Scripta Materialia 48 (2003) 1451–1455

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Fine-grain evolution in friction-stir processed 7050 aluminum

C.G. Rhodes *, M.W. Mahoney, W.H. Bingel, M. Calabrese
Rockwell Scientific Company, Thousand Oaks, CA 91360, USA
Received 25 October 2002; received in revised form 13 February 2003; accepted 13 February 2003

Abstract
Evolution of the fine-grained structure in friction-stir processed aluminum has been studied using a rotating-tool
plunge and extract technique. Initial sizes of newly recrystallized grains are on the order of 25–100 nm. These grains
then grow to a size equivalent to that found in friction-stir processed aluminum, 2–5 lm, after heating 1–4 min at 350–
450 °C.
Ó 2003 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.

Keywords: Friction stir processing; Aluminum alloys; Transmission electron microscopy; Recrystallization

1. Introduction Because the production of a fine-grained struc-

Friction stir welding is now established as a
viable method for joining aluminum alloys [1–5].
Basically, the technique involves plunging a ro-
tating tool into abutted edges of sheet or plate to
be welded and then translating the tool along the
seam to complete the solid-state joining process.
Details are available in the literature [1,2].
The dynamically recrystallized zone (DRZ), or
nugget, of friction-stir welded aluminum alloys
consists of fine (2–5 lm) equiaxed grains [6–8]. The
fine-grain characteristic of the process leads to the
concept of producing a controlled microstructure
on the surface of an aluminum plate by multi-pass,
overlapping zones. This approach has been desig-
nated friction stir processing [9].
ture is significant in terms of mechanical properties,
understanding the evolution of this structure is of
interest. Others have theorized that the resultant
fine grains are developed during the stirring oper-
ation by rotation of existing sub-grains or sub-
grains developed during processing (via dislocation
absorption into sub-boundaries) within the parent
microstructure [7,8]. Sato et al., on the other hand,
have proposed that the fine grains arise from re-
crystallization within the stir zone [10].
The objective of the present study was to ex-
amine in detail the evolution of the fine grains
found in friction-stir processed 7050Al. The results
indicate that the fine grains are initiated by re-
crystallization and not by sub-grain formation.

* 2. Experimental procedure
Corresponding author. Address: Rockwell Scientific Com-
pany, Structural Metals, P.O. Box 1085, Thousand Oaks, CA
91358, USA. Tel.: +1-8053734233; fax: +1-8053734268. A set of experiments was designed to attempt
E-mail address: crhodes@rwsc.com (C.G. Rhodes). a simulation of the conditions that initially exist

1359-6462/03/$ - see front matter Ó 2003 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.
doi:10.1016/S1359-6462(03)00082-4
1452 C.G. Rhodes et al. / Scripta Materialia 48 (2003) 1451–1455
within the DRZ (nugget) of a friction-stir weld.
These experiments involved plunging the rotating
tool into the aluminum sheet as if a weld bead were
to be produced, but instead of moving the work-
piece under the tool, the tool was immediately
retracted. Although not an exact simulation of
FSW, this procedure has left material at the bot-
tom of the hole severely deformed, both in shear
and compression, by the rotating tool.
The material was 1.0 mm gauge 7050Al sheet in
the T76 condition. The holes were plunged to a
depth of approximately 0.9 mm, leaving approxi-
mately 0.125 mm of deformed material at the
bottoms of the holes. The 1.25 mm diameter tool
was rotated at speeds of 200, 300, or 500 rpm.
To freeze in the initial microstructures, a mix-
ture of dry ice and isopropyl alcohol was flooded
onto the upper surface of the plate prior to, and
during, the plunge. In all plunges, the anvil on the
under side of the aluminum plate was cooled with
a chilled mixture of ethylene glycol and alcohol.
The plunges were completed in 1 s or less.
Post-processing heat treatments were conducted
in salt baths. The times required for the sheet
samples to reach temperature were measured using
thermocouples that simulated the sheet material.
Samples were water quenched from the salt bath.
Transmission electron microscopy (TEM)
samples were extracted from the bottoms of the
holes. This was accomplished by first grinding off
the top portion of the plate, leaving the bottom
0.125 mm. A 3 mm disc, centered over the bottom
of the plunged hole, was electro-discharge ma-
chined from the 0.125 mm plate. The disc was
mechanically ground from the bottom side to a
thickness of approximately 0.025 mm and then
electrolytically polished to electron transparency.
The foils were examined in a Philips CM30 scan-
ning/transmission electron microscope.
3. Results
TEM was used to examine the bottoms of the
plunged holes for grain structure. The results are
presented here as the effect of tool rotation speed
on the microstructure.
3.1. Effect of tool rotation speed
The sample from the 200 rpm tool rotation
speed test shows highly deformed material with
virtually no recrystallization, Fig. 1a. The single-
orientation deformed regions, such as that shown
in Fig. 1a, appear to be original grains in the Al
sheet. There are rare regions where there appear to
be isolated recrystallized grains on the order of 50
nm.
The 300-rpm-tool-rotation-speed test sample
shows many recrystallized grains within some re-
tained deformation, Fig. 1b. These recrystallized
grains are on the order of 25–40 nm. The increase
in tool speed from 200 to 300 rpm has resulted in
increased deformation as well as increased fric-
tional and deformation heating to the extent that
recrystallization has occurred.
Increasing the tool rotation speed to 500 rpm
produces a microstructure consisting of mostly
recrystallized grains with little retained deforma-
tion, Fig. 1c. The grains are on the order of 100 nm
with occasional ones up to 300 nm. The effect of
tool rotation speed on grain size is consistent with
earlier reports, i.e., as the tool rotation speed is
reduced, the final grain size is reduced [10].
3.2. Details of FSP region
Evidence shows that the extremely fine grains
(50–100 nm) present in the FSP material at the
bottom of plunged holes are not sub-grains, but
rather are grains separated by high-angle bound-
aries. This evidence is in the form of electron dif-
fraction patterns taken from various areas in the
microstructure.
Those deformed areas that show no indication
of recrystallized grains give electron diffraction
patterns indicative of the underlying parent grain,
Fig. 2. The diffraction pattern, which is a selected-
area pattern taken from the entire area inset in Fig.
2, reveals that this area is a single crystallographic
orientation. This area would be included in a sin-
gle parent grain.
In contrast to the deformed regions, electron
diffraction patterns from those areas with recrys-
tallized grains show multi-orientations from se-
lected areas comparable in size to those from the
 C.G. Rhodes et al. / Scripta Materialia 48 (2003) 1451–1455 1453

Fig. 1. TEM micrographs of FSP Ôplunge and extractÕ tested 7050Al, isopropyl alcohol/dry ice cooling. (a) 200 rpm tool rotation speed,
(b) 300 rpm rotation speed, and (c) 500 rpm rotation speed. Arrows indicate recrystallized grains in contrast.

deformed regions, Fig. 3. There are two major
grains contributing to the pattern, both near [1 1 0]
zone normal, but rotated 65° from each other
with (2 0 0) planes in one grain parallel to one of
the (1 1 1) planes in the other. Furthermore, there
are 4 other grains contributing to the pattern in
non-low index orientations. These conditions in-
dicate that the newly recrystallized grains are not
sub-grains.
3.3. Heating experiments
Stability of the very fine grains generated in the
Ôplunge and extractÕ tests has been observed by
means of heating experiments. Several Ôplunge and
extractÕ holes were made in the 7050Al sheet using
a tool speed of 300 rpm. This gives a starting
structure with some retained deformation and
many recrystallized grains on the order of 25–40
nm, see Fig. 1b.
Samples heated at 350, 400, and 450 °C reveal
grain growth, Fig. 4. After 1-min exposures, the
grain sizes are roughly 0.4 lm at 350 °C, 0.7 lm at
400 °C, and 5 lm at 450 °C. Continued aging
demonstrates the grain growth behavior of the
FSP condition. For instance, after 2 min at 350
and 400 °C, the grains have grown to 0.6 and 3.5
lm, respectively, and after 4 min at the same
temperatures, they have grown to 0.7 and 4.5 lm,
respectively, Fig. 4.
1454 C.G. Rhodes et al. / Scripta Materialia 48 (2003) 1451–1455
Fig. 2. FSP Ôplunge and extractÕ tested 7050Al, selected-area
electron diffraction pattern shows single orientation from inset
TEM image of deformed region.
Fig. 3. FSP Ôplunge and extractÕ tested 7050Al, TEM image
(inset) of recrystallized region showing a few grains in contrast;
electron diffraction pattern shows multiple orientations.
4. Discussion
It is assumed that the deformed material at the
bottom of a hole created by a plunged and ex-
tracted rotating tool is similar to the deformed
material in the nugget region of a plunged and
Fig. 4. Grain growth behavior in FSP 7050Al at 350, 400, and
450 °C.
translated rotating tool. However, there are sig-
nificant differences. These differences are twofold:
first, the amount of deformation in the nugget of a
weld will be greater as the material is carried
around the rotating tool, and second, the tem-
perature rise is greater in the nugget. Thus, the
deformed material at the bottom of a hole created
by a plunged and extracted rotating tool might be
considered an early ‘‘snapshot’’ of the deformation
experienced in the nugget at an instant in time
prior to the complete temperature and deforma-
tion cycle. Such speculation is based on the fact
that the material in the nugget of a FSW under-
goes more deformation as it is dragged around the
rotating tool than that at the bottom of a plunged
hole. Furthermore, although Sato et al. [10] sug-
gest that the onset of deformation in a FSW occurs
at a temperature near 200 °C, this temperature
remains well below the recrystallization tempera-
ture for the aluminum alloy. Hence, it is speculated
that the deformation observed at the bottom of a
plunged hole is a precursor to the severe defor-
mation experienced within a FSW nugget.
The extensive deformation shown in Fig. 1a
demonstrates that the fine-grain evolution starts
with severe deformation of the parent material,
including pre-existing sub-grains. With a temper-
ature increase, either by increasing the tool rota-
tion speed or reducing the cooling rate, the
deformed structure recrystallizes by nucleation
and growth, as shown in Fig. 1.
 C.G. Rhodes et al. / Scripta Materialia 48 (2003) 1451–1455
The initial grains are on the order of 25–50 nm,
which is significantly smaller than the size of the
pre-existing sub-grains, typically 1–2 lm [7,8]. It
does not follow, then, that the 2–5 lm grains
found in the nugget regions of FSP aluminum have
arisen from pre-existing sub-grains that have ro-
tated during processing [7] or from rotated sub-
grains that form during processing [8]. Rather, the
observations reported here are consistent with the
proposal of Sato et al. [10] that newly recrystal-
lized grains form during the stirring process.
Subsequent heating of the deformed regions of
the plunge and extract material indicates that the
nugget time/temperature exposure of a FSW during
processing falls within the 400–450 °C range. For
instance, 1 min at 450 °C or 4 min at 400 °C gen-
erates a grain size of 2–5 lm, equivalent to that
found in a FSW nugget. This is consistent with
previous postulates of nugget temperatures [4,6,11]
and agrees with measurements [10]. Times above
temperatures within the nugget of a FSW, however,
are more difficult to determine. For instance, Sato
et al. [10] measured the bottoms of weld nuggets to
be above 400 °C for only a few seconds. Lumsden
et al. [12], on the other hand, reported time above
400 °C to be on the order of 15 s in the heat affected
zone. It is likely that the core of the FSW nugget
will be at a higher temperature for longer times than
what was measured at the bottom of the weld joint
or in the heat affected zone. Furthermore, the in-
creased deformation within the FSW nugget
(compared to the bottom of the plunge and extract
hole) will lower the recrystallization temperature
and increase the subsequent grain growth rate.
5. Summary and conclusions
The evolution of the fine-grained structure in
friction-stir processed aluminum has been studied
using a rotating-tool plunge and extract technique.
In these experiments, the rotating tool has intro-
duced severe deformation in the starting grain
structure, including severe deformation of the pre-
existing sub-grains. Extreme surface cooling was
used to freeze in this starting structure.
Heat generated by the rotating tool is a function
of the rotation speed and the external cooling rate.
1455
At slower cooling rates and/or faster tool rotation
speeds, recrystallization of the deformed alumi-
num occurs. The initial sizes of the newly recrys-
tallized grains are on the order of 25–100 nm,
considerably smaller than the pre-existing sub-
grains in the starting condition.
Subsequent experiments reveal that the newly
recrystallized grains grow to a size equivalent to
that found in friction-stir processed aluminum, 2–
5 lm, after heating 1–4 min at 350–450 °C.
It is postulated that the 2–5 lm grains found in
friction-stir welded and friction-stir processed
aluminum alloys arise as the result of nucleation
and growth within a heavily deformed structure
and not from the rotation of pre-existing sub-
grains.
Acknowledgements
This work was funded by DARPA under ONR
contract no. N00014-00-C-0520.
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