Electrochemical and SEM study on Type 254 SMO stainless steel in chloride solutions
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Transcript of Electrochemical and SEM study on Type 254 SMO stainless steel in chloride solutions
www.elsevier.com/locate/corsci
Corrosion Science 46 (2004) 2431–2444
Electrochemical and SEM study on Type 254SMO stainless steel in chloride solutions
E.A. Abd El Meguid *, A.A. Abd El Latif
Department of Electrochemistry and Corrosion, National Research Centre, Dokki, Cairo, Egypt
Received 30 April 2003; accepted 29 January 2004
Available online 30 April 2004
Abstract
An investigation was conducted to examine the critical crevice potential (Ecrev) and the
critical protection potential (Eprot) for Type 254 SMO stainless steel in 4% NaCl solution by
using potentiodynamic cyclic anodic polarization (PCAP) technique at temperature ranging
from 30 to 90 �C. The critical crevice temperature (CCT) and the critical crevice protection
temperature (Tprot) were determined by plotting the values of breakdown potential and Eprot
versus solution temperature, respectively. The values of CCT and Tprot were recorded at the
abrupt transition with increasing the temperature from transpassive corrosion to crevice
corrosion and were found to be at 55 and 52 �C, respectively. Above CCT (70 �C) the fol-
lowing points were recorded. The Ecrev and Eprot decreased linearly with log [Cl�]. The addition
of bromide ions to chloride ions at a fixed halide content of 4% increased both Ecrev and Eprot.
The Ecrev value in 4% NaCl increased linearly with increasing pH in the range 1–10. The
addition of 0.5 M bicarbonate ions to 4% NaCl completely removed the crevices effect while
increasing the addition of sulphate ions to 4% NaCl increased both of Ecrev and Eprot. The
morphology of the crevice corrosion produced on the steel surface was examined by scanning
electron microscope (SEM) after PCAP treatment under different test conditions.
� 2004 Elsevier Ltd. All rights reserved.
Keywords: Stainless steel; Temperature; Crevice corrosion potential
1. Introduction
Type 254 SMO stainless steel has been recently used in condenser tubes of desali-nation plants instead of copper base alloys because it has better corrosion resistant and
* Corresponding author. Fax: +20-2-337-0931.
E-mail address: [email protected] (E.A. Abd El Meguid).
0010-938X/$ - see front matter � 2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.corsci.2004.01.022
2432 E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444
environmentally more friendly [1]. This steel is one of the high strength molybdenum
containing stainless steels which were studied in Arabian Gulf water [2], in reverse
osmosis (RO) and multi-stage flash (MSF) evaporation plants in the Middle East [3]
and in North Sea offshore oil industry [4]. The factors affecting the corrosion properties
of high strength molybdenum containing stainless steels in seawater such as compo-
sition, weldability, biofilm formation, pollution and chlorination are also studied [5,6].The excellent corrosion resistance of a Type 254 SMO stainless steel in chloride solution
is due to the synergistic action of the alloying elements [7]. Therefore, a comparative
study was carried out between the Type 254 SMO and Hastelloy C276 in HCl media [8].
A Type 254 SMO stainless steel was developed by using 6% molybdenum as an alloying
element to stabilize the passive film in chloride-containing media and thus reduce
susceptibility to crevice corrosion. Many models of the chemistry and potential in
crevices have been developed for predicting the initiation and propagation of the cre-
vice attack on stainless steel surfaces [9–13]. The models vary in their range of appli-cability as highlighted by Laycock et al. [14]. There is considerable interest in the
behaviour of crevices formed on the high molybdenum stainless steel due to the increase
in their application in the desalination plant [15] and other industries.
The purpose of the present investigation was to study the CCT and the Tprot in 4%
NaCl. The investigation was also extended to study some environmental factors such
as the influence of chloride ions concentration, pH, addition of bromide ions to
chloride ions at a fixed total halide of 4%, addition of sulphate ions and bicarbonate
ions to 4% NaCl on both Ecrev and Eprot at 70 �C. The surface morphology of thecrevices was examined after PCAP treatment in some of the previous test solutions.
2. Experimental details
The electrodes were cut from 1 mm thick sheet of a UNS S 31254 (254 SMO)
stainless steel supplied by Avesta AB (Sweden), with the following chemical com-
position (W%) 0.017 C, 17.9 Ni, 19.7 Cr, 6 Mo, 0.195 N, 0.7 Cu and balance Fe. A 1
mm thick sheet of 254 SMO was cut into discs of 14 mm in diameter as electrodes for
electrochemical measurements. These electrodes were polished with emery paper down
to 1000 grit. Then they were finely polished with 0.05 lm alumina paste, ultrasonically
cleaned and finally rinsed with double distilled water. The disc electrode to be crevicedwas pressed onto a PTFE disk crevice former at a constant torque of 5 in. lb (0.56
Nm). This torque was found to produce a crevice gap of 4 lm, found by determining
the amount of the solution contained in the crevice when torqued to 5 in. lb given that
diameter of the crevice. The assembly of the creviced disc electrode is shown in Fig. 1.
The assembly of the creviced disc electrode was introduced to a conventional
electrolytic cell of 500 ml contained the test solution. Electrical connection to the
sample was made through an isolated Cu wire. All test solutions were prepared from
analytical grade reagents and double distilled water. The experiments were conductedunder thermostat condition at a desired temperature ranging from 30 to 90 �C.
The electrolytic cell had three openings and was attached to condenser to avoid
evaporation of the electrolyte at elevated temperatures. A saturated calomel electrode
Disc ElectrodeRubber O Ring PTFE
Cu DiscPTFE Cover
Cu Wire
Rubber Cover
Fig. 1. Assembly of the crevice disc electrode.
E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444 2433
(SCE) was used as the reference electrode and all potentials quoted here refer to this
scale. A 10 cm length of 3 mm diameter graphite rod was used as the counter electrode.
The PCAP measurements were carried out for the steel in different solutions by using
a Potentiostat/Galvanostat Model 263A EG & G PARC connected to a fully
compatible IBM computer and controlled by EG & G model 352 CorrosionMeasurement and Analysis Software. PCAP experiments at 5 mV s�1 were utilized
to determine breakdown potential and Eprot at different temperatures. Ecrev was
determined potentiodynamically and reported as the potential at which the current
density continuously exceeds 100 lAcm�2 and Eprot was determined potentiodynam-
ically at the same scan rate as a potential at which the current density goes below 100
lAcm�2 in the reverse scan. At a situation where Eprot was the same as open circuit
potential value on the reverse scan, in such cases Eprot becomes the lowest value
recorded. Three measurements were made for each experimental condition. The valueof 100 lAcm�2 was chosen because it is corresponding to a marked deviation from the
passive current density which was in the range of 5–50 lAcm�2 depending on the
experimental temperature. At the end of each experiment, the sample was examined
microscopically. In most cases, crevice corrosion was successfully observed. The CCT
and the Tprot for crevice were determined at the abrupt transition with increasing the
temperature from transpassive corrosion to crevice corrosion when breakdown
potential and Eprot are plotted versus temperature, respectively. The temperature
figures given here refer to the temperature of the solution.
3. Results and discussion
3.1. Critical crevice and protection crevice potentials
Fig. 2a–c shows the PCAP curves of creviced 254 SMO steel obtained in 4% NaCl
at 32, 55 and 90 �C. The curves generally reveal that as the temperature increased,
2434 E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444
the passive current density increased and the breakdown potential decreased, which
made the solution more aggressive. At 32 �C there was a broad passive region with a
passivation current density of 10 lA cm�2 without any sign for localized corrosion
breakdown until the oxygen evolution with a little hysteresis loop on the reverse scan
was observed. This hysteresis loop should be attributed to the dissolution in the
transpassive region [16]. While at 55 �C the PCAP curve (Fig. 2b) indicated thepresence of crevice corrosion breakdown potential at 571 mV which sustained anodic
current density of 100 lA cm�2. On the backward anodic scan a hysteresis loop was
detected. The occurrence of the hysteresis loop is related to the presence of aggressive
solution formed inside the occluded area which maintained when the potential was
reversed. Therefore, it was clear that the increase in the temperature significantly
decreased the breakdown potential. Before crevice corrosion initiation, the aggres-
siveness of the solution inside the crevice was determined by the passive current
density and the geometry of the crevice. The crevice corrosion initiation occurs whenthe solution pH became lower than certain critical pH, thus the current inside the
crevice increased by orders of magnitude, which led to further lowering in the pH as
a result of hydrolysis. The large number of metal ions being dissolved attracted
chloride ions from outside for neutralizing charges. The solution inside the crevice
became saturated with metal chlorides. Precipitation of a very thin salt film occurred
until the metal ion flux across the salt layer was balanced with the diffusion flux out
of the crevice [17]. During the propagation, the solution inside the crevice was a
saturated chloride solution. When the potential was reversed to obtain the protectionpotential value, it was the active corrosion current density and not the passive
current density that determined Eprot. The active corrosion current is a function in
several parameters such as the potential and temperature. At 90 �C the PCAP curve
10-7 10-5 10-3 10-1
-400
-200
0
200
400
600
800
1000
1200
cba
E,m
V SCE
Current Density,(A/cm2)
(a) 32oC (b) 55oC (c) 90 oC
Fig. 2. PCAP curves of creviced sample of Type 254 SMO stainless steel in 4% NaCl with potential scan
rate 5 mV s�1 at (a) 32 �C, (b) 55 �C and (c) 90 �C.
E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444 2435
(Fig. 2c) revealed that the experimental condition became suitable for localized
corrosion attack (both of pitting and crevice corrosion); this result is in agreement
with that the CPT for Type 254 SMO was around 90 �C for this alloy in chloride
solution [18,19].
Fig. 3 represents SEM micrographs of a Type 254 SMO steel surface obtained
after PCAP treatment in 4% NaCl at different temperatures. The micrograph of thesurface obtained after PCAP treatment in 4% NaCl at 32 �C shows a passive surface
without any localized attack (Fig. 3a). At 55 �C, an evidence of strong crevice cor-
rosion contains a large number of small pits and a micro-crack was seen at the
boundary between the passive area and the crevice corrosion one, the micro-crack
Fig. 3. Effect of temperature on crevice morphology of Type 254 SMO stainless steel obtained after PCAP
treatment in 4% NaCl at (a) 32 �C, (b) 55 �C and (c) 90 �C. High magnification (c) for pit and crevice are
shown at (d) and (e).
2436 E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444
was formed from gathering a large number of small pits (Fig. 3b). With raising the
temperature to 90 �C, an aggressive cracked crevice corrosion with strong pitting
attack on the passive part of the surface were observed (Fig. 3c). The magnification
of the crevice corrosion area and the pitting corrosion formed on the passive part of
the steel surface is shown in Fig. 3d and e, respectively. It was clear that crevice
corrosion area consistent of roughened part which contains a small pits and strongunderneath attack at the boundary with the passive area. This means that crevice
corrosion initiated under the crevice at a critical potential and critical temperature
where the crevice solution can change the metastable pitting to stable ones. The
condition in this work could lead to an aggressive attack approximately similar to
that reported for a Type 254 SMO in seawater using immersion technique [20].
3.2. The critical crevice and protection temperatures
The transition from passive state to crevice corrosion with the increasing in
temperature indicates that the steel resistance to crevice corrosion decreases with
raising the solution temperature. The relationship between both of breakdown po-
tential and Eprot with temperature is utilized for determination of CCT and the
critical protection temperature, respectively, for 254 SMO steel in 4% NaCl solution.
The curves are characterized by S-shape as shown in Fig. 4. It was clear that at acertain temperature there was an abrupt decrease in both breakdown potential and
Eprot. This transition from transpassive dissolution to crevice corrosion is defined as
CCT (temperature below which stable crevice corrosion will not occur at any po-
tential for a given alloy). On the other hand, the transition from the most noble
values of Eprot to an active potential has the same trend as CCT but it is so-called the
critical protection temperature (Tprot) for crevice. Tprot is the temperature below which
30 40 50 60 70 80 90-200
0
200
400
600
800
1000
E,m
V SCE
Temp.oC
ECrev Eprot
Fig. 4. Effect of temperature on Ecrev and Eprot for Type 254 SMO stainless steel in 4% NaCl.
E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444 2437
initiation of crevice never occur at any potential for a given metal. The curves of Fig.
4 indicate that the Tprot for Type 254 SMO steel occurs at a little lower temperature
level (52 �C) than CCT (55 �C) in 4% NaCl. This result is very important from
engineering point of view, where it does not possible for the already initiated crevice
corrosion on the steel to propagate at much lower temperature. On contrary, It was
reported [15] that the CCT was 50–60 �C for a cast quality of UNS S31254 steel in3% NaCl and it was possible to maintain active crevice corrosion at a temperature as
low as 10 �C. Laycock et al. [14] reported that if metastable pits initiate crevice
corrosion and the CCT is the lowest temperature at which crevice corrosion occurs,
the CCT should be corresponding to the lowest temperature at which metastable
pitting is possible. This assumes that the crevice corrosion propagation is possible if
metastable pitting is possible, which seems reasonable since crevice can propagate at
relatively low potential as will be discussed later.
3.3. Effect of chloride ions concentration on Ecrev and Eprot
The effect of the chloride ion concentrations on the Ecrev and Eprot after PCAP
treatment were examined at 70 �C. This temperature was selected because it was
sufficiently above the CCT for Type 254 SMO steel in 4% NaCl solution. The results
are represented in Fig. 5. Fig. 5 reveals that both Ecrev and Eprot were linearly de-creased with the logarithm of chloride concentration at 70 �C. The two crevice
potentials were expressed by the conventional form
Fig. 5
E ¼ A� B log½Cl��
where A and B are constants. It was found that B value are 227 and 72 mV/decade for
the variation of Ecrev and Eprot, respectively, with logarithm chloride ion concentra-
tion. The line of Eprot versus the logarithm of chloride concentration is displaced, in
0.1 1-200
0
200
400
600
800
E, m
V SCE
[Cl-] / mol dm-3
ECrev Eprot
. Effect of chloride ion concentrations on Ecrev and Eprot for Type 254 SMO stainless steel at 70 �C.
2438 E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444
the negative direction, from that for Ecrev by 690 mV at low concentration and this
value decreased to 475 mV at high concentration. This indicates that the initiated
crevice corrosion on the steel can continue to grow when the potential was reduced
less than those values. It has been reported that the B values for different steels are
dependent on the steel type and the aggressiveness of the environment [21,22].
However, Newman [23] reported that the slope B should be 60 mV for steel inchloride solution at 25 �C. He attributed the higher values of B founded for stainless
steels to the formation of chloro-complexes of chromium.
3.4. Effect of pH on Ecrev and Eprot
Fig. 6 shows the relation between the crevice potentials (Ecrev and Eprot) of Type
254 SMO steel and the pH of 4% NaCl solutions at 70 �C. The Ecrev value decreased
linearly with decreasing pH value with a slope of 37.5/pH unit, whereas the Eprot was
pH independent. This is probably because the low pH aiding localized acidification
[24] which facilitates the crevice initiation. It was observed that crevice corrosion
initiated on the creviced sample of Type 254 SMO steel in 4% NaCl at 90 �C atpotential more active than pitting potential of crevice free samples as shown in Fig.
7. It was also clear from the polarization curves that the passive current density in
case of crevice is higher than the passive current density in case of pitting. However,
the crevice corrosion potential was close to the metastable pitting potential which
was normally more active than the pitting potential for the same metal [14]. This
result was regarded as supporting evidence for the metastable pitting model of
crevice corrosion. Stockert and Boehni [25] proposed that metastable pits could be
stabilized by crevice walls, so that crevice corrosion was simply a geometricallystabilized form of pitting. The aggressiveness nature of the crevice attack decreased
2 4 6 8 100
100
200
300
400
500
600
700
E,m
V SCE
pH
ECrev Eprot
Fig. 6. The relation between Ecrev and Eprot for Type 254 SMO stainless steel and pH of 4% NaCl at 70 �C.
10-8 10-6 10-4 10-2 100
-400
-200
0
200
400
600
800
1000
1200
b
aE,
mV SC
E
Current Density, (A/cm2)
(a): pure Pitting(b): Crevice + pitting
Fig. 7. PCAP curves of Type 254 SMO stainless steel in 4% NaCl with potential scan rate 5 mV s�1 at
90 �C, (a) creviced free sample (b) creviced sample.
E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444 2439
with increasing the pH values this could be attributed to the role of OH� ions which
inhibit the localized corrosion [26].
3.5. Effect of bromide ions on crevice potentials and surface morphology
The relation between both of Ecrev and Eprot of Type 254 SMO steel and the
bromide ion to chloride ion ratio, with a fixed halide content of 4% at 70 �C is
represented in Fig. 8. The Ecrev did not change with the variation of bromide to
0.0 0.2 0.4 0.6 0.8 1.0-100
0
100
200
300
400
500
600
E, m
V SCE
[Br- ]/[Br- ]+[Cl- ]
ECrev Eprot
Fig. 8. Effect of of bromide ions to chloride ions ratio at a fixed halide ions concentration of 4% on Ecrev
and Eprot for Type 254 SMO stainless steel at 70 �C.
2440 E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444
chloride ratio whereas Eprot increased at high ratio of Br�. Although this relation was
similar to that found for Epit and Eprot of crevice free of Type 254 SMO steel in
similar bromide to chloride ratio at 90 �C [19], it was dissimilar to that reported for
904 L stainless steel [22]. This difference in the trend could be attributed to the
difference in composition of high molybdenum containing stainless steels. SEM
micrographs of crevice corrosion formed on Type 254 SMO steel in the presence ofvarious ratios of chloride and bromide with a fixed halide content of 4% at 70 �Cafter PCAP treatment are represented in Fig. 9. The presence of 25% Br� from the
Fig. 9. SEM micrographs of the creviced sample of Type 254 SMO surface after PCAP treatment in
different bromide ions to chloride ions ratio at a fixed halide ions concentration of 4% at 70 �C (a) 75%
NaCl+ 25% NaBr (b) 50% NaCl+ 50% NaBr (c) pit formed on crevice free part in the case of (b).
E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444 2441
total halide content led to a deep crack in the crevice corrosion area (Fig. 9a). This
crack grows in depth and width with increasing the bromide ratio to 50% beside the
appearance of lace like pit in crevice free part of the electrode as shown in Fig. 9b
and c, respectively.
3.6. Effect of the addition of sulphate and bicarbonate ions on crevice corrosion
To examine the possibility of crevice corrosion inhibition by other anions, dif-
ferent concentrations of SO2�4 and HCO�
3 were added to 4% NaCl at 70 �C. Figs. 10and 11 represent the PCAP curves of Type 254 SMO steel in 4% NaCl in the absence
and presence of various concentration of SO2�4 and HCO�
3 ions, respectively. In case
of sulphate additions, it was found that increasing sulphate ion concentration in-
creased the crevice corrosion potential of the steel and dimensioned the hysteresis
loop (Fig. 10). This result indicates that sulphate has an inhibition effect on crevice
corrosion. The mechanism by which sulphate ion was inhibiting crevice corrosion
was through a supporting electrolyte effect [26]. The increase in the crevice corrosion
potential should be due to the competitive migration of SO2�4 and Cl�, with accu-
mulation of the critical concentration of Cl� needed being delayed.
Increasing the addition of sodium bicarbonate to chloride solution led to a sig-
nificant positive shift in the Ecrev and reduction of the hysteresis loop of the steel as
shown in Fig. 11. On the addition of 0.5 M sodium bicarbonate to 4% NaCl the
hysteresis loop was eliminated. On the forward potential sweep of the steel in 4%
NaCl in presence of 0.3 M sodium bicarbonate, it was found the initiation of small
anodic current peak at 420 mV. The magnitude of this peak increased with
increasing the concentration of bicarbonate ions. This current peak might be
10-7 10-5 10-3 10-1-600
-300
0
300
600
900
1200
1500
d c b a
E, m
V SCE
Current Density, (A/cm2)
(a) 0.0M (b) 0.1M (c) 0.5M (d) 1.0M
Fig. 10. PCAP curves of creviced sample of Type 254 SMO in 4% NaCl with potential scan rate 5 mV s�1
in the presence of (a) 0 M Na2SO4 (b) 0.1 M Na2SO4 (c) 0.5 M Na2SO4 (d) 1 M Na2SO4 at 70 �C.
10-8 10-6 10-4 10-2 100
-300
0
300
600
900
1200
1500
10-8 10-6 10-4 10-2 100-600
-300
0
300
600
900
1200
10-8 10-6 10-4 10-2 100-600
-300
0
300
600
900
1200
10-8 10-6 10-4 10-2 100
-300
0
300
600
900
1200
10-8 10-6 10-4 10-2 100-600
-300
0
300
600
900
1200
(a)
E,m
V SCE
Current Density,(A/cm2)
(b)
E,m
V SCE
Current Density,(A/cm2)
(c)
E,m
V SCE
Current Density,(A/cm2)
(d)
E,m
V SCE
Current Density,(A/cm2)
(e)
E,m
V SCE
Current Density,(A/cm2)
Fig. 11. PCAP curves of creviced sample of Type 254 SMO in 4% NaCl with potential scan rate 5 mV s�1
in the presence of (a) 0 M NaHCO3 (b) 0.1 M NaHCO3 (c) 0.3 NaHCO3 (d) 0.5 M NaHCO3 (e) 1 M
NaHCO3 at 70 �C.
2442 E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444
E.A. Abd El Meguid, A.A. Abd El Latif / Corrosion Science 46 (2004) 2431–2444 2443
attributed to the formation of a very limited crevice corrosion which delayed when
the potential was swept to more positive potential.
4. Conclusions
The results of the present work allow the following conclusions to be drawn.
1. Crevice corrosion of Type 254 SMO stainless steel occurred in 4% NaCl solution
at CCT of 55 �C and there was no significant difference in temperature between
CCT and Tprot.
2. SEM micrographs indicated the association of pitting and crevice corrosion for
Type 254 SMO stainless steel in 4% NaCl solution at 90 �C.
3. The Ecrev of Type 254 SMO stainless steel decreased linearly with increasing thechloride ion concentration and crevice attack became more strong as shown by
SEM.
4. Lowering the pH value of 4% NaCl caused more aggressive crevice attack due to
increase in the local acidification inside the crevice.
5. The Ecrev of Type 254 SMO stainless steel did not change with the change of bro-
mide ions to chloride ions ratios at a fixed halide content of 4%.
6. Sulphate and bicarbonate were found to be strong inhibitors for crevice corrosion
and operate via a competitive migration mechanism.
Acknowledgements
E. A. Abd El Meguid wishes to thank Alexander von Humboldt foundation for
providing the equipments.
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