Hydrostatic Extrusion at 100°C and Its Effect On The Grain Size and Mechanical Properties of Magnesium Alloys

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Metal Science and Heat Treatment

Vol. 48, Nos. 11 12, 2006

UDC 669.721.5:621.771.01

HYDROSTATIC EXTRUSION AT 100C AND ITS EFFECT ON THE GRAIN


SIZE AND MECHANICAL PROPERTIES OF MAGNESIUM ALLOYS
J. Swiostek,1 D. Letzing,1 and K. U. Kainer1
Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 11, pp. 31 35, November, 2006.

The microstructure and mechanical properties of magnesium alloys are studied after extrusion. Shapes are obtained from commercial magnesium alloys with the help of a rarely used technology, i.e., hydrostatic extrusion
at 100C (a temperature much lower than the one at which new slip planes are activated). All the tests are performed with allowance for typical parameters, such as the rate of extrusion and the degree of drawing, in order
to choose appropriate conditions for fabricating a material with exceptionally fine grains, which is typical for a
structure formed as a result of equal-channel angular extrusion (ECAE). The constraints connected with this
kind of treatment are discussed as well as the effects of its parameters on the microstructure and mechanical
properties of the extruded shapes.

In the present work we used hydrostatic extrusion for


fabricating experimental batches of alloys with the aim of
lowering the deformation temperature to a value noticeably
lower than 200C. In accordance with our preliminary data
[14] we expected that such a process should ensure refinement of grains and thus guarantee improvement of mechanical properties. The elongation of the alloys was also expected
to increase, because it is usually associated with the effect of
finer grains [15].
Test batches of commercial deformable magnesium alloys of various grades were chosen for the process of hydrostatic extrusion with the aim of investigation of their behavior in the process. The degree of drawing and the rate of the
extrusion corresponded to typical production parameters. It
was shown that a process conducted in a hydrostat had a favorable effect on the machinability, changes in the microstructure, and mechanical properties of magnesium alloys.
The aim of the work consisted in studying the structure
and mechanical properties of magnesium alloys after hydrostatic extrusion and choosing the conditions ensuring fine
grains in the alloy at preserved mechanical properties.

INTRODUCTION
Deformable magnesium alloys present special interest
for the production of parts because they have an improved
and more homogeneous structure than cast alloys at the same
level of mechanical properties. The market of deformable
magnesium alloys is relatively small and they are used for
special purposes due to the high cost of preforms. Today the
cost of primary magnesium has dropped and the process of
magnesium extrusion becomes compatible with the extrusion
of aluminum, which means that research in this direction requires activation.
The ECAE technology, the many-pass forging, and the
methods of powder metallurgy ensure in the treated alloys a
microstructure with grains 1 4 mm in size [1 3]. However,
these processes are quite expensive and present primarily academic interest. Recent experiments have shown applicability of hydrostatic extrusion to the production of shapes from
magnesium alloys [4, 5]. This technology ensures refinement
of grains in the alloys and permits elevated degrees and rates
of extrusion at a lower temperature as compared to the conditions of commercial direct and indirect extrusion [6, 7]. It is
well known that the adaptability of magnesium alloys to
manufacture at a temperature lower than 200 225C is either poor or totally impossible [8, 9]. Consequently, the temperatures typical for direct and indirect extrusion of magnesium alloys range within 260 450C [10]. This temperature
range is also used for forging and stamping [11 13].
1

METHODS OF STUDY
Preforms from commercial alloys AZ31, AZ61, AZ80,
ZM21, ZK30, and ZE10 with a diameter of 95 mm were obtained by pressure die casting and subjected to hydrostatic
extrusion after mechanical treatment for a diameter of
80 mm. Then the preforms were heat treated at 350C for

GKSS Research Center, Institute of Materials Research, Center of


Magnesium Technology, Geesthacht, Germany.

499
0026-0673/06/1112-0499 2006 Springer Science + Business Media, Inc.

500

J. Swiostek et al.
p, P

1400
1200
1000
800

4
5
8

20C
100C

600

200C
300C

6
400

Fig. 1. Diagram of the device and of the process of hydrostatic extrusion: 1, 3 ) seal (cup); 2 ) preform; 4 ) ready shape; 5 ) die; 6 ) container hydrostat; 7 ) working medium; 8 ) plunger.

200
0

20

40

60

80

100

120

l, mm
Fig. 3. Variation of extrusion pressure p of alloy AZ31 upon motion
of the plunger (l is the path of the motion). The figures at the curves
denote the deformation temperature.

Fig. 2. ASEA-12MN hydrostatic press (Freiburg, Germany).

12 h (AZ31, AZ61, ZM21, ZK30, and ZE10) and at 385C


for 12 h (AZ80) with cooling in air.
A schematic diagram of the device for hydrostatic extrusion is presented in Fig. 1. The moving plunger compresses
the working medium, which in its turn creates uniform hydrostatic pressure on the preform and pushes it through the
die. We performed hydrostatic extrusion in a 12MN-ASEA
(-Press) with maximum extrusion pressure of 1400 MPa (see
Fig. 2). A detailed description of the process of hydrostatic
extrusion is presented in [16].
The main tests were made for alloy AZ31 at extrusion
temperature of 20 300C. The lowest extrusion tempera-

ture to be used for further study was determined experimentally. Bars of alloy AZ31 were extruded with a draw ratio of
1 : 28 at all the temperatures. The lubricant was MoS2 molybdenum sulfide. It can be seen from Fig. 3 that the maximum extrusion pressure increases upon a decrease in the deformation temperature. Despite the high extrusion rate and
the low deformation temperature the maximum pressure in
all the cases studied did not exceed the value of 1400 MPa
admissible for the press (Fig. 3).
In order to avoid fracture of the material in the initial
stage of extrusion the die was heated preliminary to 300C,
but decrease in the temperature to 100C also gave positive
results. We will present the results obtained for the variant
with preliminary heating of the die to 300C.
All the tests of alloys AZ31, AZ61, ZM21, ZK30, and
ZE10 were performed at extrusion temperature of 100C.
Preliminary tests showed that after extrusion of alloy AZ80
at 100C cold cracks appeared on the surface of the bars. For
this reason the temperature of extrusion of alloy AZ80 was
increased to 110C. Table 1 presents the extrusion parameters of different alloys and Fig. 4 presents the shapes obtained by the extrusion. It is known from traditional tests that
the extrusion speeds of alloys AZ31 and AZ80, equal to

TABLE 1. Parameters of Extrusion of Magnesium Alloys


Alloy

AZ31
AZ61
AZ80
ZM21
ZK30
ZE10

Chemical composition (wt.%)

textr , C

Mg 2.9Al 0.98Zn 0.29Mn 300, 200, 100, room


Mg 6.5Al 0.99Zn 0.20Mn
100
Mg 8.5Al 0.51Zn 0.31Mn
110
Mg 2.0Zn 0.98Mn
100
Mg 3.0Zn 0.58Zr
100
Mg 1.22Zn 0.4Zr 0.3REM
100

dpr , mm

dsh , mm

v, m/min

80
80
80
80
80
80

15
15
15
15
15
15

28
28
28
28
28
28

8
8
8
8
8
8

Notations: textr ) extrusion temperature; dpr ) diameter of preform; dsh ) diameter of shape; n ) draw ratio; v ) speed
of extrusion.

Hydrostatic Extrusion at 100C and Its Effect on the Grain Size and Mechanical Properties of Magnesium Alloys

501

500 mm

500 mm

500 mm

500 mm

500 mm

500 mm

100 mm
Fig. 4. Shapes extruded at a low temperature and initial preforms
from magnesium alloys.

about 2 and 4 m/min, respectively, are assumed to be maximum permissible ones [17]. In the present work experiments
were made at a speed of 8 m/min, which is the minimum
possible value for hydrostatic extrusion in 12NM-ASEA
(Fig. 2).
We analyzed the microstructure under a light microscope
using polished and etched microsections cut over the direction of the extrusion. The specimens were etched by a solution based on picric acid [18]. Compressive and tensile tests
were performed at room temperature in accordance with the
DIN 50125 instruction in a Zwick Z050 commercial testing machine with a maximum permissible load of 50 kN at a
deformation rate of 10 3 sec 1.
RESULTS AND DISCUSSION
The microstructure in the central part of cast preforms in
the longitudinal direction is presented in Fig. 5. It can be
seen that the microstructure of alloys AZ31, AZ61, AZ80,
and ZM21 is characterized by quite coarse grains
300 500 mm in size (Fig. 5a d ). Alloys ZK30 and ZK10
have fine grains 40 60 mm in size (Fig. 5e and f ). These alloys contain zirconium that acts as a modifier [9].
Subsequent tests with extrusion of the alloys at 100C (at
110C for alloy AZ80) in the modes presented in Table 1 allowed us to fabricate shapes with a smooth surface (Fig. 4)
bearing neither cold nor hot cracks. Similar results that will
not be presented were obtained for shapes of other sizes.
Longitudinal specimens were cut from extrusion-formed
bars for studying the microstructure. The results of the study
are presented in Fig. 7. It can be seen that the extrusion
causes full recrystallization of the structure in all the alloys.
It can be inferred that the parameters of the process presented
in Table 1 ensure the occurrence of dynamic recrystallization
at the chosen process temperatures.
Analysis of the mean grain size in each alloy (Fig. 8)
shows that in all bars obtained by hydrostatic extrusion the

Fig. 5. Microstructure of magnesium alloys in cast state: a) AZ31;


b ) AZ61; c) AZ80; d ) ZM21; e) ZK30; f ) ZE10.

grain size becomes much smaller. For alloys of the AZ series


the grain size increases with the content of aluminum. The
smallest grain size (1.8 mm) is observed in alloy ZE10. The
mean grain size in alloys AZ31, ZK30, and AZ61 is
2 4 mm. This fineness is explainable by the less abrupt
growth in the temperature in the process of hydrostatic extrusion [21], but this hypothesis requires additional experimental confirmation. In alloys AZ80 and ZM21 the grain size decreases to 6 7 mm. Hydrostatic extrusion promotes maxi-

p, P
1200

pmax
p

1000
800
600
400
200
0
AZ31

AZ61

AZ80

ZM21

ZK30

ZE10

Fig. 6. Pressing pressure in extrusion of the alloys at 100C (110C


for AZ80).

502

J. Swiostek et al.
sr , P
400

350
300
250
200
20 mm

20 mm

150
100
50
0
AZ31

AZ61 AZ80

ZM21 ZK30 ZE10

s0.2 , P
400
20 mm

20 mm

Extension
ompression

350

300
250
200
150
100
20 mm

20 mm

Fig. 7. Microstructure of extruded alloys (the arrow shows the direction of the extrusion): a) AZ31; b ) AZ61; c) AZ80; d ) ZM21;
e) ZK30; f ) ZE10; a, b, d, e, f ) extrusion temperature 100C;
c) 110C.

50
0

AZ31

AZ61 AZ80

ZM21 ZK30 ZE10

d, %
40

35
30
25

mum refinement of grains in preforms of the AZ series and


ZM21. Consequently, we have grounds to infer that the technology in question ensures effective refinement of grains in
all the alloys. It should be noted that the grain sizes in alloys
ZE10, AZ31, ZK30, and AZ61 obtained by hydrostatic extrusion are comparable with those obtained due to ECAE [1].
Figure 9 presents mechanical properties of extruded bars
obtained in tensile and compressive tests at room tempera-

20
15
10
5
0

AZ31

AZ61 AZ80

ZM21 ZK30 ZE10

Fig. 9. Ultimate rupture strength (a), tensile and compressive yield


strength (b ), and elongation (c) of magnesium alloys after hydrostatic extrusion at 100C.

d, mm
9
8
7
6
5
4
3
2
1
0
AZ31

AZ61

AZ80

ZM21

ZK30

ZE10

Fig. 8. Mean grain size in the alloys after extrusion at 100C


(110C for AZ80).

ture at deformation rate e& = 10 3 sec 1. It can be seen that


the ultimate rupture strength of alloys AZ31, AZ61, and
ZK30 (Fig. 9a ) increases considerably (by 10 25%) with
respect to sr ensured by conventional extrusion [10, 12]. For
deformable magnesium alloys AZ80, ZM21, and ZE10 we
obtained typical values of this quantity. With growth of the
aluminum content the value of sr increased, which can be associated with more effective precipitation hardening of the
solid solution under the effect of aluminum.
When working with magnesium, it is always necessary
to remember the anisotropy of mechanical properties that
limits their use. It can be expected that magnesium alloys
having an hcp lattice should exhibit a well manifested de-

Hydrostatic Extrusion at 100C and Its Effect on the Grain Size and Mechanical Properties of Magnesium Alloys

pendence of the strain mechanisms on the orientation, which


should be responsible for the difference in the tensile and
compressive strength characteristics [19, 20]. For this reason, we determined the values of compressive and tensile
yield strengths. It can be seen from Fig. 9b that the yield
strength has a tendency to increase in the alloys with fine
grains, which agrees with the Hall Petch relation [3]. In all
the cases studied in our work the tensile yield strength had
the same or somewhat higher values as compared with the
compressive yield strength. This fact can be explained by the
absence of twinning, which is the leading orientation-dependent mechanism of strain in magnesium alloys. If the
microstructure of the alloy is characterized by very fine
grains, the role of twinning seems to be less important [22],
and this reduces the anisotropy. Only ZM21, which has the
largest grains after extrusion, exhibits noticeable anisotropy
of the properties, though the microstructure does not contain
twins (Fig. 7d ). However, it can be assumed that in addition
to grain size and twinning, the anisotropy also depends on
the chemical composition of the alloy: despite the close grain
sizes in alloys ZE10, AZ31, and ZK30 their tensile and compressive strengths differ. Figure 9c presents the values of
elongation for all the studied alloys. Alloys ZE10, AZ31, and
ZK30 with the finest grains have the highest elongation. The
grain size in the extruded bars is the strongest factor affecting
their mechanical properties.
Hydrostatic extrusion at a speed of 8 m/min turned out
to be successful for all the alloys and ensured the same or
even elevated properties. It should be mentioned specially
that hydrostatic extrusion of alloy AZ80 could be performed
without problem at a deformation rate four times higher than
in the case of conventional extrusion [17].
CONCLUSIONS
1. Deformation of magnesium alloys at a temperature below 100C is a quite inefficient method due to the inadequate
number of activated slip systems. For this reason specialists
avoid using standard processes (rolling, direct extrusion, die
forging) for the deformation. Other forming processes, such
as ECAE, are conducted at elevated temperatures.
2. Hydrostatic extrusion makes it possible to lower the
process temperature to 100C for alloys AZ31, AZ61, ZM21,
ZK30, and ZE10 and to 110C for alloy AZ80.
3. Hydrostatic extrusion of deformable magnesium alloys yields a microstructure with exceptionally fine grains at
high plasticity and yield strength. After extrusion at 100C
the expected difference in the values of tensile and compressive strengths (the anisotropy) decreases noticeably. Alloys
AZ31, AZ61, ZK30, and ZE10 present special interest from

503

the standpoint of suitability for low-temperature hydrostatic


extrusion.
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