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Acta Materialia 61 (2013) 5278–5289

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Strength and biaxial formability of cryo-rolled 2024 aluminium

subject to concurrent recovery and precipitation
M. Weiss ⇑, A.S. Taylor, P.D. Hodgson, N. Stanford
Institute for Frontier Materials, Deakin University, Geelong, VIC 3217, Australia

Received 20 March 2013; received in revised form 17 May 2013; accepted 17 May 2013
Available online 20 June 2013

Abstract

The precipitate-hardenable aluminium alloy 2024 has been processed by rolling to develop a fine microstructure. Four alloy condi-
tions were tested; these included two rolling temperatures and two different ageing sequences. For all four conditions there was an ideal
heat-treatment time at which there was a concurrent improvement in both strength and formability. Microstructural modeling has shown
that this is the result of a small processing window in which the hardening due to precipitation is larger than the softening due to recov-
ery, while the detrimental effects of particle coarsening on ductility have not yet developed. Cryo-rolling and room-temperature rolling
produced materials with similar strengths, but cryo-rolling showed inferior formability. Natural ageing before rolling significantly
decreased the formability compared to rolling in the supersaturated condition, and it is proposed that the solute clusters that develop
during natural aging inhibit dynamic recovery and consequently increase the dislocation density that develops during rolling.
Ó 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Aluminium; Cluster hardening; Precipitation; Fine grained; Formability

1. Introduction elongation in tension, cryo-rolled aluminium shows excep-

There has been interest in recent literature on the
mechanical properties of heavily deformed metals and
alloys. There are many processing routes by which these
heavily deformed structures can be produced, and exam-
ples include cryo-rolling [1,2], equal-channel angle pressing
(ECAP) [3,4] and high-pressure torsion (HPT) [5,6]. After
being deformed to high strains, systems such as steel and
aluminium develop an extremely fine grain (or subgrain)
size and a commensurate high dislocation density. These
factors provide the material with a significant increase in
yield and tensile strengths [7,8] compared to the starting
material. The trade-off for the much improved strength is
a decrease in the uniform and total elongation [9,10],
parameters typically measured in tension. However, it has
recently been shown that despite having very poor uniform
⇑ Corresponding author. Tel.: +61 3 5227 1304; fax: +61 3 5227 1103.
E-mail address: matthias.weiss@deakin.edu.au (M. Weiss).
tionally good formability in biaxial stretching [11]. In that
case, the pure aluminium showed a very large reduction in
area, and this ability to achieve high local strains was
found to provide good formability under biaxial and
plane-strain deformation. The drawback of using pure alu-
minium is that it has low strength, hence in the present
paper we examine a common precipitate-hardenable alu-
minium alloy, 2024. The method chosen to refine the
microstructure is cryo-rolling. The advantage of rolling
over other processes such as ECAP and HPT is that the
size of sheet produced is quite large and lends itself to many
formability testing techniques. Thus we can here study the
formability of this alloy system in biaxial stretching, some-
thing that has not before been reported.
The 2024 alloy system is a precipitate-hardenable sys-
tem, and we make particular note here that from the solu-
tion-treated and quenched condition, this alloy system
undergoes significant changes at room temperature. During
natural ageing the Cu and Mg solutes form into clusters or

1359-6454/$36.00 Ó 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.actamat.2013.05.019
 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289
Guinier–Preston (GP) zones [12]. These are not discrete
precipitates and cannot be viewed by transmission electron
microscopy, but account for some 60–80% of the precipi-
tate hardening measured in this alloy system [13,14].
Upon continued heat treatment, these clusters develop
into the equilibrium S phase [12–14]. We note here that
the developmental process of the S phase, and the possible
development of intermediate phases such as S’ [15–17],
remains a topic of considerable debate in the literature. It
is not our aim to contribute to the debate on the precipita-
tion sequence, but simply to summarize for the reader the
general notion that from the solid solution, this alloy devel-
ops a mixture of solute clusters, GP zones and then finally
equilibrium S-phase precipitates.
This alloy, therefore, presents us with an interesting sys-
tem that allows us to examine the effect of these clusters
and precipitates on the behaviour of fine-grained materials.
Although the cryo-rolling of 2024 aluminium has been
reported before [18,19], we choose here to control the tim-
ing of the cluster formation in order to trace its effect on
the behaviour of the alloy. Of particular interest is the effect
of these solute clusters on the development of the deformed
microstructure: will they have an effect on the cryo-rolled
material? If we suppress their development throughout
cryo-rolling, can we improve the age-hardening response?
Does the natural ageing have any effect on the rolled struc-
ture? It is clear that in a heavily rolled material, any heat
treatment could potentially soften the material through
recovery or recrystallization, but how will that affect the
precipitation? In order to investigate these parameters we
use a wide range of characterization techniques to describe
the microstructural development, and these are linked with
the deformation behaviour which we examine under two
different strain paths.
2. Experimental method
2.1. Material and thermomechanical processing procedure
The Al 2024 alloy with the chemical composition shown
in Table 1 was supplied in sheet form with an initial thick-
ness of 6.4 mm.
The as-received sheet was machined into
150 mm  150 mm plates. The alloy was solution treated
(ST) at 500 °C for 12 h followed by an immediate cold
water quench (CWQ). One group of samples was immedi-
ately rolled after the water quench, while a second group of
samples was allowed to age naturally at room temperature
for 1 week. For each of these two groups, the aged and not
Table 1
Composition (wt.%) of the material used in this study, measured by atomic emission spectroscopy. Composition range of commercial alloys designated as
2024 are also shown for comparison [20].
Cu Mg Mn
Commercial composition range 3.8–4.9 1.2–1.8 0.3–0.9
Measured composition 4.22 1.16 0.65
5279
aged groups, rolling was carried out at two temperatures,
room temperature and liquid nitrogen temperature (cryo-
rolling). Thus there were in total four alloy conditions
tested, and these are shown schematically in Fig. 1.
The rolling itself was conducted on a two-high labora-
tory mill with a roll diameter of 365 mm and a roll speed
of 15 rev min1. The rolling schedule reduced the initial
thickness by 80%, corresponding to a true strain of 1.6,
and this was completed in 28 passes (see Table 2). The roll-
ing schedule was identical for the two rolling temperatures.
Before cryo-rolling commenced samples were submerged in
liquid nitrogen until they stopped bubbling and this was
repeated between each pass.
Following the rolling process all samples were allowed
to age naturally for a period of at least 1 week. Following
this, the naturally aged samples were heat treated at 150 °C
for varying times.
2.2. Mechanical testing
Tensile tests were carried out on an Instron tensile test
frame equipped with a 30 kN load cell. The strain was mea-
sured using a non-contact extensometer. All samples were
deformed at an initial strain rate of 0.001 s1 at room
temperature. The samples had a gauge section of
60 mm  12.5 mm and the tensile direction was parallel to
the rolling direction of the sheet.
2.3. Microscopy
Samples for microstructural characterization were cold
mounted in two-part epoxy resin and then prepared using
standard metallographic techniques, finishing with a final
polish with colloidal silica. Backscattered images of the
microstructures were obtained using a Zeiss Supra 55 var-
iable-pressure FEG-SEM equipped with an angular selec-
tive backscattered (AsB) detector at 20 kV in high-current
mode. Selected specimens were examined by transmission
electron microscopy (TEM) with a JEOL 2100F field emis-
sion gun microscope. Foils were prepared by ion milling in
a Gatan PIPS.
2.4. X-ray diffraction
For X-ray diffraction (XRD) analysis samples approxi-
mately 20 mm  20 mm were mounted and polished for
examination in the rolling plane. XRD was carried out
on a Panalytical X’pert Pro with Cu Ka radiation. Only
the (1 1 3) plane, corresponding to a peak at 78° (2h),
Fe Si Zn Ti Cr Al
0.5 max. 0.5 max. 0.25 max. 0.15 max. 0.1 max. bal.
0.23 0.10 0.10 0.02 <0.01 bal.
5280 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289

coarse-grained condition with no internal stress. Thus,

tracking the change in peak width as a function of heat-
treatment time provides an indication of the recovery rate.
We consider the peak width of the solution-treated mate-
rial to be 100% recovered, and the peak width after rolling
to be a condition in which there is 0% recovery.

2.5. Formability testing

Erichsen cupping tests were performed in accordance

with ISO 20482 [21] to investigate the stretch formability
of the different material conditions. The tool set-up is
shown in Fig. 2. Square samples 70 mm  70 mm were
cut from each sheet and care was taken to align one sample
edge to the rolling direction. Using a screenprinting system
a 1 mm square grid was painted onto the samples to enable
the analysis of surface strains after testing and a thin film of
graphite grease was applied on both sides of the test piece
and the punch for lubrication. The samples were placed
between the blank-holder and the die (Fig. 2) and clamped
with a blank-holder force of 10 kN.
During the test the punch was moved upwards with a
Fig. 1. Schematic of the thermomechanical processing conditions used in speed of 5 mm min1 until rupture occurred; the initiation
the current investigation. RTR = room-temperature rolled. of rupture was determined by eye. To determine the posi-
tion of first contact between the punch and the sheet,
pre-tests were performed where the punch was moved
Table 2
Details of the rolling schedule used. upwards at low speed to the displacement measured where
the first change in punch load occurred. Using this method
Reduction Number Ave. strain
per pass (mm) of passes per pass the punch displacement at contact was found to be 0.9 mm
and in this study the indentation depth, IE, is defined as:
Step 1 0.5 1 0.08
Step 2 0.4 1 0.07 IE ¼ DR  0:9 mm; ð1Þ
Step 3 0.3 4 0.06
Step 4 0.2 6 0.05 where DR is the displacement at rupture.
Step 5 0.15 4 0.05 After testing, the major and minor surface strains were
Step 6 0.1 12 0.05 determined using the optical strain measurement system
Total 5.1 28 1.6
Autogrid Vario. To exclude the effect of the crack in the
surface strain measurements the “borderline” tool was used
which allows the areas on both sides of the crack to be han-
was measured. This peak was chosen because it showed a dled separately during strain calculation; this leads to a sig-
relatively high intensity and being at a high 2h angle gave nificant reduction in scatter [22]. The forming limit strains
good angular resolution and peak width data. The mea- were measured next to the crack area.
surements were made with a step size of 0.002° and 2.5 s All four material conditions were tested using the
per step, and provided excellent peak shape data. XRD Erichsen cup test, and we report both the IE value and
was carried out on only one series of alloy, those that were the forming limit strains. For each alloy condition, three
naturally aged after solution treatment, and then rolled at heat-treatment times were tested: 0.1, 8 and 30 h.
room temperature. Two additional specimens were tested
using XRD, a solution-treated specimen, and a specimen 3. Results
that was heat treated for 1000 h to develop an over-aged
microstructure. 3.1. Rolling behaviour
The XRD measurements were made in order to track
both the rate of static recovery resulting from heat treat- After solution treatment, samples were rolled in two dif-
ment, and also the rate of precipitation. During rolling, ferent conditions: naturally aged, or not aged (see Fig. 1).
the XRD peaks are broadened due to two effects, the devel- These two conditions behaved quite differently during roll-
opment of fine subgrains and also the development of inter- ing (Fig. 3). The samples that were not aged prior to rolling
nal strain (often referred to as residual stress) due to plastic showed good rollability and did not exhibit edge cracking.
deformation. Both of these effects are alleviated during sta- However, the samples that were naturally aged before roll-
tic recovery as the microstructure returns to a low-energy, ing showed quite extensive edge cracking.
 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289
Fig. 2. Tool set up for Erichsen cupping test.
3.2. Microstructural development
The 2024 alloy composition contains two populations of
particles. The coarse, Mn-enriched phase known as T
phase [23] was present after solution treatment, and
remained unaltered throughout rolling, ageing and heat
treatment (Fig. 4). This phase was clearly visible in the
scanning electron microscope due to atomic number con-
trast, and was also clear in the transmission electron micro-
scope in conventional bright-field imaging (Fig. 5). This
stable phase does not change significantly throughout ther-
momechanical processing and is not considered to be an
important hardening phase [23]. However, the second par-
ticle species, known as the S phase, is of great interest here,
as it is responsible for the cluster hardening and precipitate
hardening that develops in this alloy [12–17]. The S phase
Fig. 3. Photograph of edge of aged and not aged samples. The aged
sample (left) showed significant edge cracking.
5281
was quite difficult to image in the present case. The phase
is too fine to be visible by SEM, and TEM of the heavily
dislocated structure made its appearance in conventional
bright-field imaging difficult (Fig. 5b). The S phase could,
however, be identified chemically through high-angle annu-
lar dark-field imaging and energy-dispersive spectroscopy.
The chemical analysis with EDS can discriminate between
the S and T phases depending on which elements show
enrichment in the particle [23]. The T phase shows Mn
and Cu enrichment, while the S phase is enriched in Cu
and Mg. Using this as an identification tool, it was deter-
mined that the S phase particles did not develop until
30 h of heat treatment (Fig. 5c and d).
3.3. X-ray diffraction
The XRD experiments were only performed on one ser-
ies of samples, those subject to room temperature rolling
after being naturally aged at room temperature. Typical
examples of the peak shape obtained from the XRD are
shown in Fig. 6. It can be seen that the as-rolled sample
had a broad peak, and that increasing the heat-treatment
time narrowed this peak (also shown in Fig. 7a) and caused
peak shifting. The peak width data has been converted to a
percentage recovery (as described in the Materials and
methods section) and is shown in Fig. 7b. It can be seen
that after only 0.1 h of heat treatment the microstructure
has already begun to recover, and that considerable recov-
ery (nearly 40%) has taken place after 30 h.
3.4. Tensile behaviour
Examples of the flow curves obtained for the different
specimens are given in Fig. 8. All flow curves show a very
5282 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289

Fig. 4. AsB images showing how the population of the T phase remains unchanged with increasing annealing time.

Fig. 5. Transmission electron microscopy showing (a) the T phase in low-magnification bright-field imaging. A higher-magnification image of the heavily
dislocated structure is shown in (b). EDS mapping of the T phase in a sample aged for 8 h is shown in (c). EDS mapping of the S phase in a sample aged for
30 h is shown in (d).

similar shape, having minimal work hardening after yield-
ing, and all having relatively low elongations. This is in
contrast to the tensile behaviour of the starting material
which shows consistent work hardening throughout defor-
mation, and achieves a good elongation at failure (Fig. 9).
The sample of starting material that was tested in the solu-
tion treated (ST) condition (with no natural ageing)
showed significant flow serrations associated with dynamic
strain ageing effects [24,25]. It is clear that the heavy rolling
reductions have considerably increased the strength of the
materials compared to the starting conditions.
The effects of heat-treatment time on the yield strength
and total elongation for all samples are summarized in
Fig. 10. All of the rolled materials maintain their high yield
strengths up to a holding time of 8 h, and in this time frame
there is also evidence of precipitate hardening in some
cases. Above heat-treatment times of 8 h there is a sharp
drop in yield strength with further heat treatment. For both
 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289
Fig. 6. Example of the XRD scan data obtained for the RTR samples that
were aged prior to rolling.
Fig. 7. Peak width data for all of the XRD experiments (FWHM, full
width half maximum). The peak width data has been converted into the
percentage of recovery; see Section 2.3 for further details.
5283
rolling temperatures, ageing the samples before rolling
resulted in an increase in the yield strength.
The total elongations measured on the samples also
showed significant changes as a function of the heat-treat-
ment time. All four test conditions showed a rise in elonga-
tion after small heat-treatment times, but after longer
holding times the elongation showed a significant drop to
a value lower than the as-rolled state. Those samples that
were aged before rolling showed lower elongations, and
this is consistent with the yield strength observations that
showed the aged samples to have higher yield stresses.
3.5. Formability characteristics
Examples of the Erichsen dome tests results are shown
in Fig. 11, where the position of the crack is also indicated.
All materials showed sudden and brittle failure without the
formation of a distinct neck during the dome tests. While
for small dome heights the crack is positioned at the top
of the dome, for large indentation depths cracking appears
at some distance from the dome centre. The surface strains
were used to measure the major and minor strains at fail-
ure, while the indentation depth, IE, was measured from
the punch displacement (see Eq. (1)).
Looking firstly at the IE results, it can be seen in Fig. 12
that the indentation depth increased for small heat-treat-
ment times, peaking at 8 h for all samples. The highest
formability is achieved for the non-aged RTR condition
with an indentation depth of 3.2 mm; this is between 35
and 50% higher compared to the remaining material
grades. With further heat treatment the indentation depth
drops significantly for all four test conditions. The aged
RTR and the aged cryo-rolled samples showed the lowest
formability with indentation depths of only 0.1 and
0.4 mm, respectively, after heat treating for 30 h. These
changes are well outside the material variability or testing
measurement error.
The forming limit strains were determined using the
optical strain measurement system and are summarized in
Fig. 13. For most tests, near-biaxial conditions were
achieved. It can be seen in Fig. 13 that for both rolling tem-
peratures, ageing the alloy before rolling led to a reduction
in the forming limit strains compared to the non-aged con-
dition. This corresponds to the lower indentation depths
observed for the aged material grades in Fig. 12.
4. Discussion
4.1. Effect of microstructural development on formability
The formability data showed two results of particular
interest. Firstly, it was observed that all four sample condi-
tions showed a peak in indentation depth after 8 h of heat
treatment (Fig. 12). Secondly, it was found that ageing the
sample before rolling reduced formability in biaxial
stretching. Both of these observations correlate well with
the tensile test data. For the case of tensile ductility, all four
5284 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289

Fig. 8. Flow curves for (a and b) cryo-rolled material naturally aged (a) and not aged (b), and (c and d) RTR material naturally aged (c) and not age (d).

Fig. 9. Flow curves for the starting material. (ST, solution treated; NA, naturally aged; CR, cryo-rolled; RTR, room-temperature rolled).

sample conditions show a maximum in the total elongation
(Fig. 10). Although the exact time corresponding to the
maximum of each condition cannot be precisely identified
from the limited heat-treatment times tested, it is obvious
that close to an ageing time of 8 h there is a peak in tensile
ductility for the four sample conditions. The maximum
ductility observed in tension therefore correlates well with
the maximum indentation depth determined in the
Erichsen test and through that with material formability
in biaxial stretching.
 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289 5285

Fig. 10. Summary of the mechanical test data for all samples. Yield strength is shown in (a) and (b), and the total elongation is shown in (c) and (d). Trend
lines shown to guide the eye. Note logarithmic time scale on the x-axis.

This is in contrast to previous work that showed for the
case of high-purity aluminum that cryo-rolled material
with extremely low total tensile elongation can experience
high formability in biaxial stretching [11]. This study
revealed that even though the total elongation in tension
was low after cryo-rolling, the strain that the material
was able to accommodate in localized deformation in the
neck was high. This was represented by a high reduction
in area measured in the necking region (>70%) and it
was suggested that this high ability to accommodate large
strains during necking in tension results in enhanced form-
ability in biaxial stretching [11].
In the current work the analysis of fractured tensile
specimens from cryo-rolled and room-temperature rolled
(RTR) 2024 aluminum showed that for all thermomechan-
ical processing conditions investigated there is only very lit-
tle reduction in area in the necking region (<14%). The
capability of the 2024 alloys to accommodate localized
deformation is therefore low. This leads to poor formabil-
ity in biaxial stretching if the total elongation in tension is
low.
With respect to the effect of ageing on the material
behavior in uniaxial tension, it was found that ageing the
samples before rolling increased the yield strength and
reduced ductility (Fig. 10). Ageing also had a profound
effect on the maximum forming strains reached under biax-
ial tension, with the aged samples showing significantly
lower forming limit strain values compared to those that
were not aged (Fig. 13). The effect of ageing on the material
forming limits in uniaxial tension is therefore consistent
5286 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289
Fig. 11. Dome shapes with surface strains overlaid for the material grades that showed the lowest and the highest values of IE: (a) side view indicating the
difference in dome height; (b) top view showing the different positions of the crack.
with that found for biaxial tension. For both strain paths—
uniaxial tension and biaxial stretching—ageing decreased
formability.
One of the most interesting observations made in the
tensile test was the small rise in yield strength at shorter
ageing times (Fig. 11). This in itself is not unexpected:
the alloy is age hardenable and one might anticipate such
a result. However, it was somewhat unexpected that the
ductility too was improved in this ageing window. The
simultaneous improvement in strength, ductility and form-
ability (after 8 h heat treatment) is quite unusual, although
for this particular alloy system a similar result has been
reported once before [19]. The origin of this behaviour
can be explained by the delicate balance between the con-
current processes of recovery and precipitation. While the
recovery acts to soften the microstructure and improve
ductility, the precipitate process acts to harden the alloy
and decrease ductility.
In order for there to be an increase in hardness and an
increase in ductility, the heat-treatment time of 8 h must
be ideally placed such that the precipitate hardening is lar-
ger than the drop in strength due to recovery. In order to
quantify this effect, we present here a simple strength model
based on the notion that the strength can be estimated by a
simple law-of-mixtures. The yield strength has a number of
contributing factors: the alloy’s intrinsic strength, the
strength provided by the solute clusters, the strength pro-
vided by the precipitates, and the hardening due to cold
work. The intrinsic strength can be measured by measuring
the strength in the solution-treated condition, and this was
found to be 120 MPa (see Fig. 9). The strength increase due
to the cluster hardening that develops during natural age-
ing at room temperature is also readily measured (see
Fig. 9, the solution-treated and naturally aged condition)
and this was found to be 120 MPa. The strength of the
material in the as-rolled condition provides us with the
increase in strength due to cold work, and for the RTR ser-
ies of samples that were examined with XRD, the cold
work strengthening was 340 MPa (see Fig. 10b for as-rolled
data).
During heat treatment at 150 °C, the process of static
recovery alleviates work hardening, and the rate of this
recovery has been quantified using XRD for the RTR
and aged series of samples (Fig. 7). Since we know the mag-
nitude of the work hardening in the as-rolled condition, the
decrease in work hardening resulting from static recovery
during heat treatment can be deduced (Fig. 14). Since the
overall strength has also been measured for a number of
conditions (Fig. 10b), we can thus determine the contribu-
tion of precipitate and cluster hardening to the strength of
the alloy for different heat-treatment times (Fig. 14).
It can be seen that heat-treatment results in an initial
increase in the precipitate hardening, but that this compo-
nent reaches a plateau after 8 h of heat treatment. Since
there is no further precipitate hardening after 8 h, but the
static recovery continues to decrease in strength, the result
is that after 8 h of heat treatment only softening of the
alloy can occur, and this is what was observed experimen-
tally. It is also interesting to note that the clusters devel-
oped during room-temperature ageing, which provide
120 MPa strength, develop an additional 80 MPa of
strengthening during the 150 °C heat treatment. Thus the
maximum contribution of precipitates and clusters is
200 MPa, which is significantly less that the strengthening
due to work hardening, which was 340 MPa.
It is evident that, once the influence of cold work and
precipitation has been deconvoluted, the strength response
of all four tests conditions is a result of the concurrent pro-
cesses of precipitate hardening and static recovery. These
act both to harden and soften the microstructure simulta-
 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289 5287

Fig. 13. Forming limit strains for (a) RTR material and (b) cryo-rolled
material.

Fig. 12. Formability of (a) cryo-rolled and (b) RTR samples, after
different heat-treatment times. Formability is expressed as the indentation
depth, IE.

neously, and the net result is very little change in the yield
strength for small heat-treatment times. After an initial rise
in strength at short heat-treatment times, the precipitate
hardening reaches a plateau after 8 h and does not show
any change. This effect, in unison with the static recovery
process which continues to decrease the strength with
increasing time, results in a sudden and marked drop in
strength for all four test conditions.
Fig. 14. Microstructural model of the contribution of cold work and
4.2. Effect of precipitation on ductility precipitate/cluster hardening to the overall yield strength.

The electron microscopy identified that at 8 h of ageing apparent that between these two times, 8 and 30 h, the S
time there were no discrete S-phase precipitates, but that phase develops into well-defined precipitates that can be
they were well developed after 30 h of ageing. It is therefore identified by TEM. It can be seen from the tensile test data
5288 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289
(Fig. 10) and the biaxial formability data (Fig. 12) that
after 8 h of heat treatment, continued heat treatment
results in a significant drop in formability. Since these
two features, namely precipitation and a loss in formabil-
ity, seem to occur in the same heat-treatment window, it
is suggested that the drop in ductility could be associated
with this precipitation process. This is consistent with the
commonly reported observation that precipitation reduces
ductility in many alloy systems [26].
It is further interesting to note that the solute clusters
that develop during room-temperature ageing are also det-
rimental to the rollability of the material. When left to age
at room temperature, this alloy shows extensive edge crack-
ing, whereas no edge cracking is observed if rolling is com-
menced in the supersaturated condition (Fig. 2). The effect
was not so pronounced in tension where the solution-trea-
ted and aged samples showed similar elongations to failure.
The only major difference in that case was the development
of extensive flow serrations in the solution-treated material
during testing, a phenomena resulting from solute locking
of dislocations [24,25]. This dynamic strain ageing phe-
nomena did not appear to reduce tensile ductility (Fig. 9)
or the ability of the material to be rolled (Fig. 3).
4.3. Effect of the ageing sequence on microstructural
development and mechanical properties
As discussed above, there was a strong correlation
between the ageing sequence and formability. Those sam-
ples that were aged before rolling exhibited higher yield
strengths (Fig. 10), lower ductilities (Fig. 10) and signifi-
cantly poorer biaxial forming limits (Fig. 13). This effect is
likely to be the result of the differences in solute cluster
and GP zone development between the two conditions.
The aged samples are held at room temperature to develop
solute clusters after the solution treatment but before roll-
ing. These clusters are likely to be concentrated at pre-exist-
ing dislocations and grain boundaries such as found
previously [12,16]. This is in contrast to the samples that
were rolled immediately after solution treatment, in which
the alloy is in the supersaturated condition with negligible
solute clusters. Since the aged samples have higher strength
and lower ductility, it is likely that the solute clusters assist in
increasing the dislocation density during rolling in a similar
manner to what would be expected from a genuine precipi-
tate. It is also likely that these clusters inhibit the process of
dynamic recovery through subgrain boundary pining.
Another possible effect of the ageing sequence may be to
modify the size and distribution of the solute clusters. For
the samples that were rolled in the solution-treated (not
aged) condition, during the natural ageing period after
rolling the solute clustering develops within a heavily
dislocated microstructure. This is in contrast to the solu-
tion-treated case where the clusters develop inside a clean
microstructure which has not been rolled. It is likely that
the clusters which form in the rolled material (not aged
condition) will be finer and more homogenously distributed
compared to those that were produced during ageing
before rolling (aged condition). The size of these clusters
therefore may have a strong influence on the ductility,
and possibly also the strength of this alloy system. A com-
plete description of how the solute clusters change in size
and distribution, depending on the microstructure from
which they develop, would require the use of atom probe
tomography such as described previously [12]. Atom probe
measurements were outside the scope of the present paper,
but further investigation of the solute clustering behaviour
in this alloy after different rolling schedules is planned for
the near future.
4.4. Effect of rolling temperature
The effect of rolling temperature on the mechanical
properties is best shown in Fig. 10. For the case of the aged
specimens, the rolling temperature had little effect on the
yield strength, or the ductility. However for the not aged
samples there were some significant difference in tensile
behaviour. In terms of yield strength, the RTR samples
showed consistently higher yield strengths than the cryo-
rolled samples. This can be explained by the fact that when
the Unaged samples are cryo-rolled, no solute clustering
can occur until the end of the rolling schedule. However,
for the RTR samples the solutes can form clusters dynam-
ically during the rolling schedule. If we recall the earlier dis-
cussion in which it was described that the presence of
clusters inhibits dynamic recovery and increases strength,
it is now clear that dynamic clustering has increased the
strength of the RTR sample compared to the cryo-rolled
samples in which the rolling was carried out in the clus-
ter-free condition.
The improvement in the ductility of the RTR samples
compared to the cryo-rolled samples is well explained by
the notion that rolling at a higher temperature allows for
improved dynamic recovery and development of a more
defined substructure with a lower dislocation density com-
pared to the lower deformation temperature case.
5. Conclusions
The precipitate-hardenable aluminium alloy 2024 has
been rolled in two different conditions: in a solution-treated
condition immediately after water quenching; and after a
natural ageing treatment during which time the alloy devel-
ops solute clusters. For each of these two conditions the
alloy has been rolled at cryogenic and room temperatures.
From these four different processing routes, heat treat-
ments were carried out at 150 °C for up to 100 h. The fol-
lowing conclusions have been drawn:
 The natural ageing treatment significantly reduced the
rollability of the alloy leading to edge cracking in the
aged condition; this defect was not observed for the
not aged condition.
 M. Weiss et al. / Acta Materialia 61 (2013) 5278–5289
 In the tensile tests all four conditions showed a small
age-hardening response to heat treatment combined
with a significant rise in the tensile ductility.
 In biaxial tension there was a peak in the formability
after 8 h of heat treatment. This corresponded well with
the peak in tensile elongation observed in the tensile test.
 Samples that were aged before rolling showed consis-
tently higher material strength and lower ductility com-
pared to those rolled in the supersaturated condition.
This led to reduced formability with the aged samples
showing significantly lower forming limit strains in biax-
ial tension. It is proposed that the development of solute
clusters during the natural ageing inhibits dynamic
recovery and results in a higher dislocation density com-
pared to the cluster-free condition.
 For the case of the aged samples, the effect of rolling
temperature was negligible on the mechanical proper-
ties. However, for the samples rolled in the supersatu-
rated condition the rolling temperature did have some
effect. For the cryo-rolled sample, the formation of clus-
ters was inhibited by the low rolling temperature, and
this condition developed the least strengthening. It is
suggested that the lack of clusters aided in dynamic
recovery, such that this condition showed the best recov-
ery and consequently the lowest strength. For the case of
the RTR sample, the cluster formation is likely to occur
dynamically during the rolling, so this condition devel-
oped an intermediate strength level.
 A microstructural model has been presented which
shows that the precipitate-hardening increment is at
most 70 MPa and as such only minimal precipitate
hardening can be expected from this alloy in the heavily
worked condition. It is also demonstrated that after an
ageing time of 8 h at 150 °C only softening can occur
in this alloy.
Acknowledgements
The work described in this paper was jointly funded by
Peter Hodgson’s ARC Laureate Fellowship (Grant No.
5289
FL0992361) and Deakin University. The authors would
like to thanks Mahendra Ramajayam, Lynton Leigh, Ro-
sey Van Driel and Andrew Sullivan for their assistance
with the laboratory work carried out in this study.
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