.76 9 105 0.7288
1.1 4.635 24.13 2.12 9 105 0.8697 6259 1.83 9 105 0.934

Journal of Materials Engineering and Performance

was formed without potentiostatic potential, but it changed with confirming that a passive film with better corrosion resistance
the applied time. Moreover, the OCP value shifted in the formed. This shows that a long passivation time (such as 2 h)
positive direction as the applied potential time increased, results in the formation of a more stable passive film (Ref 30,
31).
25000
0h 3.3 Surface Passive Film Composition in NaCl Solution
0.5 h
20000 The compositions of the passive films formed in NaCl
1.0 h
solution at pH 3 and pH 7 were analyzed by x-ray photoelec-
1.5 h
tron spectroscopy. The XPS peaks were separated into several
2
cm

15000 2.0 h
different oxidation states by a fitting procedure. Figure 6(a)
shows the spectra of Cr 2p3/2 after the passive film was formed
-Z'' /

10000 in pH 7 solution. The Cr 2p3/2 spectra can be separated into

three peaks. The peak at approximately 574.3 eV is attributed
to Cr(met), and the other two peaks at approximately 576.4 eV
5000 and 577.1 eV are due to the presence of the Cr2O3 and Cr
(OH)3 species, respectively. Figure 6(b) shows the Cr 2p3/2
0 spectra of the passive film that formed in pH 3 NaCl solution.
0 5000 10000 15000 20000 25000 The Cr 2p3/2 spectra can be divided into three peaks, also
2
Z' / cm showing Cr(met), Cr2O3 and Cr (OH)3 species. However, the
percentage of Cr (OH)3 decreased, and the Cr2O3 increased in
Fig. 4 Nyquist plots of the passive film in neutral 1 wt.% NaCl
solution after the surface passive film was formed at 0.2 VSCE with
different times (0.5, 1.0, 1.5 and 2.0 h)

-0.12
pH 3
Co3O4
OCP value

-0.14
Co
Intensity / a.u.
OCP (V vs.SCE)

-0.16

-0.18
pH=7

-0.20 pH 7 pH=3

-0.22 770 780 790 800 810

0.0 0.5 1.0 1.5 2.0
Binding Energy (ev)
Time (h)
Fig. 7 XPS spectra of Co 2p3/2 of the passive films obtained after
Fig. 5 Open-circuit potential in neutral 1 wt.% NaCl solution after passivation at 0.2 VSCE for 1.5 h in the pH = 7 and pH = 3 solution
the surface film was formed at 0.2 VSCE within the passive region
with different times (0.5, 1.0, 1.5 and 2.0 h)

Cr2O3
Cr2O3
Intensity / a.u.
Intensity / a.u.

Cr
Cr

Cr(OH)3 Cr(OH)3

570 572 574 576 578 580 582 570 572 574 576 578 580 582
(a) Binding Energy (ev) (b) Binding Energy (ev)

Fig. 6 XPS spectra of Cr 2p3/2 of the passive films obtained after passivation at 0.2 VSCE for 1.5 h in pH = 7 (a) and pH = 3 (b) solution,
respectively

Journal of Materials Engineering and Performance

the acidic solution in comparison with the passive film formed CrðOHÞ3 þ Cr ! Cr2 O3 þ 3Hþ þ 3e ðEq 3Þ
in neutral solution.
Previous studies (Ref 32) have noted that chromic hydroxide The main reason for this is the fact that the ratio of chro-
is more stable in neutral and alkaline solution. However, in mium oxide obtained in the acidic solution is much higher
acidic environment with increase in oxidizing power it is easier than that in the neutral solution. The Fe 2p3/2 spectra are
to convert to chromium oxide via the following reaction: separated into several peaks (the fitting of the peaks is not
presented here), representing a metallic state (Fe(met)) and
bivalent (Fe2+) and trivalent (Fe3+) species. No significant dif-
ference is observed between the Fe 2p spectra of the passive
Auger peak of Fe film formed in neutral or acidic solution. Moreover, no peaks
in the Ni 2p3/2 spectra of the passive film were detected in
both neutral and acidic solutions. These results coincide with
the published work (Ref 33, 34), which report that little or no
nickel participate in the passive film of stainless steel.
Intensity / a.u.

Figure 7 shows the decomposition of the Co 2p spectra

formed in NaCl solution at pH 7 and pH 3. It can be seen that
only a little amount of Comet appears after the passive film is
formed at pH 7. Both the Comet and Co oxide are observed at
Co3O 4 pH 3.
The peak fitting of the Co 2p3/2 spectra of the film formed
Co in the pH 3 solution is displayed in Fig. 8. The Co 2p3/2 peak
can be separated into several peaks. It is obvious from Fig. 8
that the peak at 777.9 eV is due to the presence of Comet and
777 780 783 786 789 792 795
that the other peak at 780.3 eV is attributed to Co3O4.
Binding Energy (ev)
Moreover, two Fe Auger peaks appeared in the peaks, which
are consistent with previous studies (Ref 35), and the E-pH
Fig. 8 Detailed XPS spectra of Co2p3/2 of the passive films ob- diagram of the cobalt-water system (Ref 36).
tained after passivation at 0.2 VSCE for 1.5 h in pH 3 solution

Mo3d 6+
Mo3d
6+
Mo 3d5/2 Mo 3d5/2
4+
Mo 3d3/2 6+
Mo 3d3/2
Intensity / a.u.

Intensity / a.u.

4+
Mo 3d5/2
Mo3d5/2 Mo3d5/2
6+
Mo 3d3/2

Mo3d3/2 Mo3d3/2

222 225 228 231 234 237 240 222 225 228 231 234 237 240

(a) Binding Energy (ev) (b) Binding Energy (ev)

Fig. 9 Detailed XPS spectra of Mo 3d of the passive films obtained after passivation at 0.2 VSCE for 1.5 h in the pH = 7 (a) and pH = 3 (b)
solution

-
- OH
OH
Intensity / a.u.

H2O
Intensity / a.u.

2-
O
H 2O

2-
O

526 528 530 532 534 536 538 522 525 528 531 534 537
(a) Binding Energy (ev) (b) Binding Energy (ev)

Fig. 10 Detailed XPS spectra of O1 s of the passive films obtained after passivation at 0.2 VSCE for 1.5 h in the pH = 7 (a) and pH = 3 (b)
solution

Journal of Materials Engineering and Performance

 Figure 9(a) and (b) shows the high-resolution spectra of Mo
3d of the films obtained in neutral and acidic solutions. We note
that the Mo 3d spectra can be divided into several peaks:
metallic (Momet), tetra-valent Mo4+ (233.4 eV) and hexa-valent
Mo6+ (235.1 eV) species. It is difficult to distinguish the spectra
owing to the very similar energy levels of Mo 3d3/2 and Mo
3d5/2. As depicted in Fig. 9, the Mo contained in the passive
film obtained in neutral solution is in the form of metallic, tetra-
valent and hexa-valent species. The hexa-valent (Mo6+) species
is the main species in the passive film. Nevertheless, the passive
film formed in acidic solution mainly contains metallic (Momet)
and hexa-valent (Mo6+) species. As is known, Mo6+ is probably
attributed to Fe2(MoO4)3 or MoO3 species in stainless steel
(Ref 37). Thus, it can be concluded that the Mo 3d spectra of
films from neutral and acidic conditions are different. Mo6+ is
the primary molybdenum oxidized species in the passive film in
both neutral or acidic solutions. However, there is no Mo4+
species in the passive film formed in the acidic conditions.
Figure 10(a) and (b) shows the XPS spectra of O1 s of the
films from neutral and acidic solutions, respectively. The O 1 s
spectra can be split into three components: O2(530.2 eV),
OH (531.8 eV) and H2O (533 eV). The intensity of the OH
peak is much greater than that of the O2 species, indicating
that OHis the primary oxygen constituent of the passive film
from the neutral NaCl solution. As shown in Fig. 10(b), the
main oxide compositions of the passive film generated from
acidic solution are also the O2, OHand H2O species, but the
intensity of O2is much stronger than the OH, indicating that
the O2is the primary oxygen constituent of this passive film.
The O2species in the passive films are related to the formation
of iron, chromium or cobalt oxides.
4. Conclusions
The electrochemical behavior of ultrahigh-strength stainless
steel in neutral and acidic chloride solution was evaluated by
potentiodynamic polarization curves and EIS. The surface
passive film composition was observed by XPS. The following
conclusions can be made:
The results of the polarization curves showed that the Co-
Cr-Mo ultrahigh-strength stainless steel exhibited good passive
properties in neutral chloride solution. EIS data revealed that
the formation potential of the passive film had a great effect on
the corrosion resistance of the stainless steel. The corrosion
resistance increased with an increase in the potential in the
passive region, and it sharply decreased when the potential was
in the transpassive region. Moreover, the corrosion resistance
also increased with an increase in the applied potential time and
became stable after a long time. Based on the XPS results of the
passive film formed in neutral and acidic solution, the primary
constituents of the passive films were compounds of Fe, Cr, Co
and Mo oxides, and no Ni oxides were detected. Nevertheless,
the content of the Cr, Co and Mo oxides changed in the
solutions of different pH.
Acknowledgments
This work is supported by the National Natural Science
Foundation of China (No. 51401076), Natural Science Foundation
of Jiangsu Province of China (BK20140849) and Jiangsu Innova-
tion and Entrepreneurship (Shuangchuang) Program.
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