Corrosion Science 109 (2016) 246–256

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Corrosion Science
journal homepage: www.elsevier.com/locate/corsci

Passivation of X65 (UNS K03014) carbon steel in NaHCO3 solution in a

CO2 environment
Lining Xu ∗ , Hui Xiao, Weijing Shang, Bei Wang, Jinyang Zhu
Corrosion and Protection Center, Key Laboratory for Environmental Fracture (MOE), Institute for Advanced Materials and Technology, University of Science
and Technology Beijing, Beijing 100083, China

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

Article history: In this study, the use of NaHCO3 as a pH stabilizer for the corrosion control of X65 (UNS K03014) carbon
Received 6 January 2016 steel in different environments was experimentally investigated. The experiments were conducted at
Received in revised form 2 April 2016 room temperature and at 50 ◦ C in 0.5 M NaHCO3 solutions purged with CO2 . Electrochemical tests were
Accepted 12 April 2016
conducted in a high-pressure, high-temperature autoclave. The constituents of the corrosion products
Available online 13 April 2016
were investigated through scanning electron microscopy and X-ray diffraction. The results showed that
X65 steel can be passivated in 0.5 M NaHCO3 solution in a CO2 environment. Immersion in 0.5 M NaHCO3
Keywords:
solution in a high-pressure, high-temperature autoclave resulted in the formation of a dense corrosion
CO2 corrosion
X65 steel
film on the surface of the X65 steel.
pH stabilization
© 2016 Elsevier Ltd. All rights reserved.
Sodium bicarbonate
Passivation

1. Introduction an acceptable level [13]. After pH stabilization in the pipelines of

Gathering pipelines in the petroleum industry is commonly
fabricated from carbon steel because of its low costs, but CO2
corrosion is a frequently encountered problem. The dissolution
mechanisms of carbon steel at high temperatures and pressures
in CO2 -containing environments have been debated for more than
60 years, and numerous studies have investigated the parameters
influencing its corrosion rate and behavior [1–5]. pH stabiliza-
tion is an economic method of inhibiting CO2 corrosion in subsea
pipelines. Theoretically, any alkali that can increase pH can be used
as a pH stabilizer.
The combination of glycol and pH stabilizer has been success-
fully used for protecting wet gas pipelines from internal corrosion
[6–8]. NaHCO3 , one of the most commonly used pH stabilizers, was
initially used for treating two pipelines in Troll field, Norway [9].
However, pH stabilizer cannot be applied in pipelines carrying large
quantities of formation water because such water contains sub-
stances that may precipitate as CaCO3 at high pH. Furthermore, the
use of scale inhibitors may degrade the protective FeCO3 films in
carbon steel pipelines and thus increase corrosion [10–12]. In the
gas-condensate pipelines of Vega field, 30 mmol/kg of pH stabilizer
in glycol was adequate in restricting the general corrosion rate to
∗ Corresponding author.
E-mail addresses: xulining@gmail.com, xulining@ustb.edu.cn (L. Xu).
Ormen Lange field at CO2 partial pressures and temperatures of
0.30–0.82 MPa and 0–85 ◦ C, respectively, the corrosion rate deter-
mined using a test program was less than 0.10 mm/year [14].
Early relevant literatures indicate that carbon steel can be pas-
sivated in NaHCO3 solution, and the electrochemical reactions for
this system have been defined [15–22]:
Fe+HCO− +
3 → FeCO3 +H +2e (1)
Fe+2H2 O → Fe(OH)2 +2H+ +2e (2)
3FeCO3 +4H2 0 → Fe3 04 +3HCO−
3
+
+5H +2e (3)
FeCO3 + HCO− 2−
3 → Fe(CO3 )2 + H
+
(4)
Some studies have reported the dual effects of bicarbonates:
They exacerbated dissolution at low concentrations and promoted
passivation at high concentrations. Brasher reported that bicarbon-
ates do not function as a protective element at a concentration of
less than 0.006 M [23]. Eliyan et al. determined that the corrosion
rate of X100 steel after immersion in 10 g/L NaHCO3 solution for 2
days (16 g m−2 day−1 ) was notably higher than that after immer-
sion in 50 g/L NaHCO3 solution (0.28 g m−2 day−1 ) [1]. Moreover,
they reported that the anodic peaks in the passivation region were
likely associated with FeCO3 oxidation and the transformation of
Fe3 O4 or FeCO3 to ␥-Fe2 O3 . Tan et al. found that bicarbonate ions
had a beneficial effect on the charge transfer resistance, the criti-
cal chloride threshold concentration and the pitting potential [24].

http://dx.doi.org/10.1016/j.corsci.2016.04.012
0010-938X/© 2016 Elsevier Ltd. All rights reserved.
 L. Xu et al. / Corrosion Science 109 (2016) 246–256
Fig. 1. Schematic illustration of high pressure high temperature autoclave for OCP and potentiodynamic polarization curves measurements.
Fig. 2. Schematic illustration of an electrochemical autoclave for solution pH mea-
surements.
Deodeshmukh et al. showed that the presence of 0.5 M HCO3 − ions
in 3.5% NaCl solution (pH 8.5) increased the pitting potential of
medium strength carbon steel by 150 mV [25]. In some studies,
precipitation of FeCO3 as a result of direct oxidation was a valid
hypothesis describing the dissolution of ferrite in bicarbonate solu-
tions for specific ranges of anodic polarization [22]. In other studies,
Fe(OH)2 was reported to be an inner layer underlying FeCO3 , form-
ing a multilayered passivation film [26–33]. Valentini and Moina
considered the formation of Fe(OH)2 as the onset of passivation
[34]. In the current study, the morphology and composition of the
corrosion film that formed after immersion for various durations
were studied. It may further the understanding of passivation in
CO2 –NaHCO3 systems.
2. Experimental procedures
2.1. Electrode and solution
The experimental specimens used in this study were con-
structed from X65 pipeline steel; its chemical composition was as
follows (wt.%): C, 0.04; Si, 0.2; Mn, 1.5; P, 0.011; S, 0.003; Mo, 0.02;
and Fe (rest). All specimens were polished using #600, 800, 1000,
1500, and 2000 SiC grit, rinsed with deionized water, and degreased
in acetone. NaHCO3 solutions (0.5 M and 0.05 M) made from analyt-
ical grade reagents and deionized water were used as test solutions.
The solutions were deoxygenated by purging with CO2 for 12 h; the
solutions were continuously purged throughout the tests.
247
Fig. 3. Polarization curve for X65 steel using RDE specimens (2000 rpm) in CO2 -
saturated solutions.
2.2. Rotating disk electrode tests
A three-electrode system was used for the experiments: a steel
rotating disk electrode (RDE), platinum electrode, and saturated
calomel electrode (SCE) were used as the working electrode (WE),
counter electrode (CE), and reference electrode (RE), respectively.
When the open-circuit potential (OCP) of WE relatively stabilized,
potentiodynamic polarization curves were measured using a Par-
stat 4000 electrochemical system at a potential scanning rate of
0.5 mV/s from −1.00 to 0.55 V (SCE) at 2000 rpm and room temper-
ature; the solution was saturated with CO2 . The RDE tests under
different rotating speeds, 250, 350, 400, 500, 1000 and 2000 rpm,
had been done. The repeatability of the potentiodynamic polariza-
tion curves under 2000 rpm was best, so 2000 rpm was chosen as
the rotating speed.
2.3. Autoclave tests
A high-pressure high-temperature autoclave (Fig. 1) containing
2 L of the test solution were used to monitor the OCP and measure
the potentiodynamic polarization curves at a CO2 partial pressure
of 0.7 MPa and a temperature of 50 ◦ C. The autoclave tests differed
from the RDE tests in that an Ag/AgCl high-pressure electrode was
248 L. Xu et al. / Corrosion Science 109 (2016) 246–256

Fig. 4. The morphologies of the corroded surface of the specimen at potential a provided in Fig. 3 by SEM and EDS analysis of different regions on the specimen.

Fig. 5. The morphologies of the corroded surface of the specimen at potential b provided in Fig. 3 by SEM and EDS analysis of different regions on the specimen.

Fig. 6. The morphologies of the corroded surface of the specimen at potential c provided in Fig. 3 by SEM and EDS analysis of different regions on the specimen.
 L. Xu et al. / Corrosion Science 109 (2016) 246–256 249

Fig. 7. The changes in OCP of X65 steel in CO2 -saturated 0.5 M NaHCO3 solution.

Fig. 8. The morphologies of the corroded surface of the specimen at potential a provided in Fig. 7 by SEM and EDS analysis of different regions on the specimen.

used as the RE and the test was conducted under a static condi-
tion. The WEs were embedded in epoxy resin and had an exposed
area of 10 × 10 mm2 . The OCP was recorded using Fluke 289c at
6 points/min. After the immersion tests, the corroded specimens
were removed from the autoclave, and the morphology of the cor-
rosion scale was observed through scanning electron microscopy
(SEM). Three tests were conducted in 0.5 M NaHCO3 solution with
immersion times of 10 min, 0.5 h, and 6 h. In addition, one test was
conducted in 0.05 M NaHCO3 solution with an immersion time of
6 h. The potential was scanned from −1.00 to 0.55 V at 0.5 mV/s.
An electrochemical autoclave (Fig. 2) was used to simultane-
ously monitor the pH and OCP of the solutions. The WEs were
embedded in epoxy resin and had an exposed area of 10 × 10 mm2 .
A ZrO2 -based electrode and an Ag/AgCl electrode, placed close to
the WE surface (Fig. 2), served as the pH probe; the pH of the solu-
tion between these electrodes was measured. pH-immersion time
curves were automatically recorded in a computer, and the OCP
was monitored using another Ag/AgCl electrode. The CO2 partial
pressure was 0.7 MPa and the temperature was 50 ◦ C.
2.4. Analysis of corrosion products
After the tests, the surfaces of the specimens were rinsed with
deionized water and dried with a cold dry wind. Subsequently,
the surface morphologies of the corrosion scales were observed
through SEM (LEO-1450), and their composition was investigated
through energy dispersive X-ray spectroscopy (EDS, KevexSigma)
and X-ray diffraction (XRD, D/MAX-RB) using Cu K␣ radiation.
250
Fig. 9. The morphologies of the corroded surface of the specimen at potential b provided in Fig. 7 by SEM and EDS analysis of different regions on the specimen.
4000
3000
CPS-Intensity
2000
1000
0
20
Fig. 10. XRD patterns of the corroded surface of the specimen at potential b provided in Fig. 7.
3. Results
3.1. Polarization curve and surface analysis of RDE specimens
Fig. 3 shows the polarization curve for X65 steel in CO2 -
saturated solutions with 0.5 M NaHCO3 (with a pH of 8.06 at room
temperature) obtained using RDE specimens (2000 rpm). Clearly,
X65 steel can be passivated in NaHCO3 solution. Three corrosion
potentials and two oxidative current peaks were observed.
Subsequently, three individual fresh specimens were polarized
to potentials a, b and c (approximately −500, −400, and −100 mV
(SCE); Fig. 3) from approximately −1000 mV (SCE), with the scan
L. Xu et al. / Corrosion Science 109 (2016) 246–256
1
1-Fe
2-FeCO3
2
2
1
2 2 2 2 2
40 60 80
2 theta °
rate of 0.5 mV/s, then the specimens were removed from the CO2 -
saturated solutions for surface observation through SEM and EDS.
Figs. 4–6 illustrate the morphologies of the corroded surface of the
X65 and the EDS results of different specimen regions. As shown
in Fig. 4, a thin corrosion film formed on the surface of the steel
substrate. On polarization to potential b, the corrosion film became
nearly identical to that at potential a in terms of both morphology
and composition. On polarization to potential c, Na was present in
the corrosion film (Fig. 6). The cross section morphology of RDE
specimen after polarisation was observed, and no film was found
on steel surface. Because the film was thin, it may peel off during
the preparation of cross section sample.
 L. Xu et al. / Corrosion Science 109 (2016) 246–256 251

Fig. 11. The morphologies of the corroded surface of the specimen at potential c provided in Fig. 7 by SEM and EDS analysis of different regions on the specimen.

3.2. Immersion of X65 steel in a high-pressure, high-temperature
autoclave for one week
3.2.1. Ennoblement of X65 steel under high pressure and
temperature
When X65 steel was immersed in a high-pressure, high-
temperature autoclave containing 2 L of CO2 -saturated 0.5 M
NaHCO3 solution for one week, the OCP of X65 shifted toward the
noble direction, as shown in Fig. 7. In the first 2 h, the OCP increased
slightly to approximately −750 mV (Ag/AgCl) and then began to
appreciably shift toward the noble direction. After a sharp increase,
the potential changed by 600 mV within 1 h, and the OCP stabi-
lized at approximately −100 mV (Ag/AgCl). Subsequently, the OCP
increased marginally with time.
Four individual fresh specimens were immersed to potentials
a, b, c, and d (approximately −710, −380, −100, and −35 mV
252 L. Xu et al. / Corrosion Science 109 (2016) 246–256
4000
CPS-Intensity
3000
2
2000
2
1000
2 2 2
0
20
Fig. 12. XRD patterns of the corroded surface of the specimen at potential c provided in Fig. 7.
(Ag/AgCl); Fig. 7); their surface morphologies were observed after
removing the specimens from the solution. As shown in Fig. 8,
the corrosion film gradually covered the steel surface in the first
2 h. Fig. 9 presents the morphologies of the corroded surfaces at
the beginning of the sharp increase in the potential, and Fig. 10
depicts the corresponding XRD patterns. The main constituent of
the corrosion film covering the steel surface was FeCO3 . Epoxy
resin, which was used for sealing the specimens, may be responsi-
ble for the amorphous pattern in the spectra. It’s worth noting that
high-magnification images (8000 × ) of the film morphology (Fig. 9)
revealed disordered precipitation on FeCO3 film surface. The disor-
dered substance containing the elements Fe Na and O gradually
covered the FeCO3 film, as shown in Figs. 9 and 11. The disordered
substance continuously precipitated with an increase in the OCP
of X65. It is guessed that the precipitation of disordered substance
elevated OCP. XRD patterns of the corroded surface at potential c
(Fig. 12) show that the main constituent of crystalline corrosion
product was FeCO3 . At potential d, crystalline substance contain-
ing the element Na was observed along the FeCO3 grain boundary
(Fig. 13). The specimens were removed from solution after the auto-
clave cooled down. Crystalline substance containing Na may form
during this period. Fig. 14 shows the cross sectional morphology
of corrosion film at the immersion time of 168 h (potential d). The
thickness of the corrosion film was not uniform, and the maximum
thickness was about 9 ␮m.
3.2.2. Anodic polarization curves of X65 steel after immersion for
different durations
After immersion in 0.5 M NaHCO3 for 6 h in the high-pressure,
high-temperature autoclave, the OCP of X65 shifted toward the
noble direction, as shown in Fig. 15(a) (the first 6 h in Fig. 7);
moreover, after immersion in 0.05 M NaHCO3 for 6 h, the OCP
of the specimens increased slightly (to approximately −650 mV
(Ag/AgCl)), as shown in Fig. 15(b). Anodic polarization curves of X65
steel immersed in 0.5 M and 0.05 M NaHCO3 for 6 h are depicted
in Fig. 15(c). The pH value of the solution surrounding the sur-
face of the specimens at 0.5 M NaHCO3 for 6 h (0.7 MPa CO2 , 50 ◦ C)
was 6.75, and that of 0.05 M NaHCO3 was 5.37. After immersion in
0.5 M NaHCO3 solution for 6 h, X65 steel exhibited self-passivation,
whereas after immersion in the 0.05 M NaHCO3 solution, the high
potential resulted in the electrochemical passivation of X65 steel.
1
1-Fe
2-FeCO3
1
2 2
40 60 80
2 theta °
Moreover, the corrosion current density in the 0.05 M NaHCO3
solution was considerably higher than that in the 0.5 M NaHCO3
solution. Therefore, NaHCO3 concentration is crucial in the passi-
vation of X65 steel. Furthermore, there must be a critical NaHCO3
concentration level above which steel can be passivated. Anodic
polarization curves of X65 steel immersed in 0.5 M NaHCO3 for
10 min, 0.5 h, and 6 h are displayed in Fig. 15(d). When X65 was
immersed for 10 min and 0.5 h, the high potential resulted in its
electrochemical passivation. The result for the 0.5 h immersion
indicates that the corrosion film gradually covered the steel sur-
face. By contrast, after immersion for 6 h, disordered precipitation
was observed on the surface of the FeCO3 film. This disordered pre-
cipitation was critical in realizing the self-passivation capability of
the X65 steel.
Anodic polarization curves of X65 steel immersed in 0.5 M
NaHCO3 for 6 h and 7 days are shown in Fig. 16. The OCP of X65
immersed for 7 days is higher than that for 6 h, and the corrosion
current density after immersion for 7 days is lower than that after
6 h. This result suggests that after immersion in 0.5 M NaHCO3 for
more than 6 h, the X65 steel retained the self-passivation capability
with an increase in time.
3.3. In-situ pH monitoring curves of X65 steel after immersion for
hours
The OCP and pH-immersion time curves of X65 steel after
immersion in the electrochemical autoclave for hours are pre-
sented in Fig. 17. Evidently, after approximately 3 h, the pH value
of the solution surrounding the surface of the specimens started to
decrease, whereas the OCP shifted toward the positive direction.
After approximately 6 h, the pH and OCP became almost steady,
indicating that a decrease in the pH value can affect the precipita-
tion by changing the critical supersaturation ratio [35–37], which
may lead to variations in the OCP.
4. Discussion
According to Reaction (1), the H+ ion concentration increases
with the amount of FeCO3 formation, leading to a decrease in the
pH value. The decrease in the pH value in turn increases the critical
supersaturation of FeCO3 ; therefore, the nucleation rate is higher
 L. Xu et al. / Corrosion Science 109 (2016) 246–256 253

Fig. 13. The morphologies of the corroded surface of the specimen at potential d provided in Fig. 7 by SEM and EDS analysis of different regions on the specimen.

than the particle growth rate, resulting in the formation of a disor-
dered substance, probably amorphous FeCO3 [38–40]. As shown in
Fig. 8, the large grain size of FeCO3 resulted in large spaces between
the grains, which in turn led to the porous structure of the FeCO3
films. According to Figs. 9 and 10, after approximately 2 h of immer-
sion of X65 steel in the high-pressure, high-temperature autoclave,
the formation of the amorphous substance that formed a dense
corrosion film filled the spaces between the grains. The formation
of the corrosion film increased the OCP of X65 steel, resulting in
the passivation of the steel. After approximately 6 h, the pH value
and OCP of X65 steel almost stabilized. The X65 steel retained the
self-passivation capability with an increase in time, as shown in
Fig. 16.
5. Conclusions
The X65 steel was passivated in 0.5 M NaHCO3 solution in CO2
at 50 ◦ C and 0.7 MPa. Immersion in this condition resulted in the
254 L. Xu et al. / Corrosion Science 109 (2016) 246–256

Fig. 14. Cross sectional morphology of corrosion film at the immersion time of 168 h (potential d).

Fig. 15. The changes in OCP and polarization curves of X65 steel in CO2 -saturated test solutions: (a) the changes in OCP after immersion in 0.5 M NaHCO3 for 6 h; (b) the
changes in OCP after immersion in 0.05 M NaHCO3 for 6 h; (c) anodic polarization curves of X65 steel after immersion in 0.5 M and 0.05 M NaHCO3 for 6 h; (d) anodic
polarization curves of X65 steel after immersion in 0.5 M NaHCO3 for 10 min, 0.5 h and 6 h.
 L. Xu et al. / Corrosion Science 109 (2016) 246–256 255

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-0.6
-0.8
10000 20000
t (s)
Fig. 17. The OCP and pH-immersion time curves of X65 steel after immersion for
hours.
direct formation of a dense corrosion film on the surface of X65
steel that can protect the steel from corrosion. After immersion for
hours, the OCP of X65 steel appreciably shifted toward the noble
direction, and disordered precipitation containing the elements Fe
Na and O on the surface of the FeCO3 film was observed.
Acknowledgments
The authors thank Jin Zhang, Wei Li and Ziyi Zheng for their help.
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