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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 regions. The nugget zone shows greater cathodic activity as a result
of the increasing number of intermetallic compound particles from
High strength AA2024 aluminium alloy, as a typical precipita- the precipitation process. Biallas et al. [22] revealed that localized
tion hardening aluminium alloy, is difficult to join by conventional corrosion predominantly occurs near the thermo-mechanical
techniques, such as Gas Tungsten Arc Welding (GTAW) and Gas affected zone (TMAZ) after friction stir welding of AA2024 alumi-
Metal Arc Welding (GMAW), because of hot cracking sensitivity nium alloy. Paglia et al. [23,24] investigated the corrosion behavior
and significant strength drop in the joint [1]. Friction stir welding of AA7075-T6 after using FSW processing. Their experimental re-
(FSW), invented by The Welding Institute (TWI) in 1991 as a new sults showed that the heat-affected zones are the most susceptible
solid state joining technique that can provide localized modifica- to stress corrosion cracking (SCC). In addition, the corrosion behav-
tion and control of microstructures [2], has the advantage of ior is influenced by the intermetallic phases as well as the phases
reducing the grain size, refining the microstructure and improving in the grain boundary. In general, it is accepted that the welded
the mechanical properties compared to conventional welding. FSW zones are more sensitive to corrosion than the aluminium matrix
is ideal for joining aluminium alloys, especially AA2000 and in both AA2024-T3 and AA7075-T6 alloys after using FSW process-
AA7000 series aluminium alloys [3–5]. ing. However, all of these works mainly focused on the corrosion
In the welding field, extensive research on friction stir welded behavior of welded materials in the cross section. There is scarce
joints for AA2000 or AA7000 series aluminium alloys have been car- literature on the investigation of corrosion behavior on the top sur-
ried out in the past decade focusing on microstructural characteristics face of the FSW joints. In fact, the surfaces of the majority of
[6–8], mechanical properties [9–11], residual stress analysis [12–14], AA2000 or AA7000 series aluminium alloy sheets have a thin clad-
plastic flow patterns [15,16] and numerical simulation for the tem- ding layer of pure aluminium to prevent corrosion. The thin clad-
perature field [17–19]. However, there are only a few investigations ding layer will inevitably be destroyed during FSW. Because
related to the corrosion properties of the FSW aluminium alloys. corrosion attack often begins on the top surface, the study of the
Davenport et al. [20,21] reported that an AA2024-T351 welded surface is actually significant. The objective of this work is to deter-
joint by FSW is susceptible to corrosion both in the nugget and HAZ 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.
* Corresponding author. Address: State Key Laboratory of Metastable Materials
Science and Technology, Yanshan University, No. 438, Hebei Avenue, Qinhuangdao,
For high strength age-hardening aluminium alloys it is well
Hebei Prov. 066004, China. Tel.: +86 335 8074795; fax: +86 335 8074545. known that precipitates play an important role in corrosion
E-mail address: rdfu@ysu.edu.cn (R.-d. Fu). 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) 620–626 621

Table 1 2. Experimental
Chemical composition of 2024-T3 Al alloy (wt.%).

Si Fe Cu Mg Mn Zn Al AA2024-T3 aluminium alloy sheets with 1.6 mm in thickness


0.21 0.18 4.42 1.56 0.61 0.13 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
potentials among different typical precipitates, it is known that the the counterclockwise direction. All the welded sheets had been
self-corrosion potential of S phase has the lowest value in AA2024 naturally aged for three months before welding.
alloy. Thus the S phase always acts as anodic polarity taking prior- The top surface of weld seam was polished by use of a mechan-
ity of dissolving over the aluminium matrix in a NaCl solution. o-chemical polishing method with 1 lm diamond paste plus
Moreover, the investigation details show that the S phase initially 0.5 wt.% NaOH solution. Etching for metallographic observation
exhibits anodic activity and then becomes cathodic in activity was carried out using Dix-Keller’s reagent (4 ml HF, 6 ml HCl,
compared with the aluminium matrix which is attributed to selec- 10 ml HNO3 and 190 ml H2O). The microstructure in the polished
tive corrosion [25–30]. The corrosion features have been observed surface of the weld seam was observed by optical microscopy
by Queiroz et al. using scanning electronic microscopy (SEM) of an (Axiovert 200 MAT). Scanning electron microscopy (SEM, HITACHI
AA2024-T3 alloy [31]. However, there are no adequate studies S-4800) with an energy dispersive analysis system using element
focusing on the corrosion progress in the FSW joint and there is mapping mode (EDS, HORIBA EDAX) was employed to obtain the
a lack of direct observation by use of the in-situ approach, partic- chemical compositions in particles and the corrosion development
ularly from the top surface of FSW joint. of different intermetallic compound particles in the alloy.
Since the microstructure of the top surface is different from the The corrosion immersion test was performed according to the
cross section of the weld joint and the in-situ observation approach ASTM G34-01 standard [32]. In order to shorten the experimental
can directly record the evolution of the pitting corrosion, a novel cycle, the EXCO solution was chosen as electrolyte instead of
in-situ observation method was introduced to characterize the cor- 3.5 wt.% NaCl solution based on the fact that the evolution of the
rosion behavior of different regions on the top surface of a FSW pitting and exfoliation corrosions can be accelerated in the former
joint for an AA2024 alloy sheet at T3. In the study, the mechanism solution [33,34]. The EXCO test solution was prepared as follows:
for the pitting corrosion on the top surface after FSW was more 4.0 M NaCl + 0.5 M KNO3 + 0.1 M HNO3, which pH value was ad-
deeply understood by use of the current in-situ observation justed to 0.4 using HNO3 (70 wt.%). And the solution temperature
technique. was maintained at 25 °C using a thermostat.

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.
622 J. Kang et al. / Corrosion Science 52 (2010) 620–626

The current ‘‘in-situ observation” method is described as fol- In addition, the other prominent features are obvious difference
lows: first, markers were made at the regions of interest on the of the size and shape of the grains among the four typical regions.
shoulder active zone (SAZ), the heat-affected zone (HAZ), the ther- The grain size is distinctly larger in the HAZ (Fig. 1c) than in BM
mo-mechanical affected zone of the advancing side (TMAZ-A) and (Fig. 1b) due to the heating effect. Comparing the microstructures
the retreating side (TMAZ-R) of the weld seam as well as the base of the TMAZ (see Fig. 1d and e) and the HAZ (Fig. 1c), the grains in
metal (BM), then images were taken of the regions around the the areas adjacent to the tool-shoulder are deformed and elongated
markers by SEM. Finally, the samples were removed from the as a result of heat and the tool-shoulder’s friction action, so the
SEM chamber and immersed in the EXCO solution. After immersing TMAZ extends to the HAZ regions beyond the tool-shoulder active
for a desired time, the samples were dried and put into the SEM range. In the SAZ (Fig. 1f), it is seen that the fine, irregular grains
chamber again. After recording the first corrosion features around have a difference compared with that in the cross section which
the markers, the process was repeated to provide images of the is attributed to the stirring action and incomplete dynamic recrys-
evolution of the corrosion. tallization [8,36].

3. Results and discussion 3.2. Identification of the precipitate phases

3.1. Results of metallographic observation 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
The microstructures on the surface layer of the FSW joint, as in five elements (Al, Mg, Fe, Mn, and Si) shown in Fig. 2, it is easy to
the cross section of the joint, can also be divided into five distinct identify two typical particles: Al2CuMg (S phase, labeled as 1, 2,
regions: SAZ, HAZ, TMAZ-A, TMAZ-R and BM (as shown in Fig. 1). and 3) and Al–Cu–Fe–Mn phase (named as Fe-containing phase, la-
For the SAZ under the shoulder of the stir tool, many regular small beled as 4, 5, and 6). No Al2Cu phases (h phase) in the samples are
and short arc shaped stringers (as marked in Fig. 1f) are observed found under the current experimental condition. The S phases with
on the as-polished surface due to the circular extrusion action of round and rod shapes are found in the surface layer. For the
the tool. These stringers are dissimilar to the ‘‘onion rings” feature AA2024-T3 alloy sheet, the precipitates of the S phase from the
in the cross section of the nugget zone. The further observation of aging process are one of the prime strengthening phases (about
the small black stringers at high magnification is shown in Fig. 1g. 60% of all precipitates). The area fraction of the S phase on the sur-
It is noted that they are high density zones of the secondary phase face layer of the alloy is about 2.7% [29]. This is indicates that this
particles (labeled as 1, 2 in Fig. 1g) which were corroded more se- precipitate phase plays an important role in subsequent corrosion.
verely than the Al matrix after being etched in the Dix-Keller’s re- In addition, the larger particles including richer Mg element would
agent so that these zones show themselves as black stringers under be corroded faster and more severely than the base aluminium and
the optical microscope. A similar result was observed by Sutton other particles in the electrolyte. Another notable character is that
et al. with SEM [35]. They found that there is a significant differ- the distribution of the Mg element in the typical particle is heter-
ence between high spindle speed at low travel speed and low spin- ogeneous. In the center area of the particle, there is more Mg and
dle speed at high travel speed. When spindle speed is low, the Cu than that in the edge of the particle. Therefore, the rate of cor-
small black stringers are long and relatively continuous. For the rosion from the edge to center among the disperse S phases should
current welding condition of high spindle speed and low travel be different in the same corrosion condition. The intermetallic
speed, the small black particle stringers become short and discon- compounds containing Fe, generally considered as impurity
tinuous. This indicates that in this region the features of the micro- phases, are also observed (see particles 4, 5, and 6 in Fig.2). These
structure correlated with the particle distribution of the particles mostly exhibit an angular shape and contain a small
strengthening phase, while this distribution results from the metal amount of Si element [25,27,29,31,37,38].
plastic flow in the surface layer during FSW. As known to all, weld- Fig. 3 shows an Al–Cu–Fe–Mn–(Si) particle which has been bro-
ing parameters are the key factors affecting the metal plastic flow ken during the FSW process in the SAZ. In other words, the broken
in the FSW process, so this finding reveals that the distribution of Fe-containing should be from the kind of particles 4, 5, and 6 in
the intermetallic compounds can be modified by altering the weld- Fig. 2 before welding. They were broken and redistributed in the
ing parameters. aluminium matrix along the rotation direction of the tool during

Fig. 2. EDS mapping of particles of S phase in the SAZ.


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 PH > 9) can not occur in the EXCO solution (the PH  0.4 in this
in corrosion medium, they also contribute to the pitting corrosion, solution).
especially after being fractured in the aluminium matrix. The cor- In addition, from the result as shown in Fig. 4, a notable inter-
rosion behavior of the broken particles would be different com- esting feature of the corrosion (see the square marked in the
pared to that of the particles before FSW, which will be SAZ) is that there exists an Fe-containing phase surrounding an S
discussed further in Section 3.3. 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
3.3. In-situ observation of corrosion evolution be faster than that of other single particle. It is because of the Fe-
containing intermetallic compounds having a self-corrosion poten-
It is well known that the best approach to investigate the corro- tial of 0.35VSCE in chloride-containing solutions, 0.3VSCE positive
sion evolution is the in-situ observation technology. Here, the in- to aluminium matrix ( 0.65VSCE) of AA2024-T3 [40], so that the
situ method has been employed, and the corrosion features of dif- more active galvanic couple (S phase plus Fe-containing phase) is
ferent regions on the surface layer of FSW joints in EXCO solution founded at this position.
during different corrosion periods are shown in Fig. 4. Further investigation of the effect of the Fe-containing phase on
The pitting corrosion occurred in every region after being im- the corrosion behavior in the HAZ and the SAZ is shown in Figs. 5
mersed in EXCO solution for 0.5 h. The initial galvanic couple of and 6, respectively. Fig. 5a shows a typical configuration of Fe-con-
pitting corrosion was founded in the region between the S phase taining phase in the HAZ. An EDS result on the Fe-containing phase
particles and their adjacent aluminium matrix. The S phase parti- is shown in Fig. 5b. After being immersed for 0.5 h, slight corrosion
cles as anode took priority in dissolving due to the lower self-cor- occurred on the edge of the phase (see the arrow position in
rosion potential compared to the adjacent aluminium matrix. With Fig. 5c). When being immersed for 2 h, the Fe-containing phase
increasing immersion time, the S phase particles became smaller as cathode has induced the dissolution of the matrix in their vicin-
and smaller, which means that the elements Al and Mg in the S ity, and the corrosion extent became more severe. There are a cer-
phase were dissolved continuously during the initial stage. With tain number of micro cracks in the particles broken after rolling
decreasing content of Al and Mg element in the S phase, the change (see the square zone in Fig. 5a). The micro cracks with the Al matrix
in the distribution of Cu element from the edge to the center in the constitute a micro-corrosion primary cell so that pitting corrosion
particle resulted in raising the self-corrosion potential of the S preferentially occurs between the Al matrix and its neighboring Fe-
phase. Consequently, the S phase conversely acted as the cathode containing phase. The effect of Fe-containing phase on the corro-
and led to the anodic dissolution of the adjacent aluminium ma- sion behavior in the SAZ is shown in Fig. 6. It is seen that larger par-
trix. This result supports the polarity reverse theory for the S phase ticles were broken into small pieces due to the severe mechanical
proposed by Buchheit [29]. There is another likely explanation for stirring action of the stir tool. Pitting corrosion occurred in the sur-
the dissolution of the aluminium matrix around the S phase parti- roundings of these fine Fe-containing phases after being immersed
cles. The result shown in Fig. 4 reveals that the dissolution of alu- for 2 h. So the anodic dissolution of the matrix occurred around the
minium base is likely to be caused by a local alkalization [39]. fine and dense particles of Fe-containing phases as around the
However, this mechanism of corrosion is not fully supported by coarse and thin ones in the HAZ or BM. In other words, the pitting
the experimental evidence in this work, because the corresponding corrosion density is increased in the shoulder active region. Be-
cathodic reactions (water/oxygen reduction which need the local cause of this, the corrosion resistance will be reduced in this zone.

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.
J. Kang et al. / Corrosion Science 52 (2010) 620–626 625

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.

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