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ABSTRACT INTRODUCTION
The corrosion properties of friction-stir-welded (FSW) Friction stir welding (FSW) is a solid-state joining
AA7050-T7651 have been investigated. Immersion in a modi- process1-3 used to join aluminum alloys of all compo-
fied exfoliation corrosion (EXCO) solution showed that the sitions. During FSW, a rotating tool is forced between
grain boundaries in the nugget, partially recrystallized zone two plates and moved along their contact line. The
(PRZ), and heat-affected zone (HAZ) were sensitized. The
frictional heat generated by contact between the tool
most heavily sensitized region was the nugget/PRZ interface.
and plates softens the material within a narrow zone.
Pitting potentials were determined potentiodynamically in
0.6 M sodium chloride (NaCl). The nugget had the lowest pit- The rotating tool provides a continual hot working
ting potential, which was 75 mV less than the parent mate- action transporting the plasticized material from the
rial. The pitting potential of the HAZ was 50 mV less than the leading face of the tool to the trailing edge where con-
parent material. In results from the slow strain rate test, the solidation produces a continuous joint. Although
percent elongation in 0.6 M NaCl for the slowest strain rate melting does not generally occur during FSW, tem-
used was ~20% that in air, indicating susceptibility to stress peratures are sufficiently high and times at tempera-
corrosion cracking. Metallography showed that the fracture ture are long enough to cause dissolution, nucleation,
was intergranular and that the crack path was on the nugget and/or coarsening of strengthening precipitates. The
side of the nugget/PRZ interface. Analytical electron trans-
temperature-time profile changes with distance from
mission microscopy (ATEM) does not conclusively identify a
the nugget causing a gradient in microstructure and
grain boundary, precipitate-free zone, or precipitate chemis-
precipitate morphology. The altered microstructure
try, which correlates with sensitization. These chemistries
are complex and vary with distance from the center line of in the weld zone (areas where the temperature is
the weld. elevated) of FSW AA5454 demonstrated improved
pitting resistance.4 However, investigations have
KEY WORDS: aluminum alloys, friction stir welding, stress shown that weld zones in FSW AA7075-T65 and
corrosion cracking FSW AA7050-T76516 are sensitized. Studies of FSW
AA7075-T65 show the weld zone to be more suscep-
tible to pitting and intergranular corrosion than the
parent material. The work reported here extends pre-
viously reported preliminary slow strain rate (SSR)
results6 showing susceptibility to stress corrosion
Submitted for publication February 2002; in revised form, Sep- cracking (SCC) in FSW AA7050-T7651. Also reported
tember 2002.
* Rockwell Science Center, 1049 Camino dos Rios, Thousand herein are pitting and intergranular corrosion resis-
Oaks, CA 91360. tance results for FSW AA7050-T7651.
0010-9312/03/000045/$5.00+$0.50/0
212 © 2003, NACE International CORROSION—MARCH 2003
CORROSION SCIENCE SECTION
TABLE 1
Chemical Composition of AA7050 Used (wt%)
Si Fe Cu Mn Mg Cr Ti Zr Zn Al
0.04 0.08 2.18 0.1 2.04 <0.01 0.03 0.11 6.49 Bal.
EXPERIMENTAL PROCEDURES
Material
Material used in this study was 6.35-mm-thick
AA7050-T7651 with the composition listed in Table
1. Samples were friction-stir-welded using conven-
tional friction stir welding practices of 100 mm per
minute at 350 rpm.1 Following welding, samples were
tested after naturally aging for 5 months.
Shoulder
passes through the thin-foil specimen, resulting in a partially recrystallized zone (PRZ) due to the coexist-
spatial resolution on the order of 40 nm. Grain ence of both deformed grains and a necklace of re-
boundary and grain interior compositions were mea- crystallized fine grains in the grain boundaries of the
sured between precipitate particles. Compositions deformed grains. Extending 10 mm to 12 mm beyond
are reported as atomic percents. Each value reported the PRZ is the HAZ, where the microstructure has
is the average of 3 to 6 measurements, and ± values been affected by the thermal transient generated
reflect the maximum deviation from the mean in during FSW but without deformation.8
those measurements. Optical micrographs in Figure 3 show the sever-
ity of attack with exposure time to the modified
RESULTS EXCO solution. Within 2 h of exposure, attack ini-
tiates in the nugget at its boundary with the PRZ
The FSW process generates a unique microstruc- (Figure 3[a]). Figure 3(b) is a higher magnification
ture. This is shown in the optical cross-sectional view SEM photomicrograph of the attacked region in Fig-
(Figure 2) of the weld zones. Figure 2 is a transverse ure 3(a) and shows that the initial attack is inter-
view in the weld travel direction. The weld advancing granular in the recrystallized, fine grain equiaxed
side (i.e., the side where the tangential rotating tool microstructure of the nugget. After exposure for 6 h,
velocity opposes the travel direction) is characterized the intergranular attack becomes more extensive in
by the shoulder at the top of the nugget. The weld the region of the PRZ/nugget boundary and also
nugget has a fine grain, fully recrystallized micro- spreads into the PRZ and the HAZ (Figure 3[c]).
structure. Adjacent to the nugget there is a small Polarization curves for various weld regions are
transition zone with parent metal grains deformed shown in Figure 4. The anodic-to-cathodic transition
upward toward the top surface with fine grains potential for the parent material (–1,070 mV) is lower
located within the grain boundaries. This is a transi- than that of the HAZ (–960 mV) and the nugget
tion zone between the fully recrystallized nugget and (–980 mV). The nugget has the lowest pitting potential
the conventional pancake grain parent metal. Some (–825 mV) compared to the pitting potential for the
investigators believe this transition region is created HAZ (–800 mV) and the parent material (–750 mV).
via recovery. However, recovery is usually defined as Nominal stress vs elongation curves of the trans-
the restoration of physical properties without any ob- verse FSW AA7050-T7651 specimens were obtained
servable change in microstructure, and this transi- using the SSR apparatus.9 Susceptibility to SCC is
tion microstructure is decidedly different from that in expressed as the ratio of the total elongation for
either the nugget or the parent metal. Thus, for clari- specimens exposed to the NaCl solution to the aver-
fication in this manuscript, we have elected to iden- age value obtained in dry air. Dry air measurements
tify the region just adjacent to the nugget as a were made at two strain rates with total elongations
(a) (a)
(b) (b)
FIGURE 6. Specimen fractured in solution at a strain rate of 3 ×
10–4 s–1: (a) optical cross-sectional view showing the fracture through FIGURE 7. Specimen fractured in solution at a strain rate of 3 ×
the HAZ with the shoulder of the nugget in the upper right and 10–6 s–1: (a) optical cross-sectional view and (b) SEM view of the
(b) SEM view of the fracture face. intergranular fracture face.
tion of 2.7% compared to 1.4% for the specimen in the grain interiors are larger and more numerous
pulled in solution at 3 × 10–7 s–1. The optical macro- in the PRZ-at-nugget (Figure 8[c]) compared to those
graph of the failure cross section and the SEM micro- in the nugget (Figure 8[b]). This occurs because the
graph of the fracture surface were identical to those deformation in the PRZ is accompanied by a rise in
of the specimen tested in solution (Figure 7). temperature, which allows preexisting strengthening
The TEM analysis showed that the grain bound- precipitates to coarsen. (Note that the strengthening
ary precipitate size decreased when moving away precipitates are quite numerous and much smaller in
from the hottest region of the weld (i.e., from the the base metal [Figure 8(d)].) However, the deforma-
nugget center to the HAZ, Figure 8). These large an- tion is much more severe and the temperature is
gular grain boundary precipitates have a composition much higher in the nugget. Here, the preexisting pre-
of Mg(Zn2AlCu). There was no significant difference cipitates are taken into solution at the higher tem-
between the intergranular precipitate density in the perature generated during the friction stir process
nugget center and that in the nugget at the PRZ in- and only re-precipitate during cooling.
terface. Beyond the PRZ/nugget interface, the den- Table 2 presents composition results obtained
sity decreases, moving away from the nugget center. using analytical transmission microscopy. The analy-
In addition, there is a large precipitate-free zone ses gives compositions of grain boundaries and grain
(PFZ) adjacent to the boundaries in the PRZ near the interiors (away from particles) at four locations (i.e.,
PRZ/nugget interface. The strengthening precipitates center of the nugget, nugget boundary, PRZ at the
(a) (b)
(c) (d)
FIGURE 8. Comparison of grain boundary precipitation in FSW AA7050-T7651: (a) nugget center, (b) nugget at PRZ,
(c) PRZ at nugget, and (d) base metal.
nugget, and the base alloy). The grain boundaries at crease in the Zn content in the grain interiors in
the nugget center had the lowest Cu composition. moving from the nugget to the base metal; whereas,
The difference between the Cu concentration in the the Zn content in the boundaries in the nugget at the
boundaries and the grain interiors was greater at the PRZ boundary and in the PRZ at the nugget bound-
nugget center than that in the other regions ana- ary was the same as that in the boundaries in the
lyzed. However, the concentrations of Mg and Zn con- parent alloy.
centrations in the grain boundaries and the grain
interiors were approximately the same at the nugget DISCUSSION
center. At all other locations, compositions of Mg and
Zn in the grain interiors and grain boundaries were These results show that FSW AA7050-T7651 is
different; whereas, the Cu concentration was ap- sensitized to corrosion in the as-welded condition.
proximately the same as the base metal concentra- The sensitized region is susceptible to intergranular
tion. The Mg and Zn concentrations were highest in corrosion in the modified ASTM EXCO test solution
the center of the nugget. There was a monotonic de- and intergranular SCC in 0.6 M NaCl. The most
TABLE 2
Grain Boundary and Grain Interior Chemistry (a/o) in Locations in FSW AA7050-T7651
Location
Grain Boundary Grain Interiors
Region of FSW AA7050 Cu Mg Zn Cu Mg Zn
Center of nugget 0.5 ± 0.3 2.3 ± 0.0 3.0 ± 0.2 0.9 ± 0.1 2.9 ± 0.1 3.1 ± 0.5
Nugget at PRZ 1.0 ± 0.3 1.2 ± 0.8 1.8 ± 0.3 1.1 ± 0.2 0.7 ± 0.2 2.8 ± 0.7
PRZ at nugget 1.1 ± 0.3 1.2 ± 0.1 1.7 ± 0.3 1.2 ± 0.3 4.0 ± 0.6 2.5 ± 0.6
Base metal 1.1 0.3 1.8
heavily sensitized zone is a narrow region in the (3 × 10–7 s–1), further appear to support a hydrogen
boundary between the PRZ and the nugget where in- mechanism. These results are in contrast with those
tergranular corrosion first occurs and where the SCC from specimens pulled in dry air at 3 × 10–4 s–1 and
crack propagates. 3 × 10–7 s–1 where a ductile transgranular fracture
The weld nugget has a lower pitting potential mode was observed. However, it is not unequivocal
than either the HAZ or the parent metal. It was not that hydrogen caused the loss of ductility in the pre-
possible to fabricate a specimen by isolating the nug- soaked specimen since the presence of bubbles at
get/PRZ interface for pitting potential measurements. numerous points on the surface indicated that solu-
Thus, it is not known if the region most susceptible tion was trapped in cavities and capillaries under
to intergranular corrosion and SCC was also the some intermetallics causing localized corrosion. Un-
most susceptible to pitting. The weld zone, having like these results for FSW AA7050-T7651, the SSR
the lowest pitting potential, differed from results test results from others for parent AA7050-T7651
reported previously5 for FSW AA7075-T6. In these shows a minimum in the ductility/strain rate curve
earlier results, the HAZ of FSW AA7075-T6 had the in a NaCl environment, which suggest an anodic dis-
lowest pitting potential, and the nugget had a pitting solution SCC mechanism.14 Other results show no
potential between that of the HAZ and the parent loss in ductility in hydrogen-charged specimens.15
metal. However, the relationship between the Cu con- Although a comparison of results for FSW AA7050-
centration in the weld zones of the two FSW alloys T7651 and the parent base alloy AA7050 suggest the
followed the same trends (i.e., the lowest pitting po- SCC mechanism is different in the two material con-
tential was in the zone with the lowest Cu concentra- ditions, it is not definitive because of the uncertain-
tion). This observation is in accordance with results ties pointed out above.
that show the pitting potential of Al-Cu alloys in- A complete investigation of the microstructure in
creases with the amount of Cu in solid solution.11 the weld zone of the FSW AA7050-T7651 is beyond
The increasing loss in ductility with decreasing the scope of this paper. However, a comprehensive
strain rate can be explained by invoking either a hy- microstructural analysis has been reported for FSW
drogen or an anodic dissolution mechanism of SCC. AA7075-T6.8 Similar microstructures can be ex-
Available data suggest that when anodic dissolution pected for FSW AA7050-T7651. The most significant
is the cracking mechanism, there is a critical strain change caused by FSW in the sensitized region adja-
rate where the ductility reaches a minimum and then cent to the weld nugget is a coarsening of precipi-
increases as strain rate is decreased.12 No minimum tates caused by rapid grain boundary diffusion of
occurred in the SSR results of FSW AA7050-T7651. solutes. This leads to changes in grain boundary
The absence of a ductility minimum is consistent composition, size of the PFZ, and the grain boundary
with a hydrogen-assisted cracking mechanism of area fraction covered by precipitates. The precipitate
SCC.12 Using this type of correlation between the coarsening rate and relative diffusion rates are loca-
cracking mechanism and the ductility ratio-strain tion dependent because of the weld zone temperature
rate relationship for FSW materials is complicated by gradient. Local changes in composition are likely
the four zones with different microstructure over responsible for changes in both pitting and inter-
which the strain rate is averaged. Strain localization granular corrosion resistance. The intergranular SCC
occurs, increasing the local strain rate by some un- behavior, in both hydrogen and anodic dissolution
known amount.13 However, the microstructures of mechanisms, can depend on composition and
all samples are identical and, accordingly, the SSR whether the type of precipitate promotes homogenous
results are comparable. Results for the presoaked or inhomogeneous slip.15 It has not been determined
specimen, in which very low ductility and intergranu- what composition and microstructure changes,
lar fracture morphology were the same as that of the which occurred during FSW, are responsible for the
specimen pulled in solution at the same strain rate increased sensitivity to corrosion.