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Assessment of Inter-granular Corrosion Susceptibility of 304L Stainless Steel
Using Non-destructive Electrochemical Techniques
Article in ISIJ International · January 2014
DOI: 10.2355/isijinternational.54.1898
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ISIJ International, Vol. 54 (2014), No. 8, pp. 1898–1905
Assessment of Inter-granular Corrosion Susceptibility of 304L
Stainless Steel Using Non-destructive Electrochemical
Techniques
Ravindra Vasantrao TAIWADE,* Avinash Vijay INGLE and Rajesh Kisni KHATIRKAR
Department of Metallurgical and Materials Engineering, Visvesvaraya National Institute of Technology (VNIT), Nagpur, 440 010
India.
(Received on March 19, 2014; accepted on May 9, 2014)
The effect of heat treatment on the corrosion resistance of AISI 304L stainless steel is studied in the
present investigation. As-received samples of 304L stainless steel were solution annealed at 1 050°C for
90 minutes followed by thermal ageing at 750°C for various time durations (upto 24 days). ASTM standard
A-262 practice A test was used to detect susceptibility of inter-granular attack. Electron dispersive spec-
troscopy attached to scanning electron microscopy was performed for identification of carbides. It was
observed that no significant amount of attack took place upto 1 day. The extent of sensitization was quan-
titatively evaluated using double loop electrochemical potentiodynamic reactivation test. The results
obtained showed that corrosion resistance decreased with an increase in thermal ageing duration. This
behavior was attributed to the precipitation of chromium carbides causing depletion of chromium in the
areas adjacent to the grain boundaries (as determined by electron probe micro analyzer). The degree of
sensitization of highly aged sample was found to be 24.6%. Further, the degree of sensitization in terms
of polarization resistance was computed in the middle of the transpassive potential region (at 1.1 V) using
electrochemical impedance spectroscopy.
KEY WORDS: 304L stainless steel; inter-granular corrosion; SEM-EDS; double loop electrochemical poten-
tiodynamic reactivation; electrochemical impedance spectroscopy; electron probe micro analyzer.
The basic type 304 stainless steel is highly susceptible to
1. Introduction
sensitization induced inter-granular corrosion (IGC) which
Stainless steels are having 16–25% chromium and suffi- leads to the decrease in the corrosion resistance of steel. The
cient amount of austenite stabilizing elements like nickel, susceptibility to IGC is decreased in stainless steels by
manganese and nitrogen, so the steels austenitic at the room reducing their carbon content to less than 0.03 wt.%; the
temperature are called “austenitic stainless steels (ASSs)”. main type of this stainless steel class is AISI 304L, which
The most commonly used ASS is the AISI 304 grade also have been developed for minimizing the effect of complex
called as “18-8 steel” (containing 18% chromium and 8% carbide precipitation (M23C6), preferentially precipitate
nickel).1) Austenitic stainless steels have high ductility, low carbon and prevent depletion of chromium.5) A decrease in
yield stress and relatively high ultimate tensile strength. carbon content from 0.08–0.02 wt%, the nose of the time
They also offer excellent corrosion resistance in many temperature sensitization curve is shifted from 0.1 h to 100 h
organic, acidic, industrial and marine environments. Hence and chromium carbide formation can be greatly delayed by
they are widely used in steam generating plants as piping using this low carbon variant.6,7) However, it can still prove
and superheating tube materials due to their good mechani- to be detrimental and lead to sensitization. The precipitation
cal properties and corrosion resistance at elevated tempera- of carbides during welding is eliminated due to low concen-
tures.2,3) However, when ASSs have undergone a treatment tration of carbon (0.03 wt.%).8) Consequently, this 304L
like welding in the temperature range between 450°C to stainless steel can be used in the “as welded” state even in
850°C, there is a breaking corrosion resistance inter- severe corrosive conditions. In many cases it eliminates the
granularly as a result of segregation of carbides (M23C6, necessity of post-annealing of weldments, which is strictly
where M = Cr Fe Mo). This mechanism of precipitation of followed for the 304 type.1–3)
carbides consisting predominantly chromium carbide (Cr23C6) The sensitization behavior of ASS grades which leads to
at the grain boundaries, results in the formation of chromi- IGC attack has been extensively studied by many research-
um-depleted zones adjacent to it, called as sensitization.4) ers using various electrochemical tests. Usually the sensi-
tized region is evaluated using various qualitative methods
* Corresponding author: E-mail:
[email protected] mentioned in ASTM standard A 262 Practice A-F. Except
DOI: http://dx.doi.org/10.2355/isijinternational.54.1898 Practice A, all the other tests are destructive and require dif-
© 2014 ISIJ 1898
ISIJ International, Vol. 54 (2014), No. 8
ficult preparation. The Practice A is rapid qualitative and isothermal ageing treatment at temperature of 750°C for
most commonly used test in laboratory. However, from various time durations ranging from 3 h to 576 h (i.e.
industrial point of view, it is necessary to develop non- 24 days) followed by air cooling. Silicon carbide (SiC) muf-
destructive test methods (like double loop electrochemical fle furnace (Lenton, UK) was used for this purpose.15–17) The
potentiodynamic reactivation-DLEPR and electrochemical sample preparation for size 10 mm × 10 mm × 3 mm is
impedance spectroscopy-EIS) for the quantitative assess- described as follows.
ment of IGC in the localized region. Pedro de Lima-Neto et The samples were joined with a brass stud (8 mm Φ)
al.9) worked on the welded AISI 304 stainless steel using using silver paste for electrical connections. The stud was
DLEPR and EIS test to determine the length of the sensi- connected to brass wire (3 mm Φ) via M3 threads. The
tized zone (SZ). A. Arutunow et al.10) investigated the assembly was then mounted in cold setting resin, leaving
dynamic changes of impedance of AISI 304 stainless steel one of the surface of sample open for testing. The open sur-
dissolution process in conditions of IGC using dynamic EIS. face of samples were wet polished on emery papers (180,
R. V. Taiwade et al.11) worked on the qualitative and quan- 240, 400 and 600 grit), and then on velvet cloth smeared
titative comparison of degree of sensitization (DOS) of AISI with 0.75 μ alumina (Al2O3) slurry. The samples were ultra-
304 stainless steel and Cr–Mn ASS to conclude recovery sonically cleaned in distilled water prior to each test.
from sensitization which was observed only in AISI 304 A Potentiostat (Solartron-1285) was used for ASTM stan-
grade. R. V. Taiwade et al.12) worked on effect of solution dard A-262 practice A test. In practice A, the samples were
annealing on susceptibility towards IGC of ASS using elec- electrolytically etched in 10 wt.% oxalic acid solution with
trochemical tests. They concluded that the effect of cumu- current density of 1 A/cm2 for 90 seconds.18,19) For qualita-
lative sensitization and the area of sensitization zone get tive assessment of IGC, optical (Zeiss Axiolab) and scan-
reduced after solution annealed (SA) heat treatment. These ning electron microscopy (JEOL 6380 A) was carried out
extensive researches have led to the remedy for the compli- after etching. Electron dispersive spectroscopy (EDS)
cations placed by IGC on ASS grades specifically AISI 304 attached to SEM (JEOL 6380 A make) was also used for
SS. It comprises of eliminating or reducing the formation of identification of carbides.
chromium carbides that can be done by selecting an extra DLEPR test was performed in a solution consisting of 0.5 M
low modification of 304, that is 304L. V. Kain et al.13) H2SO4 + 0.001 M NH4SCN having a scan rate of 6 V/h at
worked on testing sensitization and predicting intergranular room temperature (27°C). It was carried out using a
corrosion and intergranular stress corrosion cracking sus- Potentiostat (Solartron-1285), in conventional three-electrode
ceptibility of ASSs (304/304L) using fast, nondestructive electrochemical cell, with platinum electrode as counter
and quantified electrochemical tests. S. Bhise et al.14) electrode, saturated calomel electrode (SCE) as the refer-
worked on potential measurement for predicting corrosion ence electrode and sample as the working electrode. Before
behavior of SS 304L in boiling nitric acid containing oxi- exposing the sample, the test solution was de-aerated using
dizing ions. They concluded that IGC of type 304L SS is dry (oxygen free) nitrogen gas for 1 h. All the DLEPR
dictated by the trans-passive potential in nitric acid medium. experiments were initiated after attaining nearly steady-state
However, the collective and systematic assessments of open circuit potential (about 45 min). The potential range
IGC in 304L SS using both qualitative and quantitative tech- chosen from –500 mV (SCE) to +300 mV (SCE) for for-
niques are limited. Therefore, in the present investigation ward scan. The scanning direction was then reversed, and
various electrochemical tests like ASTM A-262 A, DLEPR the potential was reduced back to –500 mV (SCE) to obtain
and EIS were conducted along with electron dispersive reverse scan. The peak activation current density (Ia) and
spectroscopy attached to scanning electron microscopy the peak reactivation current density (Ir) were measured
(SEM-EDS) and electron probe micro analyzer (EPMA) for during forward and reverse scans, respectively. The % DOS
IGC characterization. was then computed as the ratio of (Ir/Ia) x100.20,21)
EIS test was performed using EG & G PAR Versa STAT
3 in a solution consisting of 0.5 M H2SO4 + 0.2% NaCl and
2. Experimental
the remaining setup was same as that of DLEPR test. The
The AISI 304L SS was procured from market in the form potential step was 10 mV and the testing frequency range
of sheet. The chemical composition (as determined by opti- was 0.01 Hz to 1 MHz. The test was performed at potential
cal emission spectrometer) is given in Table 1. Samples for 1.1 V. During test the sample was potentiostatically cleaned
ASTM standard A-262 Practice A and electrochemical tests at –500 mV (SCE) for 2 min to remove air-formed oxide
were cut from the sheet by wire-cut electrical discharge film. The measured impedance was automatically recorded
machine to avoid heating zone during cutting operation. Sam- and saved in a personal computer to obtain the Nyquist
ples for practice A and other tests were 10 mm × 10 mm × plots. Charge transfer resistance (Rct) was evaluated from
3 mm. All the samples were solution annealed (SA) at a the Nyquist plots.22) Origin PRO 8.5 software was used for
temperature of 1 050°C for 1.5 h, followed by water quench- the analysis. In the present investigation the chromium con-
ing. The solution annealed samples were then subjected to centration across the grain boundary was measured using
electron probe micro-analyzer (EPMA). Approximately 25
data points were collected across the grain boundary.
Table 1. Chemical composition (weight%) of AISI 304L SS.
Elements Cr Ni C Mn Si S P 3. Results and Discussion
Weight% 19.610 8.301 0.018 1.362 0.381 0.001 0.011 It is previously mentioned in the introduction section that
1899 © 2014 ISIJ
ISIJ International, Vol. 54 (2014), No. 8
SS 304L gets sensitized in longer ageing duration due to for- es and hence they were classified as “dual” structure. In
mation of carbide precipitation. This section deals with the Figs. 2(g)–2(i), it can be seen that the carbides are precipi-
various electrochemical tests beginning with ASTM stan- tated along the grain boundaries. These microstructures can
dard A 262 practice-A followed by SEM, SEM-EDS, be classified under the category of ‘‘ditch’’ structure. Figure
DLEPR, EIS and EPMA for characterization of carbides and 2(i) shows the sample that was thermally aged for the max-
identification of IGC susceptibility. imum duration of time and it is evident from the microstruc-
ture that the ditching characteristic was highest in this case.
3.1. Qualitative Analysis Hence it signifies that the ditching phenomenon increases
3.1.1. ASTM Standard A-262 Practice A Test with increase in aging time. Therefore, as per ASTM stan-
This electrochemical test deals with the measurement of dard Practice A test, it can be concluded that the 304L SS
potential difference after applying a current (1 A/cm2) which samples when heat treated, indicate variations in their
results in preferential attack of high energy sites that is grain microstructure in terms of carbide precipitation and the sam-
boundaries. A typical curve obtained from galvanostatic ple which is aged for the highest duration will show a dense
mode of electrolytic etching is shown in Fig. 1 and indicates carbide attack along the grain boundaries (highly sensi-
the time potential relationship for the investigated sample tized).
which is heat treated at 750°C for 24 days. Figure 3(a) shows the well labeled SEM micrographs of
According to the microstructures obtained after ASTM thermally treated samples at 750°C for 2, 16 and 24 days,
standard Practice A test, the samples are classified as fol- where carbides are prominently observed at the grain
lows: boundaries in all the cases. Figure 3(b) indicates the carbide
1. Step structure: Absence of carbides (that is steps only point of interest in SEM micrograph. Also Fig. 3(c) shows
between grains, no carbides at grain boundaries). the EDS spectra of selected point. It is found that the car-
2. Dual structure: Discontinuous carbide precipitation bides at the grain boundaries consisted of ~75% Fe, ~19%
(that is some carbide at grain boundaries in addition to steps, Cr and 5% Ni (as determined by SEM-EDS). Therefore,
but no single grain completely surrounded by carbides). from the micrographs of Figs. 2(d)–2(i) and 3(a)–3(c) , the
3. Ditch structure: One or more grain is completely sur- IGC attack is qualified in the investigated steel.
rounded by carbides.16,17)
Figures 2(a)–2(i) shows the optical micrographs of the 3.2. Quantitative Analysis
solution annealed and heat treated samples of AISI 304L SS 3.2.1. Double Loop Electrochemical Potentiodynamic
after etching as per ASTM standard A-262 Practice A test. Reactivation (DLEPR) Test
In Fig. 2(a), single phase austenite structure observed and no This quantitative nondestructive electrochemical test
trace of secondary phases like carbides was found. Figures method is used to estimate the extent of IGC in terms of
2(b)–2(i) shows the optical micrographs of thermally aged DOS. The schematic diagram with log current on abscissa
samples of the 304L SS at 750°C for various durations of and potential on the ordinate indicating the various elements
time. In Figs. 2(b)–2(d) very less attack and no carbide pre- of DLEPR curve consisting of active, passive region along
cipitation is observed in the microstructures and hence it is with anodic and reverse scan as shown in Fig. 4. This test
called as the “Step” structure. In Figs. 2(e)–2(f), partial is based on the assumption that only sensitized grain bound-
attack or precipitations of carbides are observed at few plac- aries are active, whereas the un-sensitized grain matrix is
Fig. 1. Typical time-potential curve of electrolytic etching in galvanostatic mode for the sample heat treated at 750°C for
24 days.
© 2014 ISIJ 1900
ISIJ International, Vol. 54 (2014), No. 8
Fig. 2. Optical micrographs of 304L SS after solution annealing + heat treatment at 750°C acquired using practice-A test.
passive (due to formation of chromium oxide film). This implies greater is the DOS and more is the metal dissolution.
passive corrosion resistant film of Cr2O3 may weaken local- The quantitative effect of time and temperature on IGC of
ly due to the formation of heterogeneous microstructures at 304L SS is apparent from the DOS values and DLEPR
the grain and grain boundaries which results in potential dif- curves (Fig. 5). Table 2 shows the DOS data obtained from
ference. IGC is accelerated by the potential difference DLEPR tests. The Ir value of SA sample is very small which
between the grain (exhibit passive behavior) and the grain is also evident from the microstructure of SA sample (Fig.
boundaries (exhibit active/anodic behaviour). During this 2(a)) as it has no carbide since they were totally dissolved
phenomenon, the chromium depleted alloy sets up passive- after SA treatment. The reactivation current (Ir) values of
active cell. Further by decreasing the potential, the protective the samples heat treated at 6 h, 24 h (1 day) and 576 h
passive film over chromium-depleted areas is more easily (24 days) was 0.001107, 0.002018 and 0.018513 A/cm2 and
dissolved than that over un-depleted (i.e. non-sensitized) their DOS values were 1.47, 2.76 and 24.46 respectively.
surfaces. The value of Ir increases by one order of magnitude in case
In the current investigation, the sensitivity of aged 304L of highly sensitized condition (576 h) which is attributed to
SS samples at 750°C towards IGC was evaluated using the increase of chromium depleted zones. This indicates that
DLEPR test, which consists of a potentiokinetic scanning in during reactivation, the metal dissolution is increasing with
a suitable electrolyte, from an active to a passive domain the ageing time. In other words, it can be said that the pro-
(activation or anodic scan), followed by a return to the initial tective passive film which forms over chromium depleted
potential (reverse or reactivation scan). The ratio of reacti- areas is getting easily dissolved with the increment of age-
vation and anodic current densities “(Ir/Ia)” permit the eval- ing time duration. These quantified results are in good
uation of the DOS. The development of the reactivation agreement with results of microstructural studies carried out
peak current density can be attributed to metal dissolution in this investigation.
during reverse scan. Higher value of the reactivation current
1901 © 2014 ISIJ
ISIJ International, Vol. 54 (2014), No. 8
Fig. 3. SEM micrographs and SEM-EDS images of thermally aged (750°C) 304L SS samples. a) SEM micrographs of
aged samples (at 2, 16 and 24 days), b) Carbide point of interest for EDS scan, c) EDS spectra of selected point.
3.2.2. Electrochemical Impedance Spectroscopy (EIS)
The various electrochemical tests like anodic polariza-
tion, potentiostatic pulse techniques etc. has been extensive-
ly used by many researcher to identify anodic dissolution
behavior in austenitic stainless steels. Basically the anodic
polarization test emphasized on active-passive and transpas-
sive behavior of the materials.
In the transpassive potential region of the anodic polar-
ization curve, three types of anodic dissolution viz. passive
dissolution, grain boundary attack and pitting can be char-
acterized. Also it is well known from literature that the DOS
can be correctly evaluated in the middle of transpassive
potential region where anodic dissolution is of grain bound-
ary attack type.12,22)
Fig. 4. Schematic diagram of the active-passive DLEPR curve. In the present investigation a quick and rapid electro-
© 2014 ISIJ 1902
ISIJ International, Vol. 54 (2014), No. 8
Fig. 5. Obtained DLEPR curves of 304L SS, solution annealed and thermally aged samples at 750°C.
1903 © 2014 ISIJ
ISIJ International, Vol. 54 (2014), No. 8
Table 2. DOS values for solution annealed and thermally aged
samples.
Time Reactivation current, Activation current, %DOS
Condition
(h) Ir (A/cm2) Ia (A/cm2) (Ir/ Ia)*100
Solution
– 0.000715 0.076033 0.94
annealed
3 0.000979 0.072051 1.30
6 0.001107 0.075008 1.47
12 0.001738 0.072231 2.40
Solution
Annealed + 24 0.002018 0.072890 2.76
Thermally
aged at 48 0.006700 0.071966 9.35
750°C
192 0.008383 0.070463 11.89
384 0.008839 0.072616 12.17
576 0.018513 0.075671 24.46
Fig. 6. Anodic polarization curve for the sample heat treated at
750°C for 24 days.
chemical impedance spectroscopy (EIS) test was incorporat-
ed in the middle of the transpassive potential region for
DOS measurement. Figure 6 shows the transpassive poten-
tial region in anodic polarization curve obtained in the solu-
tion (0.5 M H2SO4 + 0.2 % NaCl) for sample heat treated at
750°C for 576 h (24 days).
In this work, the electrochemical impedance spectroscopy
(EIS) test was carried out to find the corrosion resistance of
few thermally aged samples. This test was performed in the
frequency domain of 10 kHz to 10 Hz. The remaining points
from high and low frequency were eliminated to process the
data in order to obtain the significant corrosion resistance
values. Figure 7 shows the Nyquist plots of the heat treated
samples polarized at 1.1 V and indicates the AC impedance
response in this trans-passive potential. The charge transfer
resistance (Rct) values of 6 h (less sensitized) sample was
found to be 327 Ω and for 24 days (highly sensitized) it was
171 Ω. Increase in the ageing time leads to a shift of the
curves to higher ohmic resistance values due to acceleration
in the dissolution kinetics, which explains decrease in cor-
Fig. 7. Nyquist plots for thermally aged (750°C) samples.
rosion resistance with increased ageing time. Such varia-
tions may suggest differences in the thickness of corrosion
resistant film that would delay the charge transfer and hence
helping in improving the corrosion resistance until achiev-
ing a robust and stable passive film. The current results of
EIS test are in agreement with the findings of Huang et al.22)
The Rct values of less and highly sensitized samples indi-
cate good correlation with DOS that is, higher the sensitiza-
tion, lower will be the Rct values. This correlation is evident
from the microstructures (Figs. 2(c) and 2(i)) and DLEPR
curves (Figs. 5(c) and 5(i)). Thus, with the help of values
obtained from Nyquist plots the corrosion resistance behav-
ior of the investigated 304L SS was verified.
3.2.3. Electron Probe Micro-analyzer (EPMA) Line Scans
EPMA was used to predict the wt.% of chromium con-
centration across the grain boundary. Figure 8 shows the
chromium concentration profile (wt.%) along the grain
boundaries for SA, and thermally aged samples (at 750°C
for 6 h, 1 day and 24 days). The Cr concentration along the
grain boundary in SA sample is almost constant around
19.5 wt.% for all the data points and no depleted region was Fig. 8. Chromium concentration profile of obtained EPMA line
identified. The Cr concentration was observed to be declin- scans.
© 2014 ISIJ 1904
ISIJ International, Vol. 54 (2014), No. 8
ing with the ageing time. For the less sensitized (6 h) Department of Metallurgical and Materials Engineering) for
sample, chromium concentration amounted to be around performing solution annealing treatment. The authors would
17.8 wt.%, and for partially sensitized (1 day) sample it was also like to thanks Mrs. Varsha Patankar (Technical staff,
15.8 wt.%, while for the highly sensitized (24 days) sample Testing of Materials Laboratory, Department of Metallurgi-
it was 10.2 wt.%. Since, the minimum chromium concentra- cal and Materials Engineering) for her help in conducting
tion values indicate that the passive film is weakened with heat treatments. The authors would also like to thanks Miss
increase in ageing time. Kritika Singh, Mr. Vincent and Mr. Vinayak Dakre
(Research Scholar, MME VNIT) for their help in conduct-
ing SEM and SEM-EDS analysis. Lastly, authors would like
4. Conclusion
to thank Mr. Jagdish Singh Saini (Scientific Officer Grade-
(1) Collective and systematic investigation of IGC II, Indian Institute of Technology, Roorkee, India) for con-
behaviour of 304L SS was carried out using various electro- ducting EPMA scans.
chemical techniques including practice A, DLEPR, EIS, and
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