Corrosion Science 50 (2008) 2390–2397

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Corrosion Science
j o u r n a l h o m e p a g e : w w w . e l s e v i e r. c o m / l o c a t e / c o r s c i

Intergranular corrosion of welded joints of austenitic stainless steels

studied by using an electrochemical minicell
C. Garcia, M.P. de Tiedra, Y. Blanco, O. Martin, F. Martin *
De­parta­men­to CMeIM/EGI/ICGF/IM/IPF, EUP, Uni­vers­i­dad de Val­la­do­lid, c/Fran­cisco Men­di­za­bal s/n, 47014 Val­la­do­lid, Spain

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

Article history: An inter­gran­ul­ ar cor­ro­sion study of welded joints of au­sten­it­ic stain­less steels (AISI 304 and 316L) has
Received 17 April 2008 been addressed. A spe­cific small-scale elec­tro­chem­i­cal cell (mini­cell) has been used. Four dif­fer­ent weld­
Accepted 12 June 2008 ment zones have been stud­ied. The elec­tro­chem­i­cal meth­ods applied were the elec­tro­chem­ic­ al po­ten­ti­
Available online 20 June 2008
oki­net­ic reac­ti­va­tion test and elec­tro­chem­i­cal po­ten­ti­oki­net­ic reac­ti­va­tion dou­ble loop test. These tech­
niques showed that the HAZ was the most crit­i­cal zone to inter­gran­u­lar cor­ro­sion for both mate­ri­als. The
Key­words: weld metal was sus­cep­ti­ble to in­ter­den­drit­ic cor­ro­sion and the fusion line showed a mix­ture of inter­gran­
A. Stain­less steel
u­lar and in­ter­den­drit­ic cor­ro­sion. The effect of pre- and post-weld­ing heat treat­ments for AISI 316L was
B. Polar­iz
­ a­tion
C. Inter­gran­u­lar cor­ro­sion
ana­lyzed. The HAZ was again the most crit­i­cal zone in every heat treat­ment con­di­tion. The results were
C. Weld­ing cor­re­lated to the micro­struc­tural fea­tures of the mate­ri­als.
© 2008 Elsevier Ltd. All rights reserved.

1. Intro­duc­tion because they could induce seg­re­ga­tion of alloy­ing ele­ments and

for­ma­tion of chro­mium-depleted zones [10–12].
Cor­ro­sion of stain­less steel (SS) weld­ments has been the goal All cor­ro­sion pro­cesses have been mainly stud­ied by large-scale
of a wide num­ber of works. Perhaps the most com­mon prob­lem exper­i­ments (work­ing elec­trode in the mm2–cm2 range) [13,14].
encoun­tered in SS weld­ments have been asso­ci­ated with sen­si­ti­sat­ How­ever, such pro­cesses are due to mech­a­nisms on a smaller
ion in the heat affected zone (HAZ) lead­ing to inter­gran­u­lar cor­ro­ scale. There­fore, it is advis­able to develop appro­pri­ate small-scale
sion (IGC). This is a well-known phe­nom­e­non that is found to be exper­i­men­tal devices that must nec­es­sar­ily undergo a thor­ough
due to pre­cip­i­ta­tion of car­bides and other inter­me­tal­lic phases at reduc­tion of the exposed sur­face area of the work­ing elec­trode.
grain bound­aries dur­ing heat­ing in the sen­si­ti­sat­ion tem­per­a­ture Regard­less of the numer­ous stud­ies of local­ised cor­ro­sion pro­
range, typ­i­cally 400–900 °C [1–3]. cesses on pas­sive metal weld­ments [15–18], there are some unre­
Not only phe­nom­ena asso­ci­ated to the HAZ are sig­nif­i­cant, the solved aspects related to the local acti­va­tion pro­cess. One of the
cast struc­ture of the weld metal zone poses addi­tional prob­lems rea­sons for this is due to the fact that, as said above, stan­dard
related to cor­ro­sion behav­iour. The micro-seg­re­ga­tion of chro­ elec­tro­chem­i­cal tech­niques are based on large-scale exper­i­ments
mium–molyb­de­num and the high fer­rite con­tent of the fusion line [19–24].
and its unmixed sub-zone where the metal melted but not mixed In the case of au­sten­it­ic SS weld­ments, the cor­ro­sion behav­iour
with filler metal also mod­ify cor­ro­sion behav­iour [4,5]. Fusion has been eval­u­ated with stan­dard prac­tices such as ASTM A262,
weld­ing pro­cesses can cause local changes in com­po­si­tion of the G48 and so forth [4,5]. Large-scale elec­tro­chem­i­cal tests such as
welded mate­rial which can alter the sta­bil­ity of the pas­sive layer ASTM G5 or G108 have been very suc­cess­fully applied to the study
and its cor­ro­sion behav­iour [6]. In addi­tion, from the micro­struc­ of elec­tro­chem­i­cal behav­iour of base mate­ri­als but not for weld­
tural point of view, the for­ma­tion of d-fer­rite is other param­e­ter to ments [10,25,26]. An alter­na­tive pro­ce­dure has been the use of a
take into account since can be prej­u­di­cial because of its sus­cep­ti­bil­ lacquer coat­ing to select a reduced uncov­ered area of the dif­fer­ent
ity to attack­ing in a cor­ro­sive envi­ron­ment [6,7]. welded zones [27]. In pre­vi­ous works of the research team [28,29]
In­ter­den­drit­ic cor­ro­sion, pit­ting cor­ro­sion, gal­vanic cor­ro­sion this tech­nique com­bined with small-scale elec­tro­chem­i­cal tests
besides the IGC are some of the cor­ro­sion modes that can be were inves­ti­gated. It was con­cluded that, results from lacquer coat­
found on SS weld­ments. [4–6,8,9]. The heat-input and cool­ing rate ing tech­nique, did not give good enough results due to low capa­
are two impor­tant param­e­ters affect­ing the cor­ro­sion resis­tance bil­ity to dis­crim­i­nate among weld­ing zones and some prob­lems
related to cre­vice cor­ro­sion.
The elec­tro­chem­i­cal po­ten­ti­oki­net­ic reac­ti­va­tion tests (sin­gle
* Cor­re­spond­ing author. Tel.: +34 983 42 35 15; fax: +34 983 18 45 14. and dou­ble loop) have been fre­quently applied to eval­u­ate the
E-mail address: [email protected] (F. Martin). degree of sen­si­ti­sat­ion of SS with advan­ta­ges such as quick, non

0010-938X/$ - see front matter © 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.corsci.2008.06.016
 C. Gar­cia et al. / Corrosion Science 50 (2008) 2390–2397 2391

destruc­tive and valid for in situ mea­sure­ments. They have been

used either indi­vid­u­ally or in com­par­at­ ive terms [30], some­times
have been used to eval­u­ate cor­ro­sion prop­er­ties of the HAZ of 304
SS welded by fric­tion stir as com­par­ing to GTAW (Gas Tung­sten Arc
Weld­ing) [24] or the effect of heat treat­ment on the sen­si­ti­sat­ion
of alloy 182 weld depos­ited on 304 SS sub­strate [22] or recently to
deter­mine the exten­sion of sen­si­tized zone in welded 304 SS [23].
Mi­cro­elect­ro­chem­i­cal meth­ods are pow­er­ful tech­niques to
study local­ized cor­ro­sion pro­cesses on small areas of pas­sive met­
als [27,31–37]. Most of these works used cap­il­lary-based drop­let
cells. The main ben­e­fit of using mi­cro­cells based on mi­cro­cap­il­lary
is directly related to the small size of the exposed work­ing area
[38], which is in the microm­e­ter range. Although some draw­backs
for cap­il­lary mi­cro­cells must be con­sid­ered, as has been explained
by Bir­bi­lis et al. [39].To find a solu­tion to these short­com­ings and
taken into account that for welded joint stud­ies it is not nec­es­sary
to use as small areas as those pro­vided by mi­cro­cap­il­lar­ies, it has
been designed a spe­cific small-scale elec­tro­chem­i­cal cell. It is
appro­pri­ated in size, dif­fer­ent to the cap­il­lary-based mi­cro­cell and
suit­able for cor­ro­sion stud­ies [28,29,40]. The authors, in a pre­vi­ous
work [29], have ver­i­fied the proper func­tion­ing of the mini­cell on
welded au­sten­it­ic SS to study pit­ting cor­ro­sion.
This work attempts to make a con­tri­bu­tion on cor­ro­sion stud­
ies per­formed on welded au­sten­it­ic SS by using an elec­tro­chem­i­cal
mini­cell. The main aspects are related to inter­gran­u­lar cor­ro­sion.
Two welded joints, cor­re­spond­ing to AISI 304 and AISI 316L welds,
are ana­lyzed. Also, for the weld­ing joint of AISI 316L which shows
the best cor­ro­sion resis­tance, a post-weld­ing sen­si­ti­sat­ion heat
Fig. 1. Schematic draw­ing of the mini­cell.
treat­ment is eval­u­ated. Fur­ther­more, the influ­ence of a prior to
weld­ing anneal­ing is stud­ied.

2. Exper­im
­ en­tal tion­ing. It is used the same ref­er­ence elec­trode (Sat­u­rated Cal­o­mel
Elec­trode) as for large-scale exper­i­ments and is located at a close
2.1. Mate­ri­als, heat treat­ments and weld­ing pro­ce­dure dis­tance of the work­ing elec­trode (ca. 9 mm). This posi­tion­ing is
intended to get the best pos­si­ble elec­tri­cal sig­nals. Finally, there
The mate­ri­als used in this work were two com­mer­cial SS grades, is no need to use joint seal­ant at the tip of the cell, the PMMA is
AISI 304 and AISI 316L, 4 mm thick rect­an­gu­lar plate. The chem­ already act­ing as a seal­ant, and no leak­age has been observed.
i­cal com­po­si­tions obtained by emis­sion spec­tros­copy were AISI
304: 0.07%C, 17.5%Cr, 9.15%Ni, 0.51%Si, 1.75%Mn, 0.1%Cu, 0.025%P, 2.3. Cor­ro­sion resis­tance eval­u­a­tion tests
0.007%S, bal­ance Fe; AISI 316L: 0.03%C, 17.21%Cr, 10.27%Ni, 1.86%Mo,
0.36%Si, 1.34%Mn, 0.23%Cu, 0.030%P, 0.003%S, bal­ance Fe. ASTM A262, Practice A [41], was used to estab­lish the qual­ity of
Weld­ments were prepared by an auto­matic Metal Inert Gas the mate­rial accord­ing to the three basic cat­eg ­ o­ries: “step”, “dual”
(MIG) pro­ce­dure with argon as shield gas, no edge prep­a­ra­tion, and “ditch”.
butt joint and AISI 308 type as filler mate­rial. Some AISI 316L Two elec­tro­chem­i­cal tech­niques were used: Elec­tro­chem­i­cal
welded joints were sub­jected to post-weld­ing sen­si­ti­sat­ion heat Po­ten­ti­oki­net­ic Reac­ti­va­tion test (EPR) and Dou­ble Loop Elec­tro­
treat­ments at 750 °C for 6, 24 and 75 hours, and under a stream of chem­i­cal Po­ten­ti­oki­net­ic Reac­ti­va­tion test (DLEPR). Three rep­li­cate
Argon. Some AISI 316L spec­i­mens were, prior to weld­ing, sub­jected test of each work­ing area were per­formed with­out observ­ing sig­
to a solu­tion anneal­ing treat­ment at 1050 °C for 60 min under a nif­i­cant dis­crep­an­cies. Every test was per­formed by means of the
stream of argon before being water quenched. mini­cell which was always applied on the mid­dle of the lon­gi­tu­di­
nal welded joint sec­tion for every weld­ing zone.
2.2. Mini­cell setup EPR was per­formed fol­low­ing ASTM stan­dard G-108 [42], but
since the results were shown to be depen­dent on the degree of
The mini­cell here applied for elec­tro­chem­ic­ al tests allows sur­face prep­a­ra­tion, elec­tro­chem­i­cal con­di­tion­ing was car­ried out.
study­ing sizes in about the 200–1000 lm range. Fig. 1 shows the This allowed using a degree of sur­face prep­a­ra­tion (No. 600 emery-
schematic draw­ing of this mini­cell. To sum­ma­rize, this is a cell paper) which was less severe than the estab­lished by the stan­dard
made in PMMA although Tef­lon could also be used. It is formed test. The elec­tro­lyte was 0.5 M H2SO4 + 0.01 M KSCN and the test
by two parts: the lid and the body and made by con­ven­tional tem­per­a­ture 30 °C ± 1. The exper­i­men­tal param­e­ters of the con­di­
machin­ing tech­niques. The elec­tro­lyte flows in the cell through the tion­ing were the fol­low­ing: a delay of 5 min at open cir­cuit (OC)
upper inlet (5 mm in diam­e­ter) and exits through the lower out­ potential, deaer­ated, an anodic attack ¡220 mVSCE (Sat­u­rated Cal­o­mel
let (1 mm in diam­e­ter). There­fore, the reduc­tion in sec­tion causes Elec­trode), a delay of 2 min at VOC, a cathodic clean­ing at ¡600 mVSCE
a suction effect that con­tin­u­ously ren­o­vates the chem­i­cal spe­cies for 1 min and a delay of 5 min at VOC. Pas­siv­ation is accom­plished
of the work­ing area and allows a con­tin­u­ous flow of fresh elec­tro­ by apply­ing +200 mVSCE for 2 min. The reac­ti­va­tion scan started at
lyte over the work­ing elec­trode area. The dis­turb­ing phe­nom­en ­ on 200 mV until 50 mV below the VOC at a rate of 100 mV/min.
of pos­si­ble bub­bling gets then reduced. The plat­i­num count­er­elec­ DLEPR was car­ried out fol­low­ing the test con­di­tions pro­posed
trode (0.2 mm wire) is posi­tioned in between the work­ing and the else­where [8,43]. The sur­face prep­a­ra­tion of the sam­ple was fin­
ref­er­ence elec­trode, which is con­sid­ered to be the opti­mal posi­ ished with a 1 lm dia­mond pol­ish­ing; the elec­tro­lyte was 0.5 M
2392 C. Gar­cia et al. / Corrosion Science 50 (2008) 2390–2397

H2SO4 + 0.01 M KSCN and the test tem­per­a­ture 30 °C ± 1. There three gran­u­lar (TG) and asso­ci­ated to both aus­ten­ite/d-fer­rite inter­face
stages of the test were: a 5 min delay at VOC to deter­mine cor­ro­sion and slip bands inside of some au­sten­it­ic grains. This fact sug­gested
potential, anodic polar­i­za­tion scan from cor­ro­sion potential (Ecorr) that cer­tain degree of cold work was pres­ent. Addi­tion­ally, for AISI
to 300 mVSCE in the pas­sive range at a scan­ning rate of 100 mV/min 304, the micro­struc­ture on the HAZ, at a dis­tance of 3 mm from the
and a cathodic reac­ti­va­tion scan from 300 mVSCE to VOC. In some weld string, Fig. 3, pre­sented some grooved grain bound­aries but
exper­i­ments, as will be com­mented and dis­cussed later, the pas­ at 6 mm again step struc­ture was observed. The HAZ of AISI 316L at
sive ver­tex potential was shifted from 300 to 200 mV. The results dif­fer­ent loca­tions was clas­si­fied as step.
of the test, expressed as the ratio of the cur­rent den­si­ties, ir/ia, and Because local­ised cor­ro­sion can be caused by the effect of
the charges, Qr/Qa, were used to eval­u­ate sus­cep­ti­bil­ity to IGC or expo­sure to crit­i­cal tem­per­a­tures either while weld­ing or in post-
degree of sen­si­ti­sat­ion (DOS). Qr and ir were the charge and max­i­ weld­ing ser­vic­ing con­di­tions, the AISI 316L weld­ment (resis­tant to
mum reac­ti­va­tion cur­rent den­sity dur­ing reverse scan and Qa and cor­ro­sion in as-welded state) was heat treated at sen­si­ti­sat­ion tem­
ia were the charge and max­i­mum anodic cur­rent den­sity dur­ing per­a­ture (750 °C). Large micro­struc­tural dif­fer­ences were found
anodic scan. depend­ing on treat­ment time [28]. For the shorter time, 6 h, the
most rel­e­vant changes were seen in the weld metal and the fusion
3. Results and dis­cus­sion line. Age­ing of the d-fer­rite and its trans­for­ma­tion into chro­mium
car­bide and sigma phase were observed, also sec­ond­ary aus­ten­ite
3.1. ASTM A262, Practice A and micro­struc­tural char­ac­ter­iza­tion was iden­ti­fied. Addi­tion­ally, the fusion line showed con­tin­u­ous
aged fer­rite string­ers. The HAZ and base mate­rial showed low
ASTM A262, Practice A, was used as a qual­it­ a­tive esti­mate of the degree of sen­si­ti­sat­ion and was clas­si­fied as step.
DOS for the au­sten­it­ic SS weld­ments. Addi­tion­ally, the micro­struc­ Welded joints heated for 24 h showed mas­sive chro­mium car­
tural char­ac­ter­iza­tion of the mate­ri­als being stud­ied here has been bide pre­cip­i­ta­tion in aus­ten­ite/d-fer­rite inter­face, in bound­ary
reported else­where [28]. Four weld­ing zones were dis­crim­i­nated grain and in the twins and slip bands of the HAZ and the base mate­
on each welded joint: weld metal zone, fusion line, heat affected rial [28], Fig. 4a. A slight regen­er­a­tion was observed on the HAZ
zone (HAZ) and base mate­rial. and the base mate­rial when sen­si­tiz­ing for 75 h, Fig. 4b. Although,
The base mate­ri­als showed the expected micro­struc­tural fea­ sen­si­ti­sat­ion was tak­ing place since some grains were entirely sur­
tures [28]: an au­sten­it­ic struc­ture with some prior cold work in the rounded by ditch.
sur­face zone plus some delta fer­rite string­ers in the inner region. The found degree of prior cold work is a mat­ter that must
AISI 304 also presents some scarcely chro­mium car­bides Fig. 2. AISI be accounted for. It is known that low degree of cold work­ing
316L showed some iso­lated r-phase par­ti­cles. The con­tent of the causes the increas­ing of sus­cep­ti­bil­ity to inter­gran­u­lar cor­ro­sion.
type MnS inclu­sions was very low for both steels. The sur­face mor­ Evi­dent sings of prior cold work were observed for base mate­
phol­ogy accord­ing to Practice A was clas­si­fied, for both base mate­ri­ ri­als [28]. Con­se­quently, some 316L sam­ples were sub­mit­ted to
als, as step and asso­ci­ated to non-sen­si­tized stain­less steel. solu­tion anneal­ing before weld­ing in order to remov­ing it and
Weld metal zones of AISI 304 and AISI 316L showed an aus­ten­ get­ting a more homo­ge­neous micro­struc­ture. Sub­se­quently, they
ite/d-fer­rite den­dritic struc­ture [28]. As a con­se­quence of the rapid were sen­si­tized at 750 °C for 75 h. The most rel­e­vant changes
cool­ing a high con­tent of d-fer­rite in the den­dritic bound­aries was were affect­ing to the HAZ and the base mate­rial. The trans­gran­
observed. In the fusion line, it was noticed a sig­nif­i­cant decrease u­lar attack dimin­ished due to both the decom­po­si­tion of the d-
in con­tent and mor­phol­ogy of d-fer­rite [28] for AISI 316L. Addi­tion­ fer­rite and the absence of nucle­ation sites related to slip bands.
ally, at the end of the fusion line the quan­tity of d-fer­rite increased Addi­tion­ally, the inter­gran­u­lar attack was lower for the re­crys­tal­
and also chro­mium car­bides on aus­ten­ite grain bound­ary were lized HAZ, Fig. 5.
observed. There were some com­pletely encir­cled grains in this
thin region, thus was clas­si­fied as ditch struc­ture. Also, the d-fer­ 3.2. Elec­tro­chem­i­cal reac­ti­va­tion of AISI 304
rite showed evi­dent signs of age­ing.
In the HAZ the typ­i­cal recrys­tal­li­za­tion and grain growth was The elec­tro­chem­i­cal reac­ti­va­tion of the welded joint of AISI 304
observed [28]. Fur­ther­more, in the sub-zone of the HAZ, where no is here stud­ied. The main point of inter­est was to inde­pen­dently
recrys­tal­li­za­tion takes place, some pre­cip­i­ta­tion of chro­mium rich deter­mine the DOS of the dif­fer­ent zones of the welded joint by
car­bides devel­oped. The pre­cip­i­ta­tion in the HAZ was mainly trans­ means of the mini­cell. The inter­gran­u­lar sus­cep­ti­bil­ity of this

Fig. 2. Micro­struc­ture of the base mate­rial for AISI 304 after ASTM A262, Practice Fig. 3. Micro­struc­ture of the HAZ for AISI 304 after ASTM A262, Practice A (g.b. = grain
A. bound­aries).
 C. Gar­cia et al. / Corrosion Science 50 (2008) 2390–2397 2393

Fig. 6. Curves of EPR for welded joint of AISI 304.

micro­struc­ture showed a selec­tive dis­so­lu­tion in the in­ter­den­drit­ic

inter­face of the aus­ten­ite/d-fer­rite. The spe­cial cor­ro­sion behav­iour
of weld metal could be explained con­sid­er­ing the dif­fer­ent chem­i­
cal com­po­si­tion of the filler metal (AISI 308 with higher chro­mium
con­tent than the base mate­rial) that favours the d-fer­rite for­ma­tion,
pre­vent­ing the hot crack­ing. The lack of reac­ti­va­tion peak must be
inter­preted as sus­cep­ti­bil­ity to in­ter­den­drit­ic cor­ro­sion.
The reac­ti­va­tion curves of the other three zones exhib­ited a pas­
sive cur­rent pla­teau fol­lowed by well defined reac­ti­va­tion peak. The
fusion line showed a clear reac­ti­va­tion behav­iour with high reac­ti­va­
Fig. 4. Micro­struc­ture of the HAZ for AISI 316L after post-weld­ing sen­si­ti­sat­ion at tion val­ues (Qr = 2380 Cm¡2, ir = 28 Am¡2). The HAZ (Qr = 3460 Cm¡2,
750 °C for (a) 24 h and (b) 75 h fol­lowed by ASTM A262, Practice A.
ir = 29 Am¡2) and the base mate­rial (Qr = 2230 Cm¡2, ir = 20 Am¡2)
dis­played a sim­i­lar scan but the lat­ter show­ing the low­est reac­ti­
va­tion val­ues which sug­gests that tem­per­a­ture on this HAZ region
led to max­i­mum pre­cip­i­ta­tion of chro­mium car­bides. The Qr and
ir increased as the fol­low­ing sequence: base mate­rial, fusion line
and HAZ.

3.2.2. DLEPR test

No reac­ti­va­tion was observed on the reverse scan of DLEPR,
Fig. 7. It was remark­able that this even hap­pened for the fusion

Fig. 5. Micro­struc­ture of the re­crys­tal­lized HAZ of AISI 316L sub­mit­ted to prior-weld­

ing solu­tion anneal­ing and post-weld­ing sen­si­ti­sat­ion at 750 °C for 75 h fol­lowed by
ASTM A262, Practice A.

welded joint was inves­ti­gated and, there­fore, the EPR and DLEPR
tech­niques were selected.

3.2.1. EPR test

Preliminary EPR study of this welded joint has been pub­lished
else­where [29]. It can be observed in Fig. 6 how the weld metal does
not reac­ti­vate; a con­tin­u­ous decrease was reg­is­tered in the cur­rent
den­sity as the potential decreased. This could be inter­preted as an
indi­ca­tion of a non-sen­si­tized region. How­ever, after test­ing the Fig. 7. Curves of DLEPR for welded joint of AISI 304.
2394 C. Gar­cia et al. / Corrosion Science 50 (2008) 2390–2397

line and the HAZ, which showed a well-defined reac­ti­va­tion dur­

ing sin­gle loop tests. There­fore, it became nec­es­sary to mod­ify the
test­ing pro­ce­dure. The KSCN con­cen­tra­tion, scan rate and potential
ver­tex param­e­ters were ana­lyzed. There was an increase in anodic
cur­rent when increas­ing KSCN con­cen­tra­tion but hardly notice­
able reac­ti­va­tion behav­iour was obtained. On the other hand, low­
er­ing scan rate from con­ven­tional 100 mV/min to 50 mV/min, reac­
ti­va­tion was observed for any weld­ing zone. It is because there is
time enough to allow gen­eral cor­ro­sion [30]. Finally, a third option
was to decrease the pas­sive ver­tex potential from 300 mVSCE to
200 mVSCE, then a good agree­ment between EPR and DLEPR results
was observed. This third option was cho­sen for the exper­i­men­tal
pro­ce­dure. The reverse scan polar­iz ­ a­tion curves under this new
setup, Fig. 8, clearly showed rec­og­niz­able reac­ti­va­tion behav­iour
and low ir/ia and Qr/Qa for the fusion line and the HAZ. The ir/ia and
Qr/Qa results were 0.31 and 0.32 for the fusion line and 0.88 and
0.97 for the HAZ.

3.3. Elec­tro­chem­ic­ al reac­ti­va­tion of AISI 316L

EPR and DLEPR tests were here applied by means of the mini­ Fig. 9. Curves of EPR for welded joint of AISI 316L after post-weld­ing sen­si­ti­sat­ion
cell. For as-welded AISI 316L no reac­ti­va­tion was observed after heat treat­ment at 750 °C for 6 h.
the EPR or DLEPR tests. This was not sur­pris­ing since 316L is an
au­sten­it­ic low car­bon SS with Mo con­tent, show­ing there­fore a bet­
ter cor­ro­sion behav­iour than AISI 304. Such weld­ment is cor­ro­sion the charge and cur­rent den­sity reac­ti­va­tion val­ues were the high­
resis­tant but, dur­ing ser­vice, can suf­fer some sen­si­ti­sat­ion. Regard­ est (Qr = 36 Cm¡2, ir = 0.68 Am¡2). The reac­ti­va­tion behav­iour of the
ing this mat­ter a post-weld­ing sen­si­ti­sat­ion heat treat­ment was fusion line was inter­me­di­ate between the HAZ and the base mate­
applied as described in the exper­i­men­tal sec­tion (750 °C for 6, 12 rial (Qr = 5.6 Cm¡2, ir = 0.108 Am¡2).
and 24 h). Preliminary EPR study of 316L welded joint has been Fig. 10 shows micro­struc­tures after EPR test. The in­ter­den­drit­ic
pub­lished else­where [29]. attack on cast aus­ten­ite grains was observed for the weld metal.
The fusion line showed inter­gran­u­lar attack on au­sten­it­ic grains
3.3.1. EPR test and trans­gran­u­lar attack on aus­ten­ite/d-fer­rite inter­face. The HAZ
After post-weld­ing sen­si­ti­sat­ion heat treat­ment at 750 °C showed intense inter­gran­u­lar attack. Finally, the base mate­rial
for 6 h, Fig. 9, the del­e­te­ri­ous effect of sen­si­ti­sat­ion was found showed a much slight inter­gran­u­lar attack and some trans­gran­u­lar
to be act­ing on every zone. The weld metal zone showed a con­ attack on the aus­ten­ite/d-fer­rite inter­face.
tin­u­ous decrease of cur­rent den­sity and only a slight reac­ti­va­tion The very neg­a­tive effect of sen­si­ti­sat­ion on the weld metal
(ir = 25.99 Am¡2). Addi­tion­ally, remark­able over­all cur­rent den­sity deserves cer­tain extra com­ments. The cur­rent den­sity was two
incre­ment and Ecorr shift­ing to less noble val­ues were observed. orders of mag­ni­tude higher, which could be related to seg­re­ga­tion
The other three zones exhib­ited clear reac­ti­va­tion with the base and micro­struc­tural age­ing of the d-fer­rite. Micro­graphic anal­y­sis
mate­rial show­ing min­i­mum Qr = 4.5 Cm¡2 and ir = 0.09 Am¡2. The after EPR test revealed than exten­sive in­ter­den­drit­ic cor­ro­sion
HAZ reac­ti­va­tion scan was shifted towards less noble potential and rather than IGC occurred. The high cur­rent den­sity should mainly
higher cur­rent den­si­ties with respect to the base mate­rial, while be asso­ci­ated to the attack at the den­dritic bound­ary. There­fore, the
cor­ro­sion resis­tance of the weld metal is lower than the base mate­
rial because of seg­re­ga­tion, this also has been detected for oth­ers
welded joints [9,24,22]. In fact the behav­iour of the weld deposit
is deter­mined by the min­i­mum con­tent of pas­siv­at­ing ele­ments in
the den­drite cores while extra con­tent of Cr and Mo are found in
grain bound­aries [9]. Also sigma phase, what can rap­idly be formed
by the trans­for­ma­tion of the fer­rite under sen­si­ti­sat­ion con­di­tions,
must degraded cor­ro­sion resis­tance in the weld metal sine sigma
phase gen­er­ates wider and deeper chro­mium deple­tion areas [24].
The effect of sen­si­ti­sat­ion time on EPR test param­e­ters is given
in Table 1. Sen­si­ti­sat­ion for 24 h pro­moted an increase on IGC
sus­cep­ti­bil­ity for all ana­lyzed zones but with the same trend as
observed for 6 h. The weld metal showed again dif­fer­ent reac­ti­va­
tion scan mor­phol­ogy, max­i­mum cur­rent den­si­ties, min­i­mum cor­
ro­sion potential and in­ter­den­drit­ic attack. The HAZ and the base
mate­rial were the zones show­ing a slightly stron­ger increase in
reac­ti­va­tion val­ues in rela­tion to the treat­ment at 6 h. Both regions
showed impor­tant increase of inter­gran­u­lar attack but the HAZ
kept show­ing the high­est DOS. The attacked regions on the base
mate­rial were inter­gran­u­lar and also, up to some extent, trans­gran­
u­lar. The fusion line showed an inter­me­di­ate behav­iour between
the weld metal and the base mate­rial. The micro­struc­ture devel­
Fig. 8. Curves of DLEPR for welded joint of AISI 304 under new con­di­tions (pas­sive
oped after test­ing showed mixed in­ter­den­drit­ic and inter­gran­u­lar
ver­tex potential at 200 mV). attack.
 C. Gar­cia et al. / Corrosion Science 50 (2008) 2390–2397 2395

Table 1
EPR test param­e­ters for AISI 316L weld­ing joint as a func­tion of post-weld­ing sen­si­
ti­za­tion time and weld­ing zones

Sen­si­ti­za­tion Weld­ing zones Ecorr (10¡3 V) Qr (C/m2) ir (A/m2)

time
6 h Weld metal ¡334 145.9 2.57
Fusion line ¡292 5.6 0.10
HAZ ¡329.5 36.5 0.68
Base metal ¡293.5 4.5 0.09
24 h Weld metal ¡364 – –
Fusion line ¡304 21.1 0.46
HAZ ¡328 158.4 2.69
Base metal ¡289 16.2 0.32
75 h Weld metal ¡349 – –
Fusion line ¡335.5 210.5 3.33
HAZ ¡343 319.13 4.59
Base metal ¡343 126.37 1.934

pre­vi­ous anal­y­sis (weld­ing joint with equiv­a­lent post-welded sen­

si­ti­sat­ion but with­out prior anneal­ing). In fact, the weld metal still
showed con­tin­u­ous anodic dis­so­lu­tion but anodic cur­rent den­sity
was lower. The d-fer­rite trans­for­ma­tion dur­ing anneal­ing could
explain it. Fur­ther­more, the effect on the base mate­rial was del­e­
te­ri­ous. Reac­ti­va­tion potential shifted to more noble potential in
addi­tion to an incre­ment of reac­ti­va­tion val­ues (ir and Qr). Sur­face
after test­ing showed some com­pletely dis­solved grain bound­aries
and intense attack on trans­formed d-fer­rite bands. In the HAZ, the
two sub-zones, recrys­tal­li­za­tion and grain growth, were remark­
ably dif­fer­en­ti­ated, mak­ing pos­si­ble to sep­a­rately ana­lyz­ing them.
The re­crys­tal­lized HAZ showed the best behav­iour in agree­ment
with the low inter­gran­u­lar attack detected on micro­struc­tural char­
ac­ter­iza­tion. The grain growth HAZ showed the high­est reac­ti­va­
tion param­e­ters thus it can be said that cor­re­sponds to the most
crit­i­cal region of all.
The observed wors­en­ing on inter­gran­u­lar cor­ro­sion resis­tance
for solu­tion weld­ments must be related, among other fac­tors, to
the decreas­ing amount of d-fer­rite. This causes the sup­pres­sion of
aus­ten­ite/d-fer­rite inter­face as nucle­ation site of chro­mium pre­cip­i­
tates, the chro­mium deple­tion asso­ci­ated to age­ing of d-fer­rite and
the lower sta­bil­ity of pas­sive film [44]. Also the ben­e­fi­cial effect
of d-fer­rite on IGC [45–47] and resis­tance to hot crack­ing [26] has
been widely reported. There­fore, solu­tion anneal­ing prior to weld­
ing is not rec­om­mended.

Fig. 10. Micro­struc­tures of welded joint zones of AISI 316L weld­ment after sen­si­ti­
sat­ion at 750 °C for 6 h and EPR test. (a) Weld metal and fusion line; (b) HAZ and (c)
base mate­rial.

Sen­si­ti­sat­ion for 75 h, Table 1, pro­moted an addi­tional increase

of reac­ti­va­tion val­ues. The effect was dif­fer­ent for each zone. The
weld metal kept the max­i­mum cur­rent den­si­ties. The fusion line
showed an impor­tant increase of inter­gran­u­lar attack. The base
mate­rial was the region dis­play­ing the high­est incre­ment on reac­ti­
va­tion val­ues. On the con­trary the HAZ showed the low­est. Still the
HAZ showed higher reac­ti­va­tion than the base mate­rial.
The effect of prior to weld­ing solu­tion anneal­ing is here ana­
lyzed. A subsequent post-welded sen­si­ti­sat­ion treat­ment at 750 °C
for 75 h was applied, Fig. 11. For the HAZ two sub-zones were
tested: the re­crys­tal­lized grain region (less than 3 mm from weld
string) and the typ­i­cal HAZ region (between 3 and 6 mm from weld
string). Some state­ments can be out­lined when com­par­ing with Fig. 11. Curves of EPR for welded joint of AISI 316L.
2396 C. Gar­cia et al. / Corrosion Science 50 (2008) 2390–2397

3.3.2. DLEPR test Again, like for 304, the HAZ showed the higher DOS val­ues. The
The mod­i­fied DLEPR test (pas­sive ver­tex potential at 200 mV), ir/ia and Qr/Qa results were 0.17 and 0.20 for the fusion line and 0.32
like EPR, did not revealed any sen­si­ti­sat­ion. There­fore 316L welded and 0.37 for the HAZ. All these val­ues are con­sid­er­ably lower than
joint was much more resis­tant to pre­cip­i­ta­tion of chro­mium car­ those for 304 with­out sen­si­ti­sat­ion, which indi­cates the deci­sive
bides than its equiv­a­lent 304L which is mainly due to the pres­ence effect of chem­i­cal com­po­si­tion on inter­gran­u­lar cor­ro­sion sus­cep­
of molyb­de­num and the low car­bon con­tent. ti­bil­ity.
After sen­si­ti­sat­ion at 750 °C for 75 h, DLEPR was able to detect The DLEPR detects the effect of anneal­ing prior to weld­ing of
small DOS, Fig. 12. The weld metal did not show any sing of reac­ti­ 316L, Fig. 13. Com­par­ing Fig. 12 with Fig. 13, the neg­a­tive effect of
va­tion in the reverse scan, a con­tin­u­ous dis­so­lu­tion was observed. anneal­ing, already estab­lished by EPR, was con­firmed. The sen­si­
Com­par­ing with the other zones, the anodic and pas­sive cur­rent tized base mate­rial devel­oped a clear reac­ti­va­tion. The HAZ and
den­si­ties were the high­est in the for­ward and reverse scans. The the fusion line showed an impor­tant incre­ment on DOS. The ir/ia
HAZ and the fusion lines showed reac­ti­va­tion in the reverse scan. and Qr/Qa results were 1.29 and 2.18 for the fusion line and 3.77
The base mate­rial did not show any peak on the reverse scan and 4.73 for the HAZ. Like pre­vi­ously com­mented this could be
though cur­rent den­si­ties were more than one order of mag­ni­tude attrib­uted to the pres­ence of inter­me­tal­lic phases which are a con­
lower than the weld metal. se­quence of the d-fer­rite age­ing. This must be suf ­fi­cient to make it
sus­cep­ti­ble to IGC.
Finally, com­par­ing dou­ble loop with sin­gle loop test meth­ods,
it can be con­cluded that results are in agree­ment and both give a
quan­ti­ta­tive esti­ma­tion of the sen­si­ti­sat­ion. DLEPR showed lower
sen­si­tiv­ity to inter­gran­u­lar cor­ro­sion though its repro­duc­ibil­ity
was excel­lent. DLEPR is espe­cially advis­able for mate­ri­als with
high DOS such as AISI 304 while EPR is advis­able for mate­ri­als like
AISI 316L which show lower DOS. The reac­ti­va­tion results are con­
sis­tent with the micro­struc­tures observed after Practice A which is
use­ful from a qual­i­ta­tive point of view.

4. Con­clu­sions

The main con­clu­sion is that the small-scale elec­tro­chem­i­cal

tech­nique described in this work allows study­ing the degree of sen­
si­ti­sat­ion on welded joints of au­sten­it­ic stain­less steels on every
weld­ing zone and sep­a­rately. The inter­gran­u­lar cor­ro­sion sus­cep­ti­
bil­ity of the dif­fer­ent weld­ing zones has been eval­u­ated by EPR and
DLEPR meth­ods and has been cor­re­lated with the local vari­a­tions
in mate­rial com­po­si­tions and micro­struc­ture caused by the weld­
ing pro­ce­dure and heat treat­ments.
The AISI 316L weld­ment shows, as expected, a bet­ter inter­
gran­u­lar cor­ro­sion resis­tance than AISI 304. For both welds, the
HAZ is the most crit­i­cal region. Its sus­cep­ti­bil­ity is related to the
degree of chro­mium car­bide pre­cip­i­ta­tion on grain bound­ary.
Fig. 12. Curves of DLEPR for welded joint of AISI 316L after sen­si­ti­sat­ion at 750 °C for
75 (pas­sive ver­tex potential at 200 mV).
Inter­gran­u­lar cor­ro­sion resis­tance of AISI 316L can be strongly
affected by micro­struc­tural changes induced by post-weld­ing
heat treat­ments. The in­ter­den­drit­ic attack in weld metal, age­ing
of d-fer­rite in the fusion line and chro­mium deple­tion on grain
bound­aries in the HAZ are the most rel­e­vant micro­struc­tural phe­
nom­ena. For post-weld­ing heat treated joints, anneal­ing prior
to weld­ing was clearly del­e­te­ri­ous, espe­cially for the base mate­
rial. Such fact is related with the d-fer­rite trans­for­ma­tion dur­ing
anneal­ing.

Acknowl­edge­ment

Finan­cial sup­port from Di­rec­ción Gen­eral de In­ves­ti­ga­ción, Min­

is­te­rio de Ed­u­ca­ción y Cien­cia, Spain, ref­er­ence MAT2004-00354 is
grate­fully acknowl­edged.

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