Microstructural Evolution and Stress Corrosion Cracking

Behavior of Al-5083
R. GOSWAMI, G. SPANOS, P.S. PAO, and R.L. HOLTZ

The fine scale microstructure of Al-5083 (H-131) sensitized at 448 K (175 C) for 1, 10, 25, 50,
100, 240, 500, and 1000 hours has been investigated using transmission electron microscopy
(TEM) to study the evolution of the b phase (Al3Mg2) at grain boundaries and on pre-existing
intragranular particles. In fully sensitized Al-5083, the b phase (Al3Mg2) forms heterogeneously
both at grain boundaries and on pre-existing particles, which are enriched in manganese. TEM
observations showed that the grain boundary precipitation of the b phase initially occurs
between 0 to 1 hour of aging at 448 K (175 C), and that the b phase grows with a ribbonlike
morphology. The grain boundary planes are covered by the b phase after 240 hours of aging.
The contribution of microstructure, defects, and environment on the stress corrosion cracking
(SCC) behavior is discussed.

DOI: 10.1007/s11661-010-0262-y
 The Minerals, Metals & Materials Society and ASM International 2010

I. INTRODUCTION characterization of the SCC behavior, confirming the

A LUMINUM - MAGNESIUM - MANGANESE
alloys are important for ship structural applications,
because they exhibit excellent resistance to corrosion,
weldability, and a high strength to weight ratio. How-
ever, Al-Mg-Mn alloys become susceptible to intergran-
ular corrosion and stress corrosion cracking (SCC) if
exposed to temperatures above 50 C for extended
periods of time, which occurs on ship structures in
service, as a consequence of the formation of the b
phase, Al3Mg2, at grain boundaries.[1–8] The b phase is
strongly anodic relative to the Al matrix; thus, it
corrodes and dissolves very quickly upon exposure to
seawater. Considerable work has been done on the SCC
behavior of Al-5083 as a function of aging at different
temperatures.[3] It was observed that the crack growth
rate increases with aging, which was linked to the
increased volume fraction of the b phase at the grain
boundaries.[3] The rate at which sensitization occurs is a
critical parameter in the prediction of the life cycle of
Al-Mg-Mn ship structural alloys. Detailed study of the
evolution of the beta phase, therefore, is vital to
understanding the evolution of sensitization.
Extensive transmission electron microscopy (TEM)
studies[9] were previously carried out on two types of
Al-5083 specimens provided by ALCOA: as-received in
the H-131 temper condition and subsequently annealed
at 448 K (175 C) for 10 days. Characterization of the
as-received microstructure was important for under-
standing the subsequent formation of various phases
during the annealing procedure. ALCOA also provided
resistance to SCC of the as-received specimens, and
susceptibility to SCC of the annealed material. How-
ever, this first work only encompassed the as-received
condition and the 10-day annealed condition, effectively
fully sensitized. The present study deals with the
evolution of the sensitization at 448 K (175 C) ranging
from the very early stages to heat treatments up to
1000 hours. More specifically, the objective encom-
passes investigation of the b-phase evolution both at
the aluminum matrix grain boundaries and on pre-
existing particles and correlation of the stress corrosion
behavior with the microstructure.
II. EXPERIMENTAL
TEM studies have thus been carried out here on Al-
5083 specimens provided by ALCOA in the H-131
temper condition, and subsequently aged at 448 K
(175 C) for 1, 10, 25, 50, 100, 240, 500, and 1000 hours.
Additional TEM specimens were taken from different
locations across a fracture surface, in order to study
the defects close to the fracture surface. Charac-
terization of the as-received microstructure was also
important, for understanding the subsequent b forma-
tion during the aging procedure. PHILIPS* CM-30
*PHILIPS is a trademark of FEI Company, Hillsboro, OR.
and JEOL** 2200 analytical transmission electron

R. GOSWAMI, G. SPANOS, P.S. PAO, and R.L. HOLTZ,
Scientists, are with the Naval Research Laboratory, Washington, DC
20375. Contact e-mail: ramasis.goswami@nrl.navy.mil
Manuscript submitted December 10, 2009.
Article published online June 2, 2010
**JEOL is a trademark of Japan Electron Optics Ltd., Tokyo.
microscopes operating at 300 and 200 KeV, respectively,
were used to characterize the microstructure of the

348—VOLUME 42A, FEBRUARY 2011 U.S. GOVERNMENT WORK METALLURGICAL AND MATERIALS TRANSACTIONS A
NOT PROTECTED BY U.S. COPYRIGHT
Al-5083. Final thinning of the TEM foils was carried out
in an ion mill with a gun voltage of 5 kV, a current of
5 mA, and a sputtering angle of 10 deg. Fine probe
energy-dispersive X-ray spectroscopy (EDS) was em-
ployed to determine the distribution of Mg, Mn, and Cr
at the grain boundaries, as well as within the matrix
grains and precipitates. Further compositional informa-
tion was obtained with Z-contrast imaging, also termed
high-angle annular dark-field (HAADF) imaging. In
this imaging mode, the brighter regions correspond to
heavier atoms, as the scattering cross section is propor-
tional to Z2.[10]
III. RESULTS AND DISCUSSION
SCC characterization of both the as-received Al-5083
(H-131) and the annealed samples was provided to the
Naval Research Laboratory by ALCOA and shown in
Figure 1. These were measured for a constant crack
opening displacement on precracked double cantilever
beam specimens in the short-longitudinal (S-L) orienta-
tion. A 3 pct brine solution was added dropwise
throughout the experiment. Experimental details were
given elsewhere.[1] Figure 1(a) shows a substantial
increase, 300 pct, of the initial crack length for samples
aged for 240 hours at 448 K (175 C), while a small
increase in crack length, 100 lm (<0.2 pct), was
Fig. 1—(a) Plot showing crack length with time for as-received and sensitized (448 K (175 C) for 240 h) Al-5083 samples in S-L orientation.
(b) Plot showing the decrease in stress intensity factor (K) as the crack length increases. (c) Fracture surface showing predominantly intergranu-
lar fracture. (d) Optical micrograph in S-L orientation showing the elongated grains.
METALLURGICAL AND MATERIALS TRANSACTIONS A
recorded for the as-received samples. The threshold
value of the stress intensity factor (KISCC) turned out to
be 2 MPam after aging for 240 hours at 448 K
(175 C) (Figure 1(b)). Note that there was a sudden
jump of the crack length at around 525 hours
(Figure 1(a)). This was most likely due to accumulation
of the corrosion product, which generated stress and
moved the crack rapidly. The crack length has increased
from 1.8 to 2.2 inches between 25 and 525 hours. Thus,
the average crack velocity was 5 9 10 9 ms 1 in that
time frame for the sample aged at 448 K (175 C) for
240 hours, and for the as-received sample, the velocity
was 4 9 10 11 ms 1. The crack growth rate, therefore,
has increased by almost two orders of magnitude upon
aging the as-received sample at 448 K (175 C) for
240 hours, as compared to that of the as-received
sample. The fracture surface (Figure 1(c)) for the aged
sample showed predominantly intergranular fracture.
The corresponding elongated grain structure in this
orientation is shown in the optical micrograph presented
in Figure 1(d).
Details of the microstructure of the as-received
Al-5083 (H-131), particularly the composition and
structure of several precipitates, were reported in an
earlier study.[9] These results indicated that both
equiaxed particles (50 to 100 nm in size) and rodlike
particles (with lengths ranging from 100 to 800 nm)
were present. Most of the particles (Figure 2) were
VOLUME 42A, FEBRUARY 2011—349
 Fig. 3—(a) Portion of grain boundary in as-received sample showing
no precipitates at the boundary. (b) Grain boundary in as-received
sample showing the Al-Mn-Cr type of precipitates. (c) Bright-field
micrograph showing that a number of dislocations are pinned by the
Al-Mn-Cr type particles.

Fig. 2—(a) HAADF image showing the Al-Mn-Cr type of particles

(appeared bright) in Al-matrix in the as-received Al-5083 sample. (b)
through (e) Fine probe EDS map obtained with spot size of 0.5 nm
showing the distribution of Mg, Al, Mn, and Cr, respectively.

observed to be associated with Mn and Cr and small

amounts of Fe. EDS analysis showed that the majority
of the Mn-rich particles had an average composition of
5.74 at. pct Mn, 0.97at. pct Cr, 0.3 at. pct Fe, and
balance Al. A few particles, however, were identified as
Al6(Mn-Cr). In the as-received condition, no other
solute (Mn, Fe, Cr, or Si) was detected in the a-Al
matrix. It was observed that the a-Al matrix contains
mostly Mg as a solute, ranging from 3.5 to 4 wt pct.
While most of the precipitates are located inside the Fig. 4—Plot showing Vickers hardness as a function of aging.
a-Al grains, the a-Al grain boundaries are mostly free of
Mn-rich precipitates. Figure 3(a) shows a typical grain
boundary with no precipitates in the as-received condi- on existing Al-Mn-Cr type particles, and on dislocations
tion. A few grain boundaries (Figure 3(b)), how- in the as-received condition.
ever, were observed to contain Mn-rich precipitates. The formation of b phase from the supersaturated
Figure 3(c) shows a high density of dislocations in the solid solution has been reported by several authors.[11–13]
as-received sample, and some of the dislocations appear At a higher supersaturation (>10 wt pct Mg), GP zones
to be pinned by the existing Al-Mn-Cr type particles. can form at low temperatures (<50 C), and then can
Dislocations are mostly tangled, and no dislocation transform to b¢¢ and b¢ at 100 C, and finally to
substructures were observed in the as-received condi- equilibrium b phase at around 250 C.[11–13] The trans-
tion. The yield strength is attributable to a combination formation has been found to be extremely sluggish. The
of solid solution strengthening, a relatively high density aging response of the as-received sample was studied by
of dislocations, and Mn-rich particles. No precipitation hardness as a function of aging at 448 K (175 C).
of the beta phase was observed at grain boundaries, Figure 4 is the Vickers hardness plot showing a decrease

350—VOLUME 42A, FEBRUARY 2011 METALLURGICAL AND MATERIALS TRANSACTIONS A

of hardness with aging, which is consistent with previous
observations.[14] The mean hardness was decreased by
almost 10 pct within an hour of aging and by 15 pct for
1000 hours of aging. Such a decrease in hardness
suggests that the matrix supersaturation (particularly
Mg) decreases as a function of aging, since in Al-Mg
alloys, the solid solution strengthening plays a major
part. TEM observations indeed showed that grain
boundary precipitation of the Mg-rich b phase occurs
between 0 to 1 hour of aging at 448 K (175 C).
Selected area electron diffraction patterns (SADPs)
and fine probe EDS were used to detect the grain
boundary b phase. Figure 5(a) shows the beta precipi-
tates along the grain boundary for this 1-hour aging
condition. They appear to form as individual grain
boundary allotriomorphs at different locations along the
grain boundary. The corresponding dark-field image
from the grain boundary allotriomorph indicated as b
phase (1) in Figure 5(a) is shown as an inset (obtained
using a (777) b-phase reflection). The fine probe EDS
obtained from the b-phase (1) precipitate (Figure 5(b))
showed the Mg content is 33 wt pct.
The corresponding Mg content at the grain boundary
in the Al matrix between two such allotriomorphs was
3.3 wt pct. Such b allotriomorphs were observed to
grow considerably along the grain boundary after
10 hours of aging (Figure 6(a)). The b phase was verified
by SADP and EDS. Figure 6(b) is an HAADF image of
the grain boundary b phase showing relatively dark
contrast associated with the lighter element, Mg. The
fine probe EDS map obtained with a spot size of 0.5 nm
from this area (Figures 6(c) and (d)) showed that the
dark contrast in Figure 6(b) is indeed associated with
Fig. 5—(a) Bright-field TEM image for sample aged for 1 h at 448 K (175 C) showing the formation of b phase, shown by arrows, at the grain
boundary. A dark-field TEM image obtained using (777) reflection of the b phase from region (1) is shown as an inset. (b) The fine probe EDS
from the b phase. (c) The fine probe EDS from the grain boundary between two beta-particles.
METALLURGICAL AND MATERIALS TRANSACTIONS A
higher Mg. The EDS line scan (Figure 6(e)) across the b
phase showed the enrichment of Mg and depletion of Al
at the grain boundary. No appreciable depression of Mg
concentration could be detected just adjacent (100 nm
from the grain boundary) to either side of grain
boundary beta phase (Figure 6(e)), although the fact
that the grain boundary may not perfectly edge-on could
obscure detection of any very small depression in Mg
concentration adjacent to the b phase. With continued
aging, for example, 240 hours at 448 K (175 C), again
no depleted region of Mg in the matrix adjacent to the
grain boundary b phase could be observed, as reported
in an earlier study,[9] while the sample becomes highly
susceptible to SCC (Figure 1(a)). Although these obser-
vations suggest that the susceptibility to SCC is not
associated with a significant depletion of Mg in the
matrix region close to the grain boundary b phase, very
small depletions may have gone undetected by the
techniques employed here.
Although the b phase forms readily on grain bound-
aries with 1 hour of aging at 448 K (175 C), the
formation of this phase was observed to occur atop
pre-existing Al-Mn-Cr type particles after 25 hours of
aging treatment. Figure 7(a) is a bright-field micrograph
showing the formation of the b phase on a facet of an
Al-Mn-Cr containing particle. The corresponding dark-
field image obtained using a b reflection is shown in
Figure 7(b). With further aging, more of the b phase
nucleates and grows, with an elongated (plate- or
rodlike) morphology (Figure 7(c)). At 240 hours, the
length of the b rods or plates varies from 100 to 300 nm,
and most of these particles form in association with
Al-Mn-Cr containing particles.
VOLUME 42A, FEBRUARY 2011—351

Fig. 6—(a) Bright-field TEM image showing the b phase at the grain
boundary for sample aged for 10 h at 448 K (175 C). (b) A HA-
ADF image showing the grain boundary b phase (appeared dark).
(c) and (d) The distribution of Mg and Al from this region, respec-
tively. (e) The EDS line across the grain boundary b phase obtained
from the region (thick arrow), as shown in ‘‘b.’’ The grain boundary
position is shown by the dashed line.
In order to gain further insight into the mechanism of
the coverage of b phase on the grain boundaries, a
number of grain boundaries from samples that were
aged for different times at 448 K (175 C) will now be
considered in more detail. Figures 8(a) through (f) show
the b phase on a grain boundary tilted through a large
angular range (±42 deg), for the sample aged for
50 hours. It is evident that the b phase grew in the
form of a ‘‘ribbon’’ morphology, and multiple nucle-
ation events occurred along the grain boundary.
Although at certain tilts it can appear that the grain
boundary is essentially fully covered by b (e.g.,
Figure 8(d)), when viewed under a wide range of tilts,
it becomes evident that the grain boundary plane is not
fully covered by the b phase at this stage, as empty
spaces (no b phase) between the ribbons were observed
(Figures 8(a), (b), (e), and (f)). Figures 9(a) through (d)
352—VOLUME 42A, FEBRUARY 2011
Fig. 7—(a) Bright-field TEM image showing the b-phase formation
on the Al-Mn-Cr type particle for samples aged for 25 h. (b) The
dark-field image showing the b phase. (c) An elongated b phase
formed on Al-Mn-Cr type particle for sample aged for 240 h.
show the evolution of the grain boundary b phase as a
function of aging time. A number of the grain bound-
aries observed over a wide range of tilt conditions were
observed to be fully covered by the b phase for the
sample aged for ‡240 hours. Also, as the matrix
supersaturation decreases with aging, the continued
growth of the grain boundary b phase was found to
decrease to a considerable extent beyond 240 hours of
aging. At 1000 hours of aging, for instance, the thick-
ness of the grain boundary b phase ranges from 50 to
200 nm, which is similar to what was observed around
240 hours of aging. Figures 10(a) and (b) show a typical
grain boundary and a triple point, respectively, after
1000 hours of aging.
To study the dissolution behavior of the b phase, the
TEM samples were immersed into a brine solution
containing 5 pct NaCl at room temperature, and TEM
observations were carried out after immersing the
sample for 120, 180, and 300 seconds. It was observed
that grain boundaries were completely eaten away
for samples where the grain boundary b phase was
continuous. For example, the TEM micrographs in
Figures 11(a) and (b), which show typical images of
grain boundaries after 120 seconds of immersion for
sample aged at 448 K (175 C) for 240 hours, indicate
that the b phase has been dissolved from the grain
boundaries by the salt water. The Al-Mn based parti-
cles, which are not anodic with respect to matrix, are still
present at the boundaries. For grain boundaries where
the b phase has not formed continuously, the dissolution
was observed to be partial. More grain boundaries were
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 8—(a) through (f) Bright-field TEM images showing the grain boundary containing the b phase at different tilt conditions for sample aged
for 50 h.
observed to be dissolved away as the exposure time was
increased. With a long exposure (of almost a week) in
5 pct salt water, the dissolution of the b phase was
observed at the grain boundaries as well as within the
grains. Figures 11(c) and (d) are typical SEM images of
a specimen that was aged for 240 hours, before and after
the exposure to salt water for a week, respectively,
showing the dissolution at the grain boundary and
within the grains. Fine probe EDS from the grain
boundary region, which was dissolved away, in
Figure 11(a) showed the presence of a thin layer of Al
oxide with a small amount of Cl. No amount of Na was
detected from this region. These observations indicate
that the SCC behavior of sensitized Al-5083 in salt water
is mostly governed by the dissolution of the b phase
formed continuously at the grain boundaries with long
aging time (‡100 hours at 448 K (175 C)). This is also
corroborated by the observation of predominantly
intergranular fracture (Figure 1(b)) of the 240-hour aged
samples. At lower aging time (£100 hours at 448 K
(175 C)), as the b phase is not continuous along the
grain boundaries, the dissolution along the grain bound-
aries was incomplete in the immersion experiments. It
might thus be expected that in SCC experiments, the
crack growth rate would be lower, and a higher applied
METALLURGICAL AND MATERIALS TRANSACTIONS A
stress would be required to break the grain boundary
regions between the b-phase ribbons, for the lower aging
times, compared to specimens aged for 240 hours. This is
consistent with the fact that the crack velocity has been
observed to increase linearly with aging time.[3] Specif-
ically, Jones et al.[3] observed that the crack growth rate
increased from 5 9 10 11 ms 1 for no aging to 5 9
10 10 ms 1 for 100 hours of aging at 448 K (175 C),
and the present observations showed a further increase
of the crack velocity to 5 9 10 9 ms 1 for 240 hours of
aging at 448 K (175 C) (Figure 1(a)).
To study the defects close to the fracture surface as a
result of deformation, cylinders 3 mm in diameter were
cored out from different locations of the fracture surface
of the 240-hour annealed specimens. Dislocation net-
works were observed within the grains (Figure 12(a)) as
a result of interaction of the dislocation forests, glide
dislocations, and dislocation climb.[15] Glide disloca-
tions are pushed by the applied shear stress against the
dislocation forests. In addition, dislocation pileups were
observed at grain boundaries (Figure 12(b)) as a result
of deformation, that produce high stress regions on the
grain boundary b phase. Such dislocation pileups can
significantly contribute to SCC when grain boundaries
in Al-5083 are not fully covered by the b phase.
VOLUME 42A, FEBRUARY 2011—353
Fig. 9—(a) through (d) Bright-field TEM images showing the b phase at the grain boundary for samples aged for 10, 25, 240, and 1000 h.
Fig. 10—(a) Bright-field TEM image showing the b phase at the
grain boundary close to edge-on condition for sample aged for
1000 h. (b) A bright-field image showing a triple point after 1000 h
of aging.
IV. SUMMARY
TEM was employed to investigate the microstruc-
tural evolution in Al-5083, by analyzing a number of
specimens subjected to various aging times, including
354—VOLUME 42A, FEBRUARY 2011
Fig. 11—(a) and (b) Bright-field TEM images showing the dissolu-
tion of b phase at the grain boundaries after 120 s exposure to salt
water. (c) A SEM image showing the b phase at the grain boundary
as well as on existing Al-Mn type particles within the grain after
240 h of aging at 448 K (175 C). (d) An SEM image showing the
dissolution of b phase at the grain boundary and within the grain
after a week of exposure to salt water.
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 12—(a) A weak-beam dark-field TEM image showing the dislo-
cation network structures for sample aged for 240 h. (b) Dislocations
pile up at the grain boundary for the sample aged for 240 h. The
sample was obtained close to the fracture surface.
as-received Al-5083 (H-131 temper) and as-received
specimens that were then aged at 448 K (175 C) for
1, 10, 25, 50, 100, 240, 500, and 1000 hours. A large
number of Mn-rich precipitates were observed in the Al
matrix of the as-received Al-5083, while significant
precipitation of the Mg-rich b phase from the Mg-
supersaturated Al matrix was observed in samples
subsequently annealed. This b phase formed both at
the aluminum grain boundaries and on pre-existing Mn-
rich particles in the matrix, due to the relatively low
driving force for precipitation necessitating these heter-
ogeneous nucleation sites. For aging times up to 1 hour,
TEM observations showed that the initial grain bound-
ary b phase grew as what appeared to be isolated
allotriomorphs, which then evolved into a ribbonlike
morphology. Significant empty (no b phase) regions
were observed between the b ribbons along the Al grain
boundaries, even for aging times up to 100 hours.
METALLURGICAL AND MATERIALS TRANSACTIONS A
To study the dissolution behavior of the b phase, the
TEM samples were immersed into salt water containing
5 pct NaCl at room temperature for short durations of,
120, 180, and 300 seconds, and subsequent TEM obser-
vations indicated that the grain boundaries were com-
pletely dissolved away in samples where the grain
boundary b phase was continuous along the grain
boundaries, whereas for shorter aging times where the b
phase was discontinuous, the grain boundaries were
only partially dissolved. It is thus suggested that the
SCC behavior of sensitized Al-5083 in salt water is
mostly governed by the dissolution of the b phase
formed continuously at the grain boundaries due to long
aging times (>100 hours at 448 K (175 C)). At shorter
aging times (£100 hours at 448 K (175 C)), the b phase
is not continuous along the grain boundaries, and higher
applied stress is likely required to break the grain
boundary regions between the b-phase ribbons, as
corroborated by the observation of increasing SCC
crack growth rates with increasing aging times.
ACKNOWLEDGMENTS
The authors gratefully acknowledge that the speci-
men material and preliminary SCC characterization
were provided by Dr. F. Bovard, ALCOA. This work
was funded by the Office of Naval Research.
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