Scripta Materialia 50 (2004) 1319–1323

www.actamat-journals.com

Effect of a duplex grain size on the tensile ductility

of an ultra-fine grained Al–Mg alloy, AA5754, produced
by asymmetric rolling and annealing
H. Jin, D.J. Lloyd *

Kingston Research and Development Centre, Alcan International Limited, P.O. Box 8400, Kingston, Ont., Canada K7L 5L9
Received 20 October 2003; received in revised form 27 January 2004; accepted 10 February 2004

Abstract
Asymmetric rolling and annealing are used to develop a duplex grain size in the Al–Mg alloy, AA5754. It is shown that with a
coarse grain component of about 20% significant grain size strengthening is achieved while maintaining a tensile elongation
approaching that of much lower strength material.
Ó 2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Al alloys; Ultra-fine grained microstructure; Ductility

1. Introduction 2. Experimental

There is a great deal of interest in ultra-fine grained The material used in this work was AA5754 sheet
and nanocrystalline microstructures as a means of with a nominal chemical composition of Al–3.1Mg–
achieving enhanced strengths and interesting combina- 0.3Mn–0.2Fe–0.1Si (wt.%). Various types of grain
tions of properties. Various methods have been used for structures were produced by proprietary thermal mech-
producing fine scale microstructures and high strengths, anical processing, which involved different combinations
but usually at the expense of tensile ductility [1]. How- of conventional and asymmetric rolling conditions, and
ever, several studies have indicated that introducing subsequent annealing treatments. The asymmetric roll-
coarse grains into an ultra-fine grained microstructure ing was carried out using 161.5 mm diameter rolls with
enhances ductility. Duplex grain sizes in nanophase Cu a velocity ratio between top and bottom rolls of close to
[2,3] and Al alloys [4,5] resulted in a decrease in the yield 2.0. Standard ASTM 5 cm gauge length tensile speci-
strength but a significant increase in the tensile elonga- mens were machined along the rolling direction (RD)
tion. It was recently demonstrated that ultra-fine grain and underwent different annealing treatments at 240–
sizes (grain sizes <5 lm) can be produced in Al–Mg 500 °C in a salt bath.
alloys by a combination of asymmetric rolling (ASR) The resulting grain structure was characterized by
and annealing, with the grain refinement resulting in various means, including optical microscope, transmis-
increased strength [6]. The strength–grain size relation- sion electron microscope (TEM), scanning electron
ship obeyed the Hall–Petch relationship, but the in- microscope (SEM), and electron back scatter diffraction
creased strength was generally accompanied by a (EBSD) in the SEM. The specimens for EBSD analyses
decrease in the tensile elongation. It is of interest to see if were cut from the same tensile blank after heat treat-
a duplex microstructure can enhance the ductility, ments and mounted in the through thickness NT plane,
without too great a sacrifice in strength, in this ultra-fine perpendicular to the rolling direction (RD), using con-
grained material. ductive phenolic compound. After grinding with silicon
carbide paper and 3 lm diamond compound, they were
*
Corresponding author. Tel.: +1-613-541-2012; fax: +1-613-541-
vibrated in colloidal silica for 4 h and immersed in a
2134. 0.5% HF/water solution for 10 s. This method enables
E-mail address: [email protected] (D.J. Lloyd). true through-thickness EBSD scans, since it does not
1359-6462/$ - see front matter Ó 2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.scriptamat.2004.02.021
1320 H. Jin, D.J. Lloyd / Scripta Materialia 50 (2004) 1319–1323

cause rounded specimen edge, so that the electron beam

can approach the region 3–5 lm from edge and provide
solvable Kichuchi pattern.
The through-thickness EBSD measurements were
carried out using a JEOL 5800 SEM equipped with a
Nordlys II EBSD detector, and a 0.25 lm scanning
distance was used to provide detailed spatial informa-
tion. The grain structure reconstruction and analysis
were performed based on the EBSD data using HKL
Channel 5 software. Different misorientation criteria, 3–
15°, were used to differentiate grain boundaries, result-
ing in different grain sizes, but the essential features of
the behavior do not change. In the present paper a grain
boundary is defined as having a misorientation greater
than 3°, and defining a grain as a region with an aspect
ratio less than 4. The grain size (D) was calculated from
the corresponding grain area (A) using a formula
rffiffiffiffiffiffi
4A
D¼ :
p
Tensile tests were carried out at a strain rate of 0.004
s
1 at room temperature.

3. Results

The range of microstructures developed is repre-

sented by the complete surface to surface, through-
thickness orientation maps in Fig. 1, using randomly
assigned colors to differentiate the grains. The micro-
structural evolution as a function of processing condi-
tions can be divided into three types:

1. Ultra-fine grain––after low temperature annealing,

and high levels of stored energy, the through-thick-
ness microstructure has an ultra-fine grain structure
(1 lm average grain size), except that in the sheet cen-
tre some retained deformation structure can be ob-
served (Fig. 1a).
2. Duplex grain––in general, as the annealing tempera- Fig. 1. Through-thickness grain size distribution in (a) ultra-fine
ture increases, some grains grow faster than others grained, (b) duplex and (c) coarse grained material. The transverse
resulting in a duplex grain structure (Fig. 1b). direction is horizontal, and the normal direction is vertical.
3. Coarse grain––at annealing temperature of 300 °C
and higher, the duplex grain structure evolves into a Fig. 2 shows some representative stress–strain curves
uniform coarse grain structure with average grain size for the different types of microstructures; UF is ultra-
above 4 lm (Fig. 1c). fine grained sheet, duplex is sheet with a mixture of
ultra-fine and coarser grains, and AR is the as-rolled
X-ray pole figures of the annealed sheet showed that sheet. The as-rolled sheet has very high strength,
for the ultra-fine grain sizes the deformation texture was reflecting the level of cold work, and recrystallizing the
retained but weakened relative to the worked condition, material results in a decrease in strength accompanied
while the coarse grained material showed no strong by an increase in the tensile elongation. All conditions
preferred components. This indicates that the formation exhibit serrated flow, which is expected due to the solute
of the ultra-fine grained microstructure and subsequent pinning of dislocations by Mg atoms. The morphology
grain growth are continuous processes, rather than the of the serrations is quite variable, with the duplex
more conventional particle stimulated nucleation and structure exhibiting a stepped stress–strain curve indi-
growth. cative of incremental L€ uders band propagation. The
 H. Jin, D.J. Lloyd / Scripta Materialia 50 (2004) 1319–1323 1321

400 1. deformation structure––grain aspect ratio P4;

AR 2. ultra-fine grain––grain aspect ratio <4, grain diame-
ter <4 lm;
350 3. coarse grain––grain aspect ratio <4, grain diameter
P4 lm.
300
These simplified definitions are far from ideal, and
UF any detailed analysis should consider the associated
duplex
stress (MPa)

250 boundary misorientations and their spatial distribution.

UF In fact, the analysis has been further simplified by
combining the volume fractions of the deformation
200 coarse structure and the ultra-fine grained structure into one.
This can be justified to some extent in that after
150 annealing the deformation structure consists of well
formed sub-grains with interiors free of dislocations, so
these regions should contribute a ‘‘grain size strength-
100 ening’’ comparable to the ultra-fine grained component.
The volume fractions (actually area fractions) of each
structure were measured for each processing condition
50
and the results are listed in Table 1. This table also in-
cludes a mean grain size measurement for each condi-
0 tion obtained from a linear intercept analysis.
0 5 10 15 20 25 Fig. 3 shows the influence of the volume fraction of
strain (%) the ultra-fine grained component on the yield and UTS
of the sheet. The strength increases as the concentration
Fig. 2. The stress–strain curves for the various grain structures: AR is of ultra-fine grains increases, as would be expected on
as-rolled sheet, UF is ultra-fine grained, <4 lm grain size sheet, duplex the basis of Hall–Petch grain size strengthening. The
is a duplex grain structure and coarse is conventional coarse grained,
yield and UTS graphs converge as the ultra-fine grain
>4 lm grain size sheet.
content increases, which indicates a decrease in the work
hardening component with decreasing grain size.
Fig. 4 shows the associated tensile elongation that
curves also show a yield point effect, with the L€ uders changes non-monotonically with the ultra-fine grained
strain decreasing with increasing grain size. All of these content, and the uniform strain shows exactly the same
effects are typical of what is expected in Al–Mg alloys behavior. Included in this plot is the elongation of
[7]. The key point from the figure is that the sheet with conventional processed, coarse-grained AA5754 that
the duplex grain structure shows enhanced tensile duc- has a tensile elongation of about 25%.
tility relative to the ultra-fine grained sheet, while The variation with grain structure can be divided into
maintaining a high yield strength. four regions:
To facilitate quantitative analysis, we have defined Region I, where the microstructure is the normal
three types of microstructures based on grain diameter coarse grain structure and there are actually no ultra-
and grain aspect ratio: fine grains, but there is grain refinement and a resulting

Table 1
The volume fractions of different microstructural components and the mean grain size for different processing conditions
Condition Deformation structure (%) Ultra-fine grains (%) Coarse grains (%) Mean grain size (lm)
1 13.9 81.6 4.5 1.42 ± 1.06
2 22.7 67.2 10.1 1.44 ± 0.95
3 18.6 63.3 18.1 1.37 ± 1.02
4 18.5 61.0 20.5 1.62 ± 1.12
5 12.5 47.3 40.1 1.80 ± 1.40
6 14.0 43.2 42.8 1.82 ± 1.45
7 12.4 43.5 44.1 1.95 ± 1.52
8 7.9 40.8 51.3 2.00 ± 1.62
9 0 28.7 71.3 2.93 ± 1.89
10 0 9.3 90.7 4.93 ± 2.63
11 0 3.5 96.5 6.73 ± 3.54
1322 H. Jin, D.J. Lloyd / Scripta Materialia 50 (2004) 1319–1323

300 30
YS
UTS
25
250
Strength (MPa)

Elongation (%)
20
200
15

150
10
I II III IV
100 5
0 20 40 60 80 100 0 20 40 60 80 100
Volume fraction (%) Volume fraction (%)
Fig. 3. The influence of the volume fraction of ultra-fine grains on the Fig. 4. The influence of the volume fraction of ultra-fine grains on the
yield and UTS of AA5754. tensile elongation of AA5754.

The behavior in regions I and IV is expected, with the

increase in yield strength. The apparent existence of
tensile ductility decreasing with increasing strength, but
grains less than 4 lm is due to the misinterpretation of
incorporating coarser grains into the fine grain structure
three-dimensional grains in a two-dimensional section.
enhances the ductility. The maximum effect occurs at a
The tensile elongation in this stage decreases with
coarse grain content of 20–45%.
decreasing mean grain size.
Region II, where the duplex microstructure is being
developed and the total elongation increases with
increasing volume fraction of ultra-fine grain structure. 4. Discussion
Region III, where the elongation reaches a maximum
value, which is close to the total elongation of coarse The results demonstrate that incorporating coarser
grained sheet (i.e., sheet annealed at 500 °C), and the grains into an ultra-fine grained material enhances the
duplex microstructure has 20–45% coarse grains, and tensile ductility, as it does in nanophase alloys. The
Region IV, where the ultra-fine grains dominate presence of coarse grains in the ultra-fine grained mate-
the microstructure, and the plasticity decreases drasti- rial should decrease the strength, and result in a devia-
cally as the ultra-fine grains approach 100% volume tion from the Hall–Petch relationship. Fig. 5 shows that
fraction. this is the case, where the Petch plot for conventional

250

ASR DUPLEX GRAIN

200 DC5754
YIELD STRENGTH (MPa)

150

100

50

0
0.0 0.2 0.4 0.6 0.8 1.0
-1/2 -1/2
(GRAIN SIZE) (µm)

Fig. 5. The Hall–Petch plot for AA5754 with conventional and duplex grain structures.
 H. Jin, D.J. Lloyd / Scripta Materialia 50 (2004) 1319–1323 1323

material is extrapolated out to the ultra-fine grain size tivity is negative in the present sheet, hence the serrated
regime and the expected strength can be compared with flow, and the global work hardening rate is also low at
the present duplex grain structures. Previous experiments these large strains. As a result there is nothing to retard
have shown that ultra-fine grained sheet produced by or stabilize neck growth. However, the present results
asymmetric rolling have strengths comparable to the suggest that at the local scale of the microstructure, the
extrapolated values of conventional sheet [6]. duplex grain structure may result in enhanced work
The reduced tensile ductility in ultra-fine grained and hardening and a reduced rate of neck growth. If this is
nanophase materials is often attributed to a reduced the case it will depend on the spatial distribution of
work hardening rate, resulting in satisfying the Con- grain sizes, which will require further analysis.
sid
ere criterion, dr=de ¼ r at low strains. This is con-
sistent with the behavior of the AR and highest strength
UF material compared with the other conditions in Fig. 5. Conclusions
2, and the deviation of the yield and UTS plots in Fig. 3.
However, the situation is complicated in the present Ultra-fine grained AA5754 can be produced with a
material, as in many examples of ultra-fine grained and duplex grain structure by asymmetric rolling and
nanophase alloys, by the presence of a L€ uders elonga- annealing. Introducing 20–45% coarse grains into the
tion. This can be quite extensive since the L€ uders strain ultra-fine grained microstructure enhances the tensile
is inversely dependent on the grain size [8]. In a plasticity ductility. While the coarse grains generally degrade the
context, L€ udering is localized plastic flow, generating a strength, at the 20% level a high strength is accompanied
high dislocation density with little global work harden- by a tensile ductility approaching conventionally pro-
ing. At high strengths the localized flow can result in cessed material.
fracture, as in the case of the AR sheet in Fig. 2. In the
Al–Mg alloys there is the further complication of ser-
rated flow, in which the plasticity is accommodated by Acknowledgements
localized shear packets occurring randomly in the
deforming region, or by propagation of macroscopic The authors are grateful to Alcan International
L€uders bands that form and propagate after general Limited for permission to publish this work.
yielding. The morphology of serrated flow is dependent
upon the grain structure. The stress–strain curve for the
References
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