Materials Science and Engineering A 410411 (2005) 390393

Processing routes leading to superplastic behaviour

of magnesium alloy ZK60
R. Lapovok a, , P.F. Thomson a , R. Cottam a , Y. Estrin b
a

School of Physics and Materials Engineering, Monash University, Vic. 3800, Australia
b IWW, TU Clausthal, Agricolastr. 6, 38678 Clausthal-Zellerfeld, Germany
Received in revised form 6 March 2005

Abstract
There has recently been discussion on processing of magnesium alloys by equal channel angular extrusion (ECAE) to achieve a high elongationto-failure under superplastic tensile deformation. A two-step processing route was suggested to improve superplastic capabilities of such alloys.
In this work, superplastic behaviour of ZK60 processed by ECAE alone was compared with that for the material that was rolled prior to the ECAE
processing. It was shown that deformation preceding the ECAE step does not bring any benefit with regard to superplastic behaviour in the low
temperature range around 200 C. An important finding is that ECAE processing by itself leads to a record elongation of 1400 and 2040% at the
strain rates of 3 103 and 3 104 s1 , respectively.
2005 Elsevier B.V. All rights reserved.
Keywords: ZK60 magnesium alloy; Equal channel angular extrusion (ECAE); Rolling; Superplasticity; Tension test

1. Introduction
Superplastic behaviour of magnesium alloys, which normally
have limited ductility due to their hcp crystal structure, is of
great interest to manufacturing industry as it broadens the range
of their applications. However, even for widely investigated Mg
alloys, such as ZK60 [18], there is no consensus about the optimum thermo-mechanical processing route leading to enhanced
tensile ductility. There is still no agreement on what type of
microstructure is most favorable for increased elongation-tofailure.
Severe plastic deformation methods, including extrusion,
rolling and equal channel angular extrusion (ECAE) were used
to produce uniform distributions of small grains which was
believed to be a prerequisite for superplastic behaviour [25,7].
However, the maximum elongation achieved in ultrafine grained
ZK60 did not exceed 800%. This elongation-to-failure was
attained in ZK60 processed by ECAE with uniform grains of
about 1 m in diameter [7]. By contrast, bi-modal microstructures [1,2,6,8] were found to exhibit similar, and in many cases
superior, superplastic behaviour. Tensile elongation of 1200 and

Corresponding author. Tel.: +61 3 9905 9294; fax: +61 3 9905 4940.
E-mail address: Rimma.Lapovok@spme.monash.edu.au (R. Lapovok).

0921-5093/$ see front matter 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2005.08.067

1330% was obtained in ZK60 with bi-modal microstructures

produced by double extrusion with large reductions in crosssection [1] and by isothermal rolling preceded by forging [6].
Surprisingly, the use of ECAE for grain refinement, which
produced similar bi-modal microstructures, did not yield such
a good tensile ductility [2,8]. The ability of ECAE to refine
microstructure and create a favorable texture to the same extent
as extrusion does was questioned, and a two-step processing
route, viz., extrusion followed by ECAP, was proposed [9] to
improve superplastic characteristics of magnesium alloys.
In this work, we report the results of a comparative study of
superplastic behaviour of alloy ZK60 after two different deformation histories: ECAE only and ECAE combined with rolling.
2. Experimental procedure
The plates machined from a continuously cast billet of ZK60
(Mg4.95%Zn0.71%Zr) were homogenised for 4 h at 460 C
in alumina powder used to reduce surface oxidation. As a result
of homogenisation, grain boundary precipitates were dissolved,
leaving behind regions rich in zirconium. The initial microstructure consisted of equiaxed grains with average diameter of
45.5 m and isolated zinczirconium particles dispersed within
the grains or occurring in clusters.

R. Lapovok et al. / Materials Science and Engineering A 410411 (2005) 390393

Some of these plates were then rolled at 400 C with thickness

reduction of 75%. Cylindrical specimens with 10 mm diameter and 70 mm length were machined from plates that were
just homogenised and from those rolled after homogenisation in
transverse direction. Both groups of specimens were subjected
to 6 passes of ECAE through 90 die at a ram speed of 0.5 mm/s
and the temperature of 200 C using route BC . After ECAE, tensile samples were machined and tested in the temperature range
of 200300 C at the strain rates of 3 104 to 3 102 s1
using an INSTRON 1341 machine.
Microstructures were investigated using an optical microscope (Olympus, JSM-840) and transmission electron microscope (Philips CM20). The texture of these samples was
investigated by X-ray diffraction using a texture goniometer
GBC-MMA.
3. Experimental results and discussion
The results of tensile testing after two different processing
routes for strain rate of 3 103 s1 are shown in Fig. 1(a).
All stressstrain curves show a well-pronounced strain hardening and strain softening stages, which are not typical of
superplastic behaviour. The softening branch is attributed to
intensive dynamic recrystallisation. Those samples which show
superplastic behaviour with large elongation-to-failure between
1400 and 2040% exhibit a third, plateau-like, branch on the
stressstrain curves. This type of stressstrain curve was found
only for samples processed by ECAE. The tensile ductility versus strain rate is presented in Fig. 1(b). For both processing
histories the strain rate sensitivity parameter, 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. In both cases, the value of m was similarly high, between

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0.5 and 0.6. Hence, the difference in the tensile behaviour associated with the two processing histories cannot be explained in
terms of rate sensitivity differences.
Comparison of microstructure for samples that underwent
one-step deformation (6 passes of ECAE) and two-step deformation (75% rolling followed by 6 passes of ECAE) showed that
in both cases, a bi-modal microstructure with a large average
grain size of about 12 m was formed. However, the volume
fraction of large grains in the samples processed by two-step
deformation was about half of that in the samples processed by
one-step deformation. The grain size of the small grain population, Fig. 2(a and b), was on average smaller for the samples
processed by one-step deformation. Another particularity of
interest is that within the small grain populations there are more
clearly defined recrystallised grains in samples processed by
one-step deformation, while the small grains in the other case
were more heavily deformed, with tangled dislocations within
the small grains being visible, Fig. 2(c and d).
The differences in tensile properties can be explained in terms
of different thermomechanical processing of the two groups of
specimens that results in qualitatively different microstructures.
The ECAE processing according to route BC using a 90 die at
200 C resulted in profuse twinning in the first two passes triggering dynamic recrystallisation at twin boundaries. The average
grain size in the small grain population formed in this case was
smaller than in the two-step processing case. Indeed, dynamic
recrystallisation that occurred during hot rolling reduces the
propensity for twinning during subsequent ECAE deformation,
which was shown [10] to promote dynamic recrystallisation
resulting in a finer small-grain population.
The pole figures generated from samples oriented normally to
the extrusion direction show some differences in texture developed after the two processing histories considered Fig. 3. A more

Fig. 1. Tensile tests for samples processed by one-step deformation (ECAE) and two-step deformation (rolling + ECAE). (a) Stressstrain curves at strain rate of
3 103 s1 ; (b) elongation-to-failure vs. strain rate in tensile tests performed at 220 C.

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R. Lapovok et al. / Materials Science and Engineering A 410411 (2005) 390393

Fig. 2. TEM images of samples with different processing histories. (a) Small grain population in material after ECAE; (b) small grain population in material after
rolling followed by ECAE; (c) example of small recrystallised grain in material after ECAE; (d) example of a small heavily deformed grain in material after rolling
followed by ECAE.

Fig. 3. Pole figures for specimens cut normal to the extrusion directions after the two processing histories. (a) (0 0 0 2) pole figures after ECAE; (b) (1 0 1 0) pole
figures after rolling followed by ECAE; (c) (0 0 0 2) pole figures after ECAE; (d) (1 0 1 0) pole figures after rolling followed by ECAE.

R. Lapovok et al. / Materials Science and Engineering A 410411 (2005) 390393

pronounced texture in case of two-step deformation is recognised in (0 0 0 2) pole figures, cf. Fig. 3(a and c). The difference
in (1 0 1 0) pole figures, Fig. 3(b and d), is less significant. (Note
that Fig. 3(d) can be roughly seen as a reflection of Fig. 3(b)
about the TD axis.)
It is noted that the measured textures are weak, as might
be expected if grain rotation is a contributing mechanism of
deformation in the fine-grained material produced. The fact that
the texture is more pronounced after rolling followed by ECAE
than after ECAE alone suggests a higher proportion of the large
angle grain boundaries in the latter case. This can be the cause of
higher superplastic ductility in the one-step processed material.
4. Conclusions
It is shown that ECAE of magnesium alloys ZK60 can produce microstructures favorable for a very high superplastic
elongation-to-fracture of 1400 and 2040% at low temperatures
such as 220 C and strain rates of 3 103 and 3 104 s1 ,
respectively. An additional deformation step prior the ECAE,
viz., rolling, was shown to reduce the ability of this alloy to
exhibit such record values of elongation-to-failure. The values of tensile ductility of about 480 and 860% under similar tensile testing conditions were reached. The detrimental
effect of rolling was explained by its role in reducing the profuse twinning in the first passes of ECAE which is important
in triggering dynamic recrystallisation in the following passes
and obtaining a fine grain size in the small grain population.
Another important observation is that rolling preceding ECAE
reduces the volume fraction of coarse grain population in the
bi-modal microstructure formed and induces some undesirable

393

texture that is retained after ECAE, which otherwise creates

a very weak texture that appears to be favourable for tensile
ductility.
Acknowledgements
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 Es 74-9/2. The authors are grateful to
Ms. Chamini Mendis for help with TEM.
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