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Extraordinary superplastic ductility of magnesium

alloy ZK60
R. Lapovok,a) R. Cottam, and P.F. Thomson
School of Physics and Materials Engineering, Monash University, Victoria 3800, Australia

Y. Estrin
Institut fr Werkstoffkunde und Werkstofftechnik, TU Clausthal, 38678 Clausthal-Zellerfeld, Germany
(Received 3 December 2004; accepted 9 March 2005)

Exceptionally high tensile ductility of commercial Mg alloy ZK60 is reported. It was

achieved by equal channel angular pressing without any extra processing steps. The
tensile ductility at 220 C was 2040% and 1400% for the strain rates of 3 104 s1
and 3 103 s1, respectively. The strain rate sensitivity of the flow stress exhibited a
value slightly above 0.5, which is characteristic of superplastic deformation. The grain
structure associated with this behavior was shown to be bi-modal with further
separation in two fractions with different grain sizes within the small grain size
population.

For a long time, the question of whether superplastic

properties can be achieved in magnesium alloys, which
normally have limited ductility due to their hexagonal
close-packed (hcp) crystal structure, has been challenging materials scientists and technologists. However, even
for widely investigated Mg alloys such as ZK60 (Mg
5.8% Zn0.6% Zr),18 there is no consensus about the
optimum thermomechanical processing route leading to
enhanced tensile ductility. Of special interest to the
manufacturing industry is the superplastic behavior of
ZK60 in the low-temperature range (below 280 C) at
acceptable strain rates from 3 103 s1 upward.
Summarizing published results,18 it can be noted that
severe plastic deformation methods, which have been
used to refine the grain structure, resulted in either uniform fine-grained27 or bimodal microstructures.1,2,8 The
latter are characterized by coexistence of two populations
of grains with distinctly different average size and morphology. Generally, superplastic behavior was attributed
to uniform distributions of small grains, the tensile ductility being improved by decreasing average grain size.
The maximum elongation achieved in ZK60 processed
by equal channel angular pressing (ECAP) resulting in
uniform grains of 1 m in diameter was 800%.7

a)

Address all correspondence to this author.

e-mail: Rimma.Lapovok@spme.monash.edu.au
DOI: 10.1557/JMR.2005.0180
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A very high tensile ductility with an elongation

of 1200% was obtained in bimodal microstructures1
produced by double extrusion with large reductions in
cross-section. Surprisingly, the use of ECAP for grain
refinement, which produced similar bimodal microstructures, did not yield such a good tensile ductility.2,8 The
ability of ECAP to refine microstructure and create a
favorable texture to the same extent extrusion does, was
questioned, and a two-step processing routenamely,
extrusion followed by ECAPwas proposed9 to improve superplastic characteristics of magnesium alloys.
The questions of whether a superplastic elongation beyond the 1200% reported in Ref. 1 is attainable by ECAP
without an extrusion step, and what microstructures give
rise to such a level of ductility, are still open.
The present study demonstrates that ECAP as such,
without any extra processing steps, is capable of yielding
an extremely high superplastic ductility. As shown in
Fig. 1, very high tensile elongation of more than 2040%
and more than 1400% were achieved for the strain rates
of 3 104 and 3 103 s1, respectively, at a temperature of 220 C. All tests were repeated at least two or
more times if variation in ductility was significant.
The two samples tested at the strain rate of 3 103 s1
(Fig. 1) correspond to the largest (1700%) and the smallest (1400%) extension obtained at this strain rate. This
superplastic ductility is extraordinarily high, compared to
any result on low temperature superplasticity of ZK60
ever published.
2005 Materials Research Society

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FIG. 1. Tensile samples shown in the initial geometry (upper photograph) and after deformation with various strain rates at 220 C.

The experiments that yielded these results were conducted in the following way. Cylindrical samples 10 mm
in diameter and 70 mm in length were machined from a
continuously cast billet and homogenized for 4 h at
460 C in alumina powder. The initial microstructure
consisted of equiaxed grains with average diameter of
45.5 m. Warm ECAP was performed at 200 C with a
90 die, using ECAP route Bc with a constant ram velocity of 0.5 mm/s. After 6 ECAP passes, tensile specimens machined from ECAP processed material (Fig. 1,
upper photograph) were tested in the temperature range
of 200 260 C at different strain rates in the range of
3 104 to 3 102 s1. The engineering stress versus
strain curves for these tests are depicted in Fig. 2. The
best result of all in terms of tensile ductility is that obtained at 220 C for a strain rate of 3 104 s1(see the
lowest photograph in Fig. 1). However, the tensile ductility at a higher strain rate of 3 103 s1 also exceeded
all previously published results and reached a value of at
least 1400%. A study of microstructure after tensile testing at different temperatures showed the microstructure
was stable as long as the tensile test temperature did not
significantly exceed the ECAP temperature (up to 220 C
in the case under consideration).
One of the prerequisites of superplastic deformation
is an increased strain rate sensitivity of flow stress m
( ln / ln ), where is the flow stress, and and
denote the strain and the strain rate, respectively. There is
a consensus in literature that, in addition to sufficiently
small grain size, the magnitude of m should be at least 0.3
or higher for superplastic behavior to be possible (see
Ref. 10). In the present study, m was measured in strain
rate jump tests at various strains, particularly in the strain
hardening, stress peak, and strain softening regions of the
tensile curves. The strain rate in these tests was changed
abruptly between 3 104 and 3 103 s1 several times
along a tensile curve. At temperature of 220 C, the
measured values of m close to 0.5 were fairly insensitive
to the strain at which a strain rate jump was performed.
This level of m is typical of classical superplastic behavior believed to involve grain boundary sliding.11
Identification of the mechanism responsible for the
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FIG. 2. Stress versus strain curves corresponding to tensile deformation of the ECAP processed material (a) at different strain rates and
(b) different temperatures.

extraordinary superplasticity obtained by the aforementioned ECAP processing requires further study, which is
beyond the scope of this paper. However, first insight
into the microstructure of the material produced after 6
ECAP passes was obtained by transmission electron
microscopy (TEM). Some data were available from a
previous study,12 which showed the occurrence of a
bimodal grain size distribution in the grain structure of
ECAP processed ZK60. It was further established that
both the average grain size for either population and its
volume fraction depend on the ECAP route, the processing temperature, and the amount of strain produced in
each pass (and thus the cumulative strain). The ECAP
processing according to route BC using a 90 die at
200 C resulted in profuse twinning in the first two
passes triggering dynamic recrystallization at twin
boundaries. The twinning activity then decreased over

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FIG. 3. Bimodal grain structure after 6 ECAP passes at 200 C as

observed by light microscopy.

the subsequent four passes. Grain refinement appeared to

result from two concurrent effects: formation of a large
population of small recrystallised grains at old grain
boundaries and fragmentation of large grains by twins
serving as sites at which new recrystallised grains formed
in a necklace. A general trend observed was that the
area fraction of surviving large grains and their average
diameter, as well as the diameter of small recrystallized
grains, were the smallest for the lowest possible temperature of ECAP in combination with the highest strain per
pass.12
Further microstructural investigations conducted in the
present work confirmed the bi-modality of grain size
distribution obtained. The two grain populations had distinctly different grain sizes in the range of 1.8 1.5 m
for small grains and about 12.5 2.2 m for large grains,
as seen in a light microscopy image (Fig. 3) and in a
TEM micrograph [Fig. 4(a)]. However, the microstructure is even more complex than that. Indeed, the
small grain population itself can, in turn, be considered

FIG. 4. TEM images of the microstructure of ZK60 processed by 6 ECAP passes: (a) part of (1) a large grain 10 m surrounded by (2) small
recrystallised grains; (b) small grains 0.50.6 m in diameter with visibly different dislocation structure; (c) two fractions within small grain
population, (1) relatively large 4 m and (2) small 0.4 m grains; (d) fragmentation of a 4 m grain into dislocation cells.
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bimodal,as it is a mixture of two fractions: relatively

large grains (4 m) and very small ones (0.4 m)
[Figs. 4(b) and 4(c)]. The grain structure after the ECAP
processing used is, thus, effectively trimodal. It is interesting to mention that after 6 ECAP passes, no twinning
was recorded across the entire grain population studied,
even in the grains 4 m and above in size. Instead, grain
fragmentation by dislocation cell formation was observed, as illustrated by the micrograph in Fig. 4(d).
These microstructural observations are in agreement
with the statement by Wang et al.,13 who claim that
enhanced ductility of severely deformed metallic materials is a result of bimodality of their grain structure.
However, we have yet to investigate whether our observation of splitting of the small grain population into two
fractions has any relevance to the extraordinary ductility
of this alloy under the conditions studied.
TEM evidence (not presented here) also shows the
presence of MgZnZr precipitates in the ECAP processed material, as expected from the study of deformation induced precipitation sequences in ZK60.14 These
precipitates are believed to stabilize the ultrafine grain
structure produced by ECAP through grain boundary
pinning.
A comment on the shape of the stress versus strain
curves shown in Fig. 2 is also due here, as these do not
exhibit plateaulike portions typical of classical superplastic behavior and corresponding to steady state deformation. By contrast, a pronounced strain hardening portion,
followed by a continual drop-off in stress, was observed
at all strain rates and temperatures investigated. The ascending branches of the curves can be associated with the
presence of a population of large grains deforming by
dislocation glide12 and giving rise to strain hardening.
The reason for the descending branches may be seen in
an increase of the population of small recrystallized
grains during tensile deformation. Provided that the small
grains do not give rise to strain hardening, but rather
deform by grain boundary sliding11 or another mechanism involving diffusion, an increase in their volume
fraction will lead to overall softening.
In conclusion, it has been demonstrated that ECAP
without any further thermomechanical processing steps
is capable of ensuring superplastic deformation of magnesium alloy ZK60. The expectation that severe plastic
deformation by ECAP can produce enhanced ductility15
has been confirmed for this material. Moreover, the
amount of tensile ductility achieved at the relatively low
temperature of 220 C and at strain rate usable for technological applications of the material, is at a record level.
Microstructural observations revealed bimodality of the
grain size distribution, which according to Wang et al.,13
may be responsible for the superplastic behavior observed. Additional break-down of the small grain

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population into two distinct fractions effectively producing a tri-modal grain size distribution might be a factor as
well.
ACKNOWLEDGMENTS

This work was supported by the Australian Research

Council through Large Grant No. A00013833. One of
the authors (Y.E.) also acknowledges support from the
Deutsche Forschungsgemeinschaft through Grant No. Es
74-9/2. The authors are grateful to Ms. Chamini Mendis
for help with TEM.
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