Corrosion Science 52 (2010) 620–626

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

In-situ investigation on the pitting corrosion behavior of friction stir welded joint
of AA2024-T3 aluminium alloy
Ju Kang b, Rui-dong Fu a,b,*, Guo-hong Luan c, Chun-lin Dong c, Miao He c
a
State Key Laboratory of Metastable Materials Science and Technology, Qinhuangdao, Hebei Prov. 066004, PR China
b
College of Materials Science and Engineering, Yanshan University, Qinhuangdao, Hebei Prov. 066004, PR China
c
China FSW Center, Beijing FSW Technology Limited Company, Beijing 100024, PR China

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

Article history: The surface corrosion behavior of an AA2024-T3 aluminium alloy sheet after friction stir welding was
Received 18 July 2009 investigated by using an ‘‘in-situ observation” method. SEM observations showed that the density and
Accepted 21 October 2009 degree of the pitting corrosion in the shoulder active zone were slightly larger compared to the other
Available online 27 October 2009
regions on the top surface. The origins of the pitting corrosion were in the regions between the S phase
particles and the adjacent aluminium base. The effect of Al–Cu–Fe–Mn–(Si) intermetallic compounds on
Keywords: the pitting corrosion was attributed to their high self-corrosion potential which induced the anodic dis-
A. Aluminium
solution of the surrounding aluminium matrix.
A. Intermetallics
B. SEM
Ó 2009 Elsevier Ltd. All rights reserved.
C. Pitting corrosion
C. Welding

1. Introduction
High strength AA2024 aluminium alloy, as a typical precipita-
tion hardening aluminium alloy, is difficult to join by conventional
techniques, such as Gas Tungsten Arc Welding (GTAW) and Gas
Metal Arc Welding (GMAW), because of hot cracking sensitivity
and significant strength drop in the joint [1]. Friction stir welding
(FSW), invented by The Welding Institute (TWI) in 1991 as a new
solid state joining technique that can provide localized modifica-
tion and control of microstructures [2], has the advantage of
reducing the grain size, refining the microstructure and improving
the mechanical properties compared to conventional welding. FSW
is ideal for joining aluminium alloys, especially AA2000 and
AA7000 series aluminium alloys [3–5].
In the welding field, extensive research on friction stir welded
joints for AA2000 or AA7000 series aluminium alloys have been car-
ried out in the past decade focusing on microstructural characteristics
[6–8], mechanical properties [9–11], residual stress analysis [12–14],
plastic flow patterns [15,16] and numerical simulation for the tem-
perature field [17–19]. However, there are only a few investigations
related to the corrosion properties of the FSW aluminium alloys.
Davenport et al. [20,21] reported that an AA2024-T351 welded
joint by FSW is susceptible to corrosion both in the nugget and HAZ
* Corresponding author. Address: State Key Laboratory of Metastable Materials
Science and Technology, Yanshan University, No. 438, Hebei Avenue, Qinhuangdao,
Hebei Prov. 066004, China. Tel.: +86 335 8074795; fax: +86 335 8074545.
E-mail address: rdfu@ysu.edu.cn (R.-d. Fu).
regions. The nugget zone shows greater cathodic activity as a result
of the increasing number of intermetallic compound particles from
the precipitation process. Biallas et al. [22] revealed that localized
corrosion predominantly occurs near the thermo-mechanical
affected zone (TMAZ) after friction stir welding of AA2024 alumi-
nium alloy. Paglia et al. [23,24] investigated the corrosion behavior
of AA7075-T6 after using FSW processing. Their experimental re-
sults showed that the heat-affected zones are the most susceptible
to stress corrosion cracking (SCC). In addition, the corrosion behav-
ior is influenced by the intermetallic phases as well as the phases
in the grain boundary. In general, it is accepted that the welded
zones are more sensitive to corrosion than the aluminium matrix
in both AA2024-T3 and AA7075-T6 alloys after using FSW process-
ing. However, all of these works mainly focused on the corrosion
behavior of welded materials in the cross section. There is scarce
literature on the investigation of corrosion behavior on the top sur-
face of the FSW joints. In fact, the surfaces of the majority of
AA2000 or AA7000 series aluminium alloy sheets have a thin clad-
ding layer of pure aluminium to prevent corrosion. The thin clad-
ding layer will inevitably be destroyed during FSW. Because
corrosion attack often begins on the top surface, the study of the
surface is actually significant. The objective of this work is to deter-
mine the corrosion susceptibility of the exposed microstructures
on the top surface after FSW processing, so it will be more signifi-
cant in terms of industrial application.
For high strength age-hardening aluminium alloys it is well
known that precipitates play an important role in corrosion
performance. According to the comparison of the self-corrosion

0010-938X/$ - see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.corsci.2009.10.027
 J. Kang et al. / Corrosion Science 52 (2010) 620–626
Table 1
Chemical composition of 2024-T3 Al alloy (wt.%).
Si Fe Cu Mg Mn Zn
0.21 0.18 4.42 1.56 0.61 0.13
potentials among different typical precipitates, it is known that the
self-corrosion potential of S phase has the lowest value in AA2024
alloy. Thus the S phase always acts as anodic polarity taking prior-
ity of dissolving over the aluminium matrix in a NaCl solution.
Moreover, the investigation details show that the S phase initially
exhibits anodic activity and then becomes cathodic in activity
compared with the aluminium matrix which is attributed to selec-
tive corrosion [25–30]. The corrosion features have been observed
by Queiroz et al. using scanning electronic microscopy (SEM) of an
AA2024-T3 alloy [31]. However, there are no adequate studies
focusing on the corrosion progress in the FSW joint and there is
a lack of direct observation by use of the in-situ approach, partic-
ularly from the top surface of FSW joint.
Since the microstructure of the top surface is different from the
cross section of the weld joint and the in-situ observation approach
can directly record the evolution of the pitting corrosion, a novel
in-situ observation method was introduced to characterize the cor-
rosion behavior of different regions on the top surface of a FSW
joint for an AA2024 alloy sheet at T3. In the study, the mechanism
for the pitting corrosion on the top surface after FSW was more
deeply understood by use of the current in-situ observation
technique.
Fig. 1. Microstructures on the top surface of the FSW joint. (a) overview, (b) base metal, (c) HAZ, (d) TMAZ-R, (e) TMAZ-A, (f) SAZ, (g) intermetallics in SAZ.
621
2. Experimental
Al AA2024-T3 aluminium alloy sheets with 1.6 mm in thickness
Bal. were used in the present work. The nominal chemical composition
of this alloy is listed in Table 1. The sheets were joined using a fric-
tion stir welding process with 8 mm shoulder made of H13 steel at
a travel speed of 200 mm/min and a spindle speed of 700 rpm in
the counterclockwise direction. All the welded sheets had been
naturally aged for three months before welding.
The top surface of weld seam was polished by use of a mechan-
o-chemical polishing method with 1 lm diamond paste plus
0.5 wt.% NaOH solution. Etching for metallographic observation
was carried out using Dix-Keller’s reagent (4 ml HF, 6 ml HCl,
10 ml HNO3 and 190 ml H2O). The microstructure in the polished
surface of the weld seam was observed by optical microscopy
(Axiovert 200 MAT). Scanning electron microscopy (SEM, HITACHI
S-4800) with an energy dispersive analysis system using element
mapping mode (EDS, HORIBA EDAX) was employed to obtain the
chemical compositions in particles and the corrosion development
of different intermetallic compound particles in the alloy.
The corrosion immersion test was performed according to the
ASTM G34-01 standard [32]. In order to shorten the experimental
cycle, the EXCO solution was chosen as electrolyte instead of
3.5 wt.% NaCl solution based on the fact that the evolution of the
pitting and exfoliation corrosions can be accelerated in the former
solution [33,34]. The EXCO test solution was prepared as follows:
4.0 M NaCl + 0.5 M KNO3 + 0.1 M HNO3, which pH value was ad-
justed to 0.4 using HNO3 (70 wt.%). And the solution temperature
was maintained at 25 °C using a thermostat.
622 J. Kang et al. / Corrosion Science 52 (2010) 620–626
The current ‘‘in-situ observation” method is described as fol-
lows: first, markers were made at the regions of interest on the
shoulder active zone (SAZ), the heat-affected zone (HAZ), the ther-
mo-mechanical affected zone of the advancing side (TMAZ-A) and
the retreating side (TMAZ-R) of the weld seam as well as the base
metal (BM), then images were taken of the regions around the
markers by SEM. Finally, the samples were removed from the
SEM chamber and immersed in the EXCO solution. After immersing
for a desired time, the samples were dried and put into the SEM
chamber again. After recording the first corrosion features around
the markers, the process was repeated to provide images of the
evolution of the corrosion.
3. Results and discussion
3.1. Results of metallographic observation
The microstructures on the surface layer of the FSW joint, as in
the cross section of the joint, can also be divided into five distinct
regions: SAZ, HAZ, TMAZ-A, TMAZ-R and BM (as shown in Fig. 1).
For the SAZ under the shoulder of the stir tool, many regular small
and short arc shaped stringers (as marked in Fig. 1f) are observed
on the as-polished surface due to the circular extrusion action of
the tool. These stringers are dissimilar to the ‘‘onion rings” feature
in the cross section of the nugget zone. The further observation of
the small black stringers at high magnification is shown in Fig. 1g.
It is noted that they are high density zones of the secondary phase
particles (labeled as 1, 2 in Fig. 1g) which were corroded more se-
verely than the Al matrix after being etched in the Dix-Keller’s re-
agent so that these zones show themselves as black stringers under
the optical microscope. A similar result was observed by Sutton
et al. with SEM [35]. They found that there is a significant differ-
ence between high spindle speed at low travel speed and low spin-
dle speed at high travel speed. When spindle speed is low, the
small black stringers are long and relatively continuous. For the
current welding condition of high spindle speed and low travel
speed, the small black particle stringers become short and discon-
tinuous. This indicates that in this region the features of the micro-
structure correlated with the particle distribution of the
strengthening phase, while this distribution results from the metal
plastic flow in the surface layer during FSW. As known to all, weld-
ing parameters are the key factors affecting the metal plastic flow
in the FSW process, so this finding reveals that the distribution of
the intermetallic compounds can be modified by altering the weld-
ing parameters.
Fig. 2. EDS mapping of particles of S phase in the SAZ.
In addition, the other prominent features are obvious difference
of the size and shape of the grains among the four typical regions.
The grain size is distinctly larger in the HAZ (Fig. 1c) than in BM
(Fig. 1b) due to the heating effect. Comparing the microstructures
of the TMAZ (see Fig. 1d and e) and the HAZ (Fig. 1c), the grains in
the areas adjacent to the tool-shoulder are deformed and elongated
as a result of heat and the tool-shoulder’s friction action, so the
TMAZ extends to the HAZ regions beyond the tool-shoulder active
range. In the SAZ (Fig. 1f), it is seen that the fine, irregular grains
have a difference compared with that in the cross section which
is attributed to the stirring action and incomplete dynamic recrys-
tallization [8,36].
3.2. Identification of the precipitate phases
The results of SEM/EDS analysis of two different typical precip-
itate particles are shown in Figs. 2 and 3. From the EDS mapping of
five elements (Al, Mg, Fe, Mn, and Si) shown in Fig. 2, it is easy to
identify two typical particles: Al2CuMg (S phase, labeled as 1, 2,
and 3) and Al–Cu–Fe–Mn phase (named as Fe-containing phase, la-
beled as 4, 5, and 6). No Al2Cu phases (h phase) in the samples are
found under the current experimental condition. The S phases with
round and rod shapes are found in the surface layer. For the
AA2024-T3 alloy sheet, the precipitates of the S phase from the
aging process are one of the prime strengthening phases (about
60% of all precipitates). The area fraction of the S phase on the sur-
face layer of the alloy is about 2.7% [29]. This is indicates that this
precipitate phase plays an important role in subsequent corrosion.
In addition, the larger particles including richer Mg element would
be corroded faster and more severely than the base aluminium and
other particles in the electrolyte. Another notable character is that
the distribution of the Mg element in the typical particle is heter-
ogeneous. In the center area of the particle, there is more Mg and
Cu than that in the edge of the particle. Therefore, the rate of cor-
rosion from the edge to center among the disperse S phases should
be different in the same corrosion condition. The intermetallic
compounds containing Fe, generally considered as impurity
phases, are also observed (see particles 4, 5, and 6 in Fig.2). These
particles mostly exhibit an angular shape and contain a small
amount of Si element [25,27,29,31,37,38].
Fig. 3 shows an Al–Cu–Fe–Mn–(Si) particle which has been bro-
ken during the FSW process in the SAZ. In other words, the broken
Fe-containing should be from the kind of particles 4, 5, and 6 in
Fig. 2 before welding. They were broken and redistributed in the
aluminium matrix along the rotation direction of the tool during
 J. Kang et al. / Corrosion Science 52 (2010) 620–626 623

Fig. 3. EDS mapping of Al–Cu–Fe–Mn–(Si) particles in the SAZ.

Fig. 4. The corrosion behavior in the different regions during different corrosion periods.
624 J. Kang et al. / Corrosion Science 52 (2010) 620–626
FSW process. Although these particles commonly exhibit notably
in corrosion medium, they also contribute to the pitting corrosion,
especially after being fractured in the aluminium matrix. The cor-
rosion behavior of the broken particles would be different com-
pared to that of the particles before FSW, which will be
discussed further in Section 3.3.
3.3. In-situ observation of corrosion evolution
It is well known that the best approach to investigate the corro-
sion evolution is the in-situ observation technology. Here, the in-
situ method has been employed, and the corrosion features of dif-
ferent regions on the surface layer of FSW joints in EXCO solution
during different corrosion periods are shown in Fig. 4.
The pitting corrosion occurred in every region after being im-
mersed in EXCO solution for 0.5 h. The initial galvanic couple of
pitting corrosion was founded in the region between the S phase
particles and their adjacent aluminium matrix. The S phase parti-
cles as anode took priority in dissolving due to the lower self-cor-
rosion potential compared to the adjacent aluminium matrix. With
increasing immersion time, the S phase particles became smaller
and smaller, which means that the elements Al and Mg in the S
phase were dissolved continuously during the initial stage. With
decreasing content of Al and Mg element in the S phase, the change
in the distribution of Cu element from the edge to the center in the
particle resulted in raising the self-corrosion potential of the S
phase. Consequently, the S phase conversely acted as the cathode
and led to the anodic dissolution of the adjacent aluminium ma-
trix. This result supports the polarity reverse theory for the S phase
proposed by Buchheit [29]. There is another likely explanation for
the dissolution of the aluminium matrix around the S phase parti-
cles. The result shown in Fig. 4 reveals that the dissolution of alu-
minium base is likely to be caused by a local alkalization [39].
However, this mechanism of corrosion is not fully supported by
the experimental evidence in this work, because the corresponding
cathodic reactions (water/oxygen reduction which need the local
Fig. 5. The corrosion behavior of Al–Cu–Fe–Mn–(Si) phase in HAZ. (a) before immersion, (b) the EDS spectra of the particle, (c) after being immersed for 0.5 h, (d) after being
immersed for 2 h.
PH > 9) can not occur in the EXCO solution (the PH  0.4 in this
solution).
In addition, from the result as shown in Fig. 4, a notable inter-
esting feature of the corrosion (see the square marked in the
SAZ) is that there exists an Fe-containing phase surrounding an S
phase in the center of the particle. The dissolution rate of the kind
of particle with the S phase plus the Fe-containing phase seems to
be faster than that of other single particle. It is because of the Fe-
containing intermetallic compounds having a self-corrosion poten-
tial of 0.35VSCE in chloride-containing solutions, 0.3VSCE positive
to aluminium matrix ( 0.65VSCE) of AA2024-T3 [40], so that the
more active galvanic couple (S phase plus Fe-containing phase) is
founded at this position.
Further investigation of the effect of the Fe-containing phase on
the corrosion behavior in the HAZ and the SAZ is shown in Figs. 5
and 6, respectively. Fig. 5a shows a typical configuration of Fe-con-
taining phase in the HAZ. An EDS result on the Fe-containing phase
is shown in Fig. 5b. After being immersed for 0.5 h, slight corrosion
occurred on the edge of the phase (see the arrow position in
Fig. 5c). When being immersed for 2 h, the Fe-containing phase
as cathode has induced the dissolution of the matrix in their vicin-
ity, and the corrosion extent became more severe. There are a cer-
tain number of micro cracks in the particles broken after rolling
(see the square zone in Fig. 5a). The micro cracks with the Al matrix
constitute a micro-corrosion primary cell so that pitting corrosion
preferentially occurs between the Al matrix and its neighboring Fe-
containing phase. The effect of Fe-containing phase on the corro-
sion behavior in the SAZ is shown in Fig. 6. It is seen that larger par-
ticles were broken into small pieces due to the severe mechanical
stirring action of the stir tool. Pitting corrosion occurred in the sur-
roundings of these fine Fe-containing phases after being immersed
for 2 h. So the anodic dissolution of the matrix occurred around the
fine and dense particles of Fe-containing phases as around the
coarse and thin ones in the HAZ or BM. In other words, the pitting
corrosion density is increased in the shoulder active region. Be-
cause of this, the corrosion resistance will be reduced in this zone.
 J. Kang et al. / Corrosion Science 52 (2010) 620–626
Fig. 6. The corrosion behavior of Al–Cu–Fe–Mn–(Si) phase in SAZ. (a) before immersion, (b) after being immersed for 0.5 h, (c) after being immersed for 2 h.
From the above analysis, it can be concluded that the secondary
phase particles are the main source of the pitting corrosion for FSW
joint of the AA2024-T3 alloy. The welding parameters are impor-
tant factors for the redistribution of different particles, especially
for the Fe-containing phase in the SAZ. The corrosion resistance
property of FSW joint could be improved by optimizing the weld-
ing parameters.
4. Conclusions
In this study, in-situ observation of the pitting corrosion behav-
ior for a friction stir welded joint of AA2024-T3 aluminium alloy
sheet was investigated, the main conclusions are as follows:
(1) Many regular black stringers are observed in the top surface
microstructure of the FSW joint after being etched by Dix-
Keller’s reagent. They consist of very small typical secondary
phase particles. Two types of particles such as Al–Cu–Mg
phase and Al–Cu–Fe–Mn–(Si) phase are observed in the
weld zone and base metal. The size and distribution of these
particles are obviously different in different regions.
(2) After being immersed in EXCO solution for 0.5 h, the pitting
corrosion was observed for all regions of the weld joint’s top
surface. The density and degree of the pitting corrosion for
the shoulder active zone are slightly larger than those in
other regions.
(3) The pitting corrosion initially originates in dissolving of the S
phase and finally develops to the dissolving of the adjacent
matrix due to the raising self-corrosion potential of the S
phase with increase in the corrosion period. The particles
of Al–Cu–Fe–Mn–(Si) phase also contribute to the pitting
corrosion.
(4) The reason for the pitting corrosion is the higher self-corro-
sion potential of the S phase. Optimization of the welding
parameters could improve the corrosion resistance for a
FSW joint of AA2024-T3.
Acknowledgements
The authors thank the China Friction Stir Welding Center, Bei-
jing Friction Stir Welding Technology Limited Company for finan-
cial support. The authors express their gratitude to Ph.D. Xiyu
Wen of the Center for Aluminium Technology, University of Ken-
tucky, USA, for fruitful discussions.
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