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H2S Corrosion 304 Vs 316
H2S Corrosion 304 Vs 316
Corrosion Science
journal homepage: www.elsevier.com/locate/corsci
A comparative H2S corrosion study of 304L and 316L stainless steels in acidic media
A. Davoodi a,⇑, M. Pakshir b, M. Babaiee b, G.R. Ebrahimi a
a
Department of Materials Science and Engineering, Faculty of Engineering, Sabzevar Tarbiat Moallem University, Iran
b
Department of Materials Science and Engineering, School of Engineering, Shiraz University, Iran
a r t i c l e i n f o a b s t r a c t
Article history: H2S corrosion of 304L and 316L in oxygen-free Na2SO4 + Na2S solution at pH 3 and temperature of 60 °C
Received 24 April 2010 were investigated by EIS, potentiodynamic polarisation, multi-component Pourbaix diagrams and micro-
Accepted 18 September 2010 structure characterization. At similar conditions, lower corrosion rate was observed on 316L, attributed to
Available online 1 October 2010
its denser (1.5 times) and smoother (6%) surface layer and confirmed by SEM micrograph. During polar-
isation, H2S increases significantly the critical current density on 304L and passivation current density, ip,
Keywords: on 316L. Higher ip on 316L was associated to simultaneous FeS2–MoS2 preservation, confirmed by XRD
A. Stainless steel
examination. H2S could have an inhibiting effect on 304L in passivity region.
B. EIS
C. Acid corrosion
Ó 2010 Elsevier Ltd. All rights reserved.
C. Passive films
C. Passivity
C. Pourbaix diagram
⇑ Corresponding author. Tel.: +98 5714003536; fax: +98 5714411160. Analytical grade Na2SO4, Na2S, and H2SO4 reagents were used.
E-mail address: adavoodi@kth.se (A. Davoodi). To prepare the solution, 1 M Na2SO4 solution was buffered by
0010-938X/$ - see front matter Ó 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.corsci.2010.09.050
400 A. Davoodi et al. / Corrosion Science 53 (2011) 399–408
H2SO4 to a pH of 3. To exclusively investigate the H2S corrosion However, as can be seen in the reference, [24], theses compounds
mechanism, it is common to purge an inert gas into the solution are most likely stable at neutral and alkaline conditions. Therefore,
to remove dissolved oxygen [14–17]. Otherwise, several involved most likely they have no contribution in the present study.
cathodic reactions could interfere (oxygen and HS reduction). Finally, scanning electron microscopy (SEM, Leica Cambridge,
Prior to each experiment, the prepared solution was purged by in- S360) and XRD (Bruker model D8 ADVANCE) were used to charac-
ert gas (Argon) for 15 min. Then a required amount of Na2S, pro- terize the samples surface morphology and compositions after
ducing 5 and 15 ppm H2S, was added to the solution (All exposure to the H2S corrosive media.
concentrations are reported in ppm by mole). According to the fol-
lowing reaction, Na2S is dissociated to H2S in acidic solution [2– 3. Results and discussion
5,11,12,21–22]:
3.1. OCP results
Na2 S þ 2Hþ ! 2Naþ þ H2 S ð1Þ
As a result, a trace amount of H2S is locally generated at the The results of OCP variations are shown in Fig. 1. In all H2S con-
vicinity of alloy surface. It should be emphasized that the argon centrations, the OCP values associated to 316L alloy are more posi-
purging and deoxygenating were continuously applied during all tive than 304L, but their difference diminishes by increase in H2S
measurements. A sealed electrochemical flat-cell (with 500 cm3 concentration. As seen in Fig. 1, increase in H2S concentration de-
in volume) was used and prior to adding Na2S, the inert gas was creases OCP of both alloys. For instance, in 316L alloy, its decrease
purged into the solution (with 4.5 bar pressure). After adding is almost three times higher than 304L at 5 ppm H2S concentration.
Na2S (and producing H2S), argon was purged above (not into) the Decrease in OCP is an indication of alloy nobleness deterioration
solution at a safe distance from the solution surface with lowest and surface activity acceleration.
possible pressure just to avoid oxygen entrance. This could help
to avoid any decreasing in H2S concentration during measuring 3.2. LPR results
time. Mounted cylindrical 304L and 316L austenitic stainless steel
specimens with 1 cm in diameter were used as working electrode. Fig. 2 represents the influence of H2S concentration on LPR
The chemical compositions of alloys in wt.% are given in Table 1. (polarisation resistance, RP) values. In all H2S concentrations, the
Prior to each experiment, the specimens were ground up 1200 RP value of 316L is higher than for 304L. However, by an increase
SiC abrasive paper and then polished with 3 and 1 lm alumina in the H2S concentration, the decrease in RP value of 316L is quicker
slurry to obtain mirror-like exposure surface. than for 304L. This means that the results of the LPR and OCP mea-
The corrosion experiments were performed in the following surements follow a similar trend. The corrosiveness of the solution
sequence: increases by an increase in H2S concentration to 5 ppm. For 316L
alloy, the RP decrease is six times higher than that one for 304L.
(a) 900 s OCP recording. Accordingly, the corrosion rate of both alloys increases. Although
(b) LPR test with potential domain of ± 10 mV and sweep rate of the 316L alloy has a higher corrosion resistance compared with
0.5 mV/s. the 304L alloy, the difference reduces by increase in H2S concentra-
(c) Potentiostatic EIS test at OCP with amplitude of 10 mV and tion. This indicates that the influence of H2S is more profound on
normally a frequency range of 102 to 105 Hz. the 316L alloy.
(d) PD test with a sweep rate of 1 mV/s and potential range from The influence of H2S on cathodic reactions including proton
200 to 2000 mV with respect to OCP. reduction is as follows [14–17]:
H2 S ! Hþ þ HS ð2Þ
All measurements were performed three times to assure repro-
ducibility. All corrosion tests were carried out by an Ivium Poten- HS ! Hþ þ S2 ð3Þ
tiostat instrument, using saturated calomel and Pt wire as
reference and counter electrodes, respectively. Ivium and EIS Spec-
2Hþ þ 2e ! H2 or 2H ð4Þ
trum Analyzer were used to extract the EIS equivalent circuit com-
ponents. Simulated data was fitted by less than 1% error in
calculation.
All measurements were performed in a water bath with a con-
trolled temperature of 60 ± 1 °C. This temperature represents ac-
tual conditions for gas purification units. To identify the
influence of alloying elements, the experimental results were final-
ly compared with multi-component Pourbaix diagrams of Fe-Ni-Cr
(304L) and Fe-Ni-Cr-Mo (316L) aqueous systems and in the pres-
ence of H2S species. All Pourbaix diagrams were plotted at 60 °C
by using Medusa software [23]. An equilibrium concentration of
106 M has been used for dissolved Fe, Ni, Cr and Mo ions (i.e.
[Fe2+(aq)] = [Cr3+(aq)] = [Ni2+(aq)] = [Mo4+(aq)] = 106 M). It should
be noticed that in Me-S-H2O systems (where Me = Fe, Ni, Cr, and
Mo), some other species may be also existed which may not be ta-
ken into account such as FeCr2O4, NiFe2O4, NiCr2O4, etc. [24].
Table 1
Chemical composition (in wt.%) of used 304L and 316L alloys.
C S P Mo Mn Si Cr Ni Fe
304L 0.02 0.02 0.03 0.30 1.62 0.46 18.13 8.71 Bal.
316L 0.02 0.02 0.02 2.32 1.71 0.49 18.16 8.25 Bal. Fig. 1. OCP variations of 304L and 316L alloys vs. H2S concentration (ppm by mole)
in Na2SO4 + Na2S (pH 3).
A. Davoodi et al. / Corrosion Science 53 (2011) 399–408 401
Fig. 2. LPR (Rp) variations of 304L and 316L alloys vs. H2S concentration (ppm by
mole) in Na2SO4 + Na2S (pH 3).
ðFeSHþ Þads þ H3 Oþ ! Fe2þ þ H2 S þ H2 O ð7Þ Fig. 3. (a) Nyquist and (b) Bode plots of 304L in Na2SO4 + Na2S, pH 3, at various H2S
concentrations (ppm by mole), T = 60 °C. Inserted graph in Nyquist plot is the used
Consequently, the dissolution of iron is accelerated. In fact, it equivalent circuit.
has been reported that on pure iron, H2S plays an accelerative role
on both the anodic iron dissolution and the cathodic hydrogen evo-
lution [14,17]. The difference in corrosion behaviour of 304L and the angular frequency. Applying CPE instead of pure capacitance
316L can be related to the chemical reactions involved by other improves EIS data fitness of the experimental results [25,26]. EIS
alloying elements such as Cr, Ni, and Mo which is discussed in data simulation on wide frequency spectrum, 105 to 103 Hz (not
the following sections. shown here) also indicates that a charge transfer resistance condi-
tion occurs in the surface reactions. Although, presence of H2S does
3.3. EIS results not induce any other time constants, however, a decrease in the
capacitance loop diameter and charge transfer resistance can be
Figs. 3 and 4 show the Nyquist and Bode plots of 304L and 316L observed by an increase in the H2S concentration. Therefore, the
specimens at 60 °C and different H2S concentrations. Various EIS results can be used to identify the corrosion mechanism by
equivalent circuits have been proposed for H2S corrosion the presence of H2S species.
[7,10,14–17,20]. Certainly, complex reactions could occur on the Extracted fitted data from the equivalent circuits are shown in
surface (particularly since the Cr, Ni are active and FeS2 and Table 2. The RP values obtained by EIS are very similar to the RP val-
MoS2 are formed in this pH), but their reaction steps could not ues obtained by LPR measurements (with less than 5% difference),
be distinguished by the EIS. The total impedance is quite low and Fig. 2. Comparing Nyquist curves of the two alloys depicts that in
most likely the time constants of involved reactions have overlap all H2S concentrations, the semicircle diameter associated with
and cannot be separated. For this reason, the possible and sepa- 316L is larger than for 304L. In solution without H2S, RP of 316L
rated reaction steps of the alloying elements were borrowed from is about three times larger than for 304L. However, by an increase
the previous studies where H2S corrosion of the pure Cr, Ni, and Fe in the H2S concentration, RP of both alloys reduce more or less with
elements were investigated individually [14–17]. In all conditions, the same trend. It seems that although the 316L alloy has a greater
the Nyquist curves indicate a single capacitance loop having a time corrosion resistance at solution without H2S, its superior perfor-
constant in Bode plots. Therefore, the alloy-electrolyte interface mance is diminished by an increase in H2S concentration.
can be simulated by an Randles equivalent circuit as shown in The n and C parameters extracted from CPE are shown in Fig. 5.
the inserted graph in Fig. 3, where Rs is the solution resistance, Although in solution without H2S, the n value in 316L is smaller
RP is the polarisation resistance at the alloy–electrolyte interface than for 304L, however, as shown in Fig. 5, in solution with H2S,
(also known as charge transfer resistance) and CPE is the constant the n values in 316L are greater than for 304L. For the 304L alloy,
phase element. The CPE value can be expressed in the form of an increase in the H2S concentration to 5 ppm results in rapid de-
P(ix)n in which P is proportional to the capacitance, n is a param- crease of n value from 0.89 to 0.78. A slight decrease down to 0.77
eter related to surface roughness and cell configuration, and x is could be observed by further increase in H2S concentration. For the
402 A. Davoodi et al. / Corrosion Science 53 (2011) 399–408
Fig. 4. (a) Nyquist and (b) Bode plots of 316L in Na2SO4 + Na2S, pH 3, at various H2S
concentrations (ppm by mole), T = 60 °C.
316L alloy, the n value decreases slightly from 0.83 to 0.81 by the Fig. 5. Calculated (a) n and (b) C variations with H2S concentration (ppm by mole)
presence of 5 ppm H2S, but remains almost constant by further in- at 60 °C.
crease in H2S concentration. A decrease in the n value is an indica-
tion of surface roughening which is due to an increase in the alloy
surface dissolution [22,25,26]. Therefore, a more rapid decrease in 316L alloy, the Cct value increases steadily by an increase in H2S
the n value for the 304L alloy indicates that the H2S influence on concentration from 27.2 to 56.0 lF cm2. It is well known that
the 304L surface roughness is greater than on the 316L alloy. In the capacitance is inversely proportional to the surface film thick-
other words, in 316L, H2S does not affect the surface roughness; ness according to [22,25,26]:
consequently the n value does not change significantly. This means
that in solution without H2S, the surface roughness of 316L is 7% eo e
Cct ¼ S ð9Þ
higher than 304L. In contrast, by producing H2S, the surface rough- d
ness on 304L is 6% higher than 316L.
Surface capacitance values were calculated and plotted in where d is thickness of the surface film, S is surface area of the elec-
Fig. 5(b), according to the following equation [25,26]: trode, eo is the permittivity of air and e is the local dielectric con-
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi stant. Therefore, an increase in Cct is an indication of surface layer
Cct ¼ n PðRP Þ1n ð8Þ dissolution and thinning process. The 316L alloy has a greater Cct
in compare with 304L which indicates that it has a thinner surface
In 304L alloy, in presence of 5 ppm H2S, Cct decreases rapidly layer. But since it has greater n, its surface layer is more uniform
from 118 to 23.6 lF cm2 and by further increase in H2S concentra- and condensed. Comparing C values indicates that in H2S-free solu-
tion it increases slightly to 37.4 lF cm2. On the other hand, in tion, the surface layer thickness of 316L is 4–5 times thicker than
Table 2
Extracted fitted data from EIS test.
chosen as bare and the initial air formed oxide layer, FeO–Cr2O3,
was not shown. In fact, air formed oxide is almost dissolved in
the present solution and is replaced by the sulfide layer (see Sec-
tion 3.5). The scheme shows that a thicker and more porous surface
layer on 304L is formed. More details of identified layer constitu-
ents, FeS2 and MoS2, will be discussed in Section 3.5.
Fig. 7. Schematic images of relative surface layer thickness and porosity (roughness) on (a) 304L and (b) 316L samples exposed to 0, 5 and 15 ppm (by mole) H2S containing
media. The white and black spots represent the porosities and MoS2 constituents, respectively. To simplify, sample in 0 ppm H2S was chosen as base and the initial air formed
oxide layer, (FeO–Cr2O3) was not shown.
During sample rinsing and drying for SEM imaging and XRD sults at a overpotential of about 1000 mV vs. SCE; See Figs. 8 and
characterization, pyrite may be decomposed to the pyrrohtite as 9(a). The Pourbaix diagram does not show any stability region
follows [27,28]: for FeS at the present investigated conditions which has been re-
ported previously on carbon steel [6,13].
3FeS2 þ 2H2 O $ 3FeS þ 3H2 S þ SO2 ð12Þ Moreover, Cr and Ni do not exhibit a passive layer at pH 3, based
However, studies of pyrite reactions are even more contradic- on Pourbaix diagrams. Following reactions could be proposed for
tory, the products being listed variously as FeSO4, Fe2(SO4)3, FeO, dissolution process [15,16]:
Fe2O3, FeS, H2SO4 or S either as single products or as complex mix- Ni þ H2 S þ H2 O $ ðNiHSÞads þ H3 Oþ þ e ð13Þ
ture [27–29]. XRD characterization was also performed on rinsed
and dried specimens. Figure 13 reveals XRD results on 304L and ðNiHSÞads $ NiHS þ e
þ
ð14Þ
316L samples exposed to 15 ppm H2S containing media. Presence
of FeS2 on both alloys and MoS2 on 316L is clear. Moreover, FeS þ 2þ
NiHS þ H3 Oþ $ Ni þ H2 S þ H2 O ð15Þ
and MoO2 components also exist. This is enough to conclude that
the sulfur-bearing Fe compounds and MoS2 surface layer are and
formed. Since XRD is an ex-situ technique and it is performed on
Cr þ H2 S þ H2 O $ ðCrSH Þads þ H3 Oþ ð16Þ
sample after washing and drying, its results do not exactly resem-
ble the actual corrosion products during aqueous corrosion occur-
Cr þ H2 S þ H2 O ! ðCrSHÞads þ H3 Oþ þ e ð17Þ
rence [27,28]. Recently, X-ray photoelectron spectroscopy (XPS)
studies of surface layer on H2S attack on 316L also revealed that
ðCrSH Þads $ ðCrSHÞads þ e ð18Þ
relatively high concentration of sulfur could be found inside the
formed oxide, which indicates that sulfur entered the oxide film
ðCrSHÞads ! CrSHþ þ e ð19Þ
through local weakening of the oxide [19]. In fact, using an
in situ technique would be further supportive to identify S com-
pounds in the surface layer during corrosion phenomenon. CrSHþ þ Hþ $ Cr2þ þ H2 S ð20Þ
At higher potentials, FeS2 is replaced by iron oxide, Fe2O3 (and According to the Pourbaix diagrams of Fe, Ni, Cr, and Mo (alloy
consequently iron hydroxiode), as seen in Fig. 10. This means that constituents of the 316L alloy), Figs. 10–12, the passivation in low
by detaching the sulfur species from the surface at high enough anodic overpotential could be mainly associated to formation of
potentials, hydroxyl ions could take an opportunity to reach the FeS2, Eq. (10) and also MoS2, as below [19–20,23]:
surface and iron oxide could be formed [18,23–24]. This can be
confirmed by an extra peak in the passivation region of 304L PD re- Mo þ 2H2 S ! MoS2 þ 2H2 ð21Þ
A. Davoodi et al. / Corrosion Science 53 (2011) 399–408 405
Fig. 9. (a) Critical passivation current density, icr and (b) passivation current
This can be confirmed by a decrease in current density after icr. density, ip (at potential 500 mV vs. SCE) of 304L and 316L alloys in Na2SO4 + Na2S,
At higher potentials, replacement of MoS2 by MoO2 could be pre- pH 3, at various H2S concentrations (ppm by mole), T = 60 °C.
Fig. 10. Pourbaix diagrams of (a) Fe-H2O and (b) Fe–H2O–S systems at 15 ppm (by Fig. 11. Pourbaix diagrams of (a) Cr–H2O–S and (b) Ni–H2O–S systems at 15 ppm
mole) H2S concentration, T = 60 °C, [Fe2+(aq)] = 106 M, calculated from the (by mole) H2S concentration, T = 60 °C, [Cr3+(aq)] = [Ni2+(aq)] = 106 M, calculated
thermodynamic data of reference [23]. from the thermodynamic data of reference [23].
Acknowledgements
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