Scripta Materialia 54 (2006) 903–908

www.actamat-journals.com

A new heat treatment procedure for rheo-diecast

AZ91D magnesium alloy
Y. Wang *, G. Liu, Z. Fan
Brunel Centre for Advanced Solidification Technology (BCAST), Brunel University, Uxbridge, Middlesex UB8 3PH, UK

Received 24 April 2005; received in revised form 22 September 2005; accepted 31 October 2005
Available online 28 November 2005

Abstract

A new heat treatment procedure for rheo-diecast AZ91D Mg-alloy, denoted as Tx, has been developed for achieving optimised com-
bination of strength and ductility. Samples were heated at a temperature close to the solvus for a short exposure time to break-up the
brittle b-Mg17Al12 network. In addition, Tx incurs lower heat treatment costs compared with the existing heat treatments.
Ó 2005 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Mg-alloy; Rheo-diecasting; Heat treatment; Microstructure

1. Introduction 16–24 h (T4) followed by aging at 168 °C for 16 h or

AZ91 alloy is the most widely used commercial magne-
sium alloy. It offers a good combination of castability,
mechanical strength and ductility [1]. Currently, the appli-
cations of the Mg alloys are mainly achieved by high pres-
sure diecasting (HPDC), which is characterised by high
efficiency, high production volume and low production
cost. However, the HPDC components contain a substan-
tial amount of porosity due to gas entrapment during die
filling and hot tearing during the solidification in the die
cavity [2]. Such porosity not only deteriorates mechanical
properties, but also denies the opportunity for property
enhancement by subsequent heat treatment. A new semi-
solid processing technology, rheo-diecasting (RDC), has
been recently developed by BCAST at Brunel University
[3–5] and offers advantages, such as extremely low porosity,
fine and uniform microstructure and enhanced mechanical
properties [6]. In addition, the RDC samples are heat treat-
able due to to their low porosity level [6,7].
A full heat treatment (T6) for AZ91D alloy usually
involves two separate steps, solutioning at 430 °C for
*
Corresponding author. Tel.: +44 1895 266411; fax: +44 1895 269758.
E-mail address: yun.wang@brunel.ac.uk (Y. Wang).
alternatively 216 °C for 6 h (T5) [8]. T4 treatment causes
the dissolution of the b-Mg17Al12-phase and improves
ductility significantly, but while sacrificing mechanical
strength. T5 treatment results in precipitation of the coarse
equilibrium b-phase without the appearance of Guinier–
Preston (GP) zones or intermediate precipitates, leading
to a very limited precipitation strengthening effect and a
substantial reduction in ductility [9]. Therefore, it is neces-
sary to develop a new heat treatment schedule to achieve
an optimised combination of mechanical properties.
In order to develop such a new heat treatment schedule,
the following considerations need to be taken into account:
(a) it should break up the b-phase network in such a way
that the ductility is enhanced without losing strength, as
schematically illustrated in Fig. 1; (b) the heat treatment
temperature should be high enough to enhance the kinetics
of phase transformation, but low enough to prevent or
slow down the grain growth; (c) the precipitation of the
b-phase should be avoided to prevent a decrease in ductil-
ity; and (d) it should reduce the heat treatment costs. Based
on such considerations, the best compromise can be
achieved by treating the as-cast AZ91D alloy at a tem-
perature around its solvus, i.e., 370 °C. This has been
named the Tx heat treatment. In this paper, we report

1359-6462/$ - see front matter Ó 2005 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.scriptamat.2005.10.073
904 Y. Wang et al. / Scripta Materialia 54 (2006) 903–908

β β

α-Mg α-Mg

(a) as-cast (b) after Tx

Fig. 1. Schematic illustration of (a) the b-phase network in the RDC

AZ91D alloy and (b) the break-up of the network by Tx heat treatment.

the microstructure and mechanical properties of RDC

AZ91D alloy after Tx heat treatment.
Fig. 2. Optical micrograph showing the as-cast microstructure of the
2. Experimental RDC AZ91D alloy.

The AZ91D alloy with a chemical composition of

and only hot cracks due to solidification shrinkage could
Mg 8.8Al 0.67Zn 0.22Mn 0.03Si 0.002Fe (in wt.%),
be seen occasionally. The measured total porosity in the
was provided by MEL (Magnesium Elektron, Manchester,
RDC sample was well below 0.5 vol.%. The primary parti-
UK). The alloy samples were prepared by the RDC process
cles had a spherical morphology, fine particle size (41 lm)
[3–5]. AZ91D Mg alloy ingots were melted at 675 °C under
and a uniform distribution throughout the entire sample.
the protection of a N2 + 0.5 vol.%SF6 gas mixture and fed
Due to the high cooling rate provided by the metallic die
into the twin screw slurry maker at 630 °C. The slurry
block, the microstructure produced during secondary
maker was operated at a temperature of 593 °C, a screw
rotation speed of 500 rpm and a shearing time of 35 s to
produce the semisolid slurry, which is referred to as
primary solidification. The semisolid produced is then trans-
ferred to a 280-ton cold chamber HPDC machine for
secondary solidification. The RDC samples (/ 6 mm tensile
test pieces) were subsequently heat treated for different
exposure times at temperatures around the solvus (370 °C).
The mechanical properties were characterised using a
Lloyd Instrument EZ50 tensile tester with a crosshead speed
of 1 mm/min. The microstructural characterisation was
carried out using optical microscopy (OM), scanning elec-
tron microscopy (SEM) and transmission electron micros-
copy (TEM). The specimens for OM and SEM were
prepared by the standard technique of grinding and polish-
ing, followed by etching in a solution of 60 vol.% ethylene
glycol, 20 vol.% acetic acid, 1 vol.% concentrated HNO3
and 19 vol.% water. A Zeiss optical microscope was utilised
for the OM and the quantitative metallography, while a Jeol
JXA-840 A was used to perform the SEM. For TEM exam-
ination, samples were cut from the 6 mm diameter tensile
samples along the transverse direction, and 3 mm diameter
discs were hand polished followed by ion bean thinning on
a Gatan precision ion polishing system. TEM analysis was
carried out on a JEOL FX2000 machine operated at 200 kV.

3. Results

3.1. Solidification microstructure of rheo-diecast AZ91D

alloy
Fig. 3. SEM micrographs of the RDC AZ91D alloy showing (a) the
Fig. 2 shows the typical microstructure of the RDC microstructure produced by the secondary solidification and (b) the
AZ91D alloy. No entrapped gas porosity was observed, b-phase network.
 Y. Wang et al. / Scripta Materialia 54 (2006) 903–908 905

Fig. 4. SEM micrographs showing the microstructures of the RDC AZ91D alloy after different heat treatments. (a) 365 °C, 1 h; (b) 365 °C, 1.5 h; (c)
390 °C, 40 min and (d) 390 °C, 1 h.

solidification was very fine. The equiaxed a-Mg grains with

a mean grain size of 6.5 lm were delineated by the b-phase
(Fig. 3a), which formed a network (Fig. 3b). There was no
evidence of coupled eutectic structure in the RDC sample.
It should be pointed out that the b-phase was formed as a
result of non-equilibrium solidification during secondary
solidification in the RDC process.

3.2. Microstructural evolution during Tx heat treatment

SEM micrographs in Fig. 4 show the microstructure of

the RDC AZ91D alloy after different heat treatments.
The heat treatment at 365 °C and 390 °C resulted in partial
dissolution of the b-phase. The b network in the cast struc-
ture (Fig. 3) was broken up through the partial dissolution,
with the majority of the b grains being situated at the triple
grain boundary junctions. Quantitative metallography
revealed that the volume fraction of the b-phase decreased
from 14.8% in the as-cast state, to 6.7% and 4.3% after
being treated at 365 °C for 1 and 1.5 h, respectively, indi-
cating a relatively quick dissolution of the b-phase. A faster
dissolution was observed at higher temperatures, as shown
in Fig. 4. For instance, less than 4 vol.% of the b-phase
could be achieved by a treatment at 390 °C for 1.5 h. A typ-
ical composite structure produced by Tx treatment is
presented in Fig. 5, where the a globules with a volume
Fig. 5. SEM micrograph showing the typical microstructure of the
secondary solidification area in the RDC AZ91D alloy after heat
treatment at 365 °C for 2 h. The average size for the a-Mg grains and
the b intermetallic grains were measured to be 9.3 and 2.8 lm, respectively.
fraction of 19.1% and an average size of 41 lm were uni-
formly distributed in an a–b mixture with a fine grain size.
Due to the much shorter treatment time and lower temper-
ature, severe grain growth was prevented and the fine a
grain structure produced during secondary solidification
of the RDC process was retained. The average grain sizes
906 Y. Wang et al. / Scripta Materialia 54 (2006) 903–908

of the fine a-Mg phase and the b-phase were 9.3 and
2.8 lm, respectively, after Tx treatment at 365 °C for 2 h,
compared with 6.5 lm for the secondary a grains in the
as-cast condition. This composite structure is expected to
offer a superior combination of strength and ductility.
Fig. 6 is a TEM bright field image taken from the sample
treated at 365 °C for 2 h, with the [0 0 1] selected area elec-
tron diffraction (SAD) pattern taken from the labelled
b-Mg17Al12-phase. It can be seen that the remaining b
grains were located at the grain boundaries. The b grains
are found to be virtually free of dislocations, in contrast
to the areas inside the a-Mg grains adjacent to the b-grains.
No precipitation of the b from the supersaturated a-Mg
was observed by TEM after Tx treatment.
Microstructural modification and solute redistribution
has also involved the primary a-Mg particles solidified
inside the slurry maker. The size of the globular particles
was not changed significantly due to the short exposure
time. However, as shown in Fig. 4, halos were observed
inside the primary a globules, which was because of the
diffusion of Al from the b-phase towards the a globules.
The contrast in the SEM images was due to the different
response of different compositions to chemical etching.
The peak in the SEM/energy dispersive spectroscopy
(EDS) line scan, as shown in Fig. 7, could be attributed
to either the contribution from another b particle beneath
the surface, or the local enrichment in Al in the a-Mg due Fig. 7. SEM micrograph and EDS line scan showing the distribution of Al
to the dissolution of the b-phase as a result of the heat concentration across a primary a-Mg particle and the secondary solidi-
fication area after heat treatment at 365 °C for 2 h.
treatment. In addition, the EDS result reveals a gradual
increase in Al concentration inside the a globules towards
the secondary solidification area (Fig. 7). This indicates 3.3. Mechanical properties of the rheo-diecast
that diffusion of Al from the b-phase has reached a certain AZ91D alloy
depth in the a-Mg globules, depending on temperature
and time. This is in contrast to the as-cast structure, where The RDC process has been shown to offer improved
little coring effect was detected inside the a-Mg globules mechanical properties for AZ91D alloy compared with
[6]. those obtained from either the HPDC process or any other
semisolid processing techniques [6,10–13]. A further
improvement can be achieved by Tx treatment. Table 1 lists
the mechanical properties of the RDC alloy after Tx treat-
ment in comparison with those for the same alloy under
different heat treatment conditions. T4 heat treatment
improved ductility substantially but decreased strength,
particularly yield strength. Both T6 and T5 hardly
improved strength, but caused a substantial decrease in
ductility. In contrast, Tx gives a further improvement in

Table 1
Mechanical properties of RDC AZ91D alloy heat treated under different
conditions
Samples Conditions YS UTS Elongation
(MPa) (MPa) (%)
RDC As-cast 145 248 7.4
RDC + T4 413 °C, 5 h 91 230 11.2
Fig. 6. TEM bright field image with the [0 0 1] selected area electron RDC + T5 216 °C, 5 h 133 236 6.5
diffraction (SAD) pattern taken from the labelled b-Mg17Al12-phase, RDC + T6 413 °C, 5 h 134 255 6.7
showing size and morphology of the intermetallic located along the triple + 216 °C, 5.5 h
grain boundary junctions, in the RDC AZ91D alloy after heat treatment RDC + Tx 365 °C, 2 h 132 249 9.1
at 365 °C for 2 h. YS: yield strength.
 Y. Wang et al. / Scripta Materialia 54 (2006) 903–908
ductility at no sacrifice of strength, offering a superior com-
bination of yield strength, ultimate tensile strength and
elongation. An additional advantage of the Tx treatment
is the reduction in heat treatment cost due to the lower tem-
perature and shorter treatment time.
4. Discussion
AZ91D Mg alloy contains about 9 wt.% Al and 1 wt.%
Zn. Under equilibrium conditions, it solidifies as a single
a-Mg solid solution with possible precipitation of the
b-phase from the supersaturated a-phase during subsequent
solid state cooling. However, the cooling rates in most
commercial processes are sufficient to offer a metastable
solidification for all the Mg–Al alloys containing more than
2 wt.% Al [14], resulting in the appearance of the brittle
b-network around the grain boundaries. As the aluminium
content increases, the ductility decreases rapidly above
8 wt.%Al [1,14]. Therefore, the AZ series of Mg-alloys
usually suffer from low ductility in the as-cast condition.
AZ91 alloy generally displays features of brittle fracture,
with cleavage being the principal fracture mode [15,16].
The incompatibility between the body-centred cubic
b-phase and the hexagonal close-packed a-phase leads to
the brittleness of the a/b interface. In addition, the b-phase
itself is a relatively brittle phase and micro-cracks tend to
initiate at the a/b interface and inside the b-grains
[15,16]. The formation of the b-phase network is obviously
detrimental to the mechanical properties, particularly
ductility. Modification of the b-phase by the subsequent
heat treatment is therefore essential to achieve balanced
mechanical properties. For this purpose, solution treat-
ment at 430 °C followed by aging at 220 °C is usually
applied [9,17–21], with the precipitation of the b-phase
from supersaturated a solid solution being extensively
investigated for Mg–Al based alloys including AZ91
[9,17–21]. T4 causes the b-phase to dissolve and it might
be expected that subsequent quenching and aging would
induce significant precipitation hardening. However, aging
results in coarse equilibrium b precipitates without the
appearance of GP zones or intermediate precipitates [9].
The strengthening response to aging is relatively poor.
Tx treatment utilises neither solid solutioning nor the
precipitation of the b-phase due to the relatively poor pre-
cipitation strengthening effect and the significant reduction
of ductility after aging. Instead, the establishment of the Tx
treatment is based upon breaking up the b-phase network
to promote ductility, and retaining the fine and uniform
cast microstructure to maintain high strengths. Indeed,
the b network has been effectively broken up after Tx
and the remaining b grains were fine and uniform, locating
at the a grain boundaries, mostly at the triple grain bound-
ary junctions (Fig. 5), forming a composite structure. It is
obvious that the fine (average 2.8 lm in size) and homoge-
neously dispersed b grains contribute to strengthening,
although b-phase is not an ideal reinforcement [15]. In
addition, the fine grain structure of the secondary solidifi-
907
cation area has been retained, with the secondary a grains
being as fine as 9.3 lm. The dissolution of the b-phase also
increases the supersaturation of Al in the solid solution
matrix, which increases solid solution strengthening
[22,23].
Tx treatment offers an improved combination of
strength and ductility. The substantially improved ductil-
ity, together with the high level of strength, provided by
the RDC process plus the subsequent Tx heat treatment,
could promote wider applications of Mg-alloys. More
importantly, Tx is a single step process carried out at an
intermediate temperature for a much shorter time, which
not only introduces less thermal stresses and increases the
dimensional precision of the heat treated components,
but also reduces the heat treatment cost. In practice, tem-
perature and time for Tx can be selected to suit specific cast
components, offering technological flexibility.
5. Conclusions
(1) A new heat treatment schedule, denoted as Tx, has
been established for rheo-diecast AZ91D alloy in
the present study. As a single step process, the Tx
treatment is carried out at an intermediate tempera-
ture close to the solvus (370 °C) for a much shorter
length of time.
(2) Tx offers an improved combination of strength and
ductility for AZ91D alloy. Compared with T4, it
offers much higher strengths with slightly reduced
elongation. More importantly, Tx is carried out at
low temperature for a short exposure time, therefore
it not only decreases thermal stresses in alloy compo-
nents but also reduces heat treatment costs.
(3) Tx causes partial dissolution of the non-equilibrium b
phase and breaks up the b network, resulting in a
composite structure. This composite structure with
a fine grain size and uniform distribution is believed
to contribute to the superior combination of mecha-
nical properties.
Acknowledgements
The financial support from EPSRC (UK), Ford Motor
Co. and Magnesium Elektron Ltd. (UK) is acknowledged
with gratitude.
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