Micro-extrusion of ECAP processed magnesium alloy for

production of high strength magnesium micro-gears

W.J. Kim
*
, Y.K. Sa
Department of Materials Science and Engineering, Hong-Ik University 72-1, Sangsu-dong, Mapo-gu, Seoul 121-791, South Korea
Received 18 October 2005; received in revised form 20 November 2005; accepted 24 November 2005
Available online 18 January 2006
Abstract
Micro-gear extrusion of the ne-grained equal channel angular pressed (ECAPed) AZ31 alloy was successfully performed. High
strength gears (yield stress >350 MPa) could be produced by eective grain-renement through ECAP and texture restoration to the
original state before ECAP by subsequent extrusion.
2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Keywords: Extrusion; Equal channel angular pressing (ECAP); Magnesium alloys; Hardness test; Superplasticity
1. Introduction
Fabrication of components for microsystems is a key
enabling technology for a new generation of miniaturized
devices in a wide range of application areas such as optics,
medical equipment, semiconductor manufacture, robotics
and biotechnology. Usage of metal, ceramics, or metallic
glasses in microsystem technology becomes important in
future technology because these materials have higher
strength and wear resistance than the polymers that are
being used most widely. Currently, the microinjection
molding method is used to produce micro-components of
metals or ceramics. From the viewpoint of production
engineering, however, plastic forming processes can oer
an advantage in productivity and enable mass production
with controlled quality, low cost and reduced processing
steps. Saotome and Iwazaki [1] demonstrated that amor-
phous alloys exhibiting Newtonian viscous ow under
special conditions can be used as materials for fabricating
various microparts for micro-electro-mechanical systems
by plastic working. When dealing with polycrystalline
metallic alloys, on the other hand, a small grain size is
important since superplastic ow controlled by grain
boundary sliding can be enhanced and has a great advan-
tage in achieving large deformation under low stresses
compared to conventional plastic deformation.
Magnesium is the lightest metal that can be used for
structural application and has superior specic stiness
and strength. Signicant grain-renement by equal channel
angular pressing (ECAP) has been demonstrated in Mg
alloys [27]. During ECAP, the sample undergoes plastic
deformation by pure shear, in theory, as it is deformed
through the intersecting corner. As it can be deformed
repeatedly, very high strain can be accumulated on the
same sample. Superplasticity of the ECAPed Mg alloys
has been studied by several authors [2,3,7]. The ECAPed
Mg alloys were capable of producing both low temperature
superplasticity and high-strain rate superplasticity. Super-
plastic forging ability of the ECAPed AZ31 alloys in a
closed die at a relatively low temperature and high-strain
rate has been investigated by the current authors [8]. The
forged sample shown in Fig. 1 is where a cylinder-shaped
ECAPed Mg billet prepared from the AZ31 alloy after 6
passes (13.5 mm diameter 14.5 mm height) was deformed
to 2 mm in height at 553 K at an initial strain rate of
2 10
2
s
1
. An emblem with high surface quality and
good replication could be produced.
1359-6462/$ - see front matter 2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.scriptamat.2005.11.066
*
Corresponding author. Tel.: +82 2320 1468; fax: +82 2325 6116.
E-mail address: kimwj@wow.hongik.ac.kr (W.J. Kim).
www.actamat-journals.com
Scripta Materialia 54 (2006) 13911395
In this paper, micro-extrusion ability of the ECAPed
Mg alloy was examined. The present result demonstrates
that high strength AZ31 micro-components with yield
stress of >350 MPa could be fabricated by controlling
grain-renement and texture.
2. Experimental methods
The extruded rod of AZ31 alloy with a diameter of
14.5 mm was cut to pieces with a length of 100 mm. The
rod was held at 553 K for 1.8 ks and then pressed with a
speed of 4 mm/s through a die made of SKD 61, with an
internal angle (U) of 90 between the vertical and horizon-
tal channels and a curvature angle (W) of 30, which was
preheated to 533 K. Molybdenum disulphide (MoS
2
) was
used as a lubricant. Repetitive pressings of the same sample
were performed to 6 passes by rotating it about the longi-
tudinal axis by 90 in the same direction between consecu-
tive passes (designated as route B
c
). After the ECAP
process, the sample was cooled to room temperature in
air. Tensile specimens of dog-bone geometry with the
5 mm gauge length, 4 mm width, 2 mm thickness, and
2 mm shoulder radius, having the gauge length parallel to
the longitudinal axis were extracted from the center portion
of the ECAPed Mg by using electro-discharge machining
(EDM).
For micro-extrusion testing, a forward micro-extrusion
machine has been developed. The machine is composed
of two parts: the extrusion unit and the container unit.
A stepping motor has been employed as a punch driver
with 1.8 of resolution capability in the extrusion unit.
Extrusion velocity was controlled to move 1 mm as the
stepping motor rotates by 360. In Fig. 2, a schematic illus-
tration of the container unit is shown. The container unit
is divided into four parts: dummy, specimen, micro-die
and die supporter. Micro-extrusion samples with 2 mm
in diameter and 6 mm in length were extracted from the
center of the ECAPed AZ31. The dimensions of the die
machined with a wire electrical discharge machine are as
follows: the gear module is 0.18 mm and the number of
teeth is 8, and consequently, diameter of pitch circle is
1.44 mm and diameter of outer tooth is 1.8 mm. The shape
of micro-die is shown in Fig. 2. Micro-extrusion testing
was conducted at 533 or 573 K at a ram speed of
0.4 mm/min in a chamber purged by N
2
gas. Boron nitride
lubricant was used to reduce the friction between the sam-
ple and container as well as between the sample and micro-
die. The sample was loaded into a container, heated to the
testing temperature and then extruded into the gear die
after a holding time of 10 min. Testing temperature was
controlled to be within 1 K throughout the test. The
Vickers micro-hardness (H
V
) was measured on the plane
perpendicular to the longitudinal axes, by imposing a load
of 100 g for 15 s.
3. Results and discussion
Fig. 3 shows the photographs of the materials before
ECAP and after ECAP at 553 K by 6 passes. As seen from
the gures, the microstructure of the as-extruded material
(d = 23.9 lm, where d is the true grain size) has been signif-
icantly rened to ne grains after 6 passes (d = 4.1 lm).
More uniform distribution of grain size is also resulted.
Fig. 4 shows the engineering stressengineering strain
curves of the unECAPed and ECAPed AZ31 alloys after
6 passes. Comparison of the two materials indicates that
there occurs a large drop in yield stress after ECAP despite
the large reduction in grain size. According to the texture
analysis, EDkh10

10i ber texture of the unECAPed

AZ31 alloy where {0001} basal planes and h10

10i direc-
tions in most grains are distributed parallel to the extrusion
direction (ED) has completely changed to 01

12

243
Fig. 1. A cylinder-shaped ECAPed Mg billet obtained after 6 passes
(13.5 mm diameter 14.5 mm height) was forged to an emblem to 2 mm in
height in a close die at 553 K at an initial strain rate of 2 10
2
s
1
.
Fig. 2. A schematic diagram for the forward extrusion unit (left) and a gear die made by electro-discharge machining (right).
1392 W.J. Kim, Y.K. Sa / Scripta Materialia 54 (2006) 13911395
after 6 passes at 553 K [4]. Schmid factors of three slip
directions on the basal and prismatic planes could be calcu-
lated based on the major texture components [4,5] and it
was found that the basal planes originally aligned parallel
to the extrusion direction (ber texture) rotated to be
favorably oriented for slip during ECAP as proved by
the increased Schmid factors. Another observation from
the curves is that uniform tensile elongation as well as total
tensile elongation have been signicantly improved after 6
passes, namely, by about three times. This is a consequence
of strain-hardening increase after ECAP, and activation of
non-basal slip systems and twinning are considered to yield
this result. Based on TEM work, Koike et al. [9] proposed
that the activities of dynamic recovery as well as non-basal
slip systems are important in enhancement of tensile ductil-
ity of the ECAPed Mg.
Fig. 5 shows the load vs. displacement measured during
micro-extrusion. The load increases at the beginning,
becomes saturated for a while and then increases again.
The load is larger as the extrusion temperature is lower.
Fig. 6 shows SEM micrographs of a micro-gear shaft
extruded from the ECAPed AZ 31 alloy. Microparts with
a height of 5 mm and a diameter of approximately
1.8 mm could be successfully extruded, as shown in
Fig. 6(a) and (b). The extruded gear shaft shows good
replication of the die dimension with high surface quality.
The presence of scratch lines is observed parallel to the
extrusion direction at a high magnication (insert in
Fig. 6(a)) and this reects the die-surface condition with
high roughness created during the EDM process.
The cross-section of the gear shaft extruded at 533 K
after chemical etching is shown in Fig. 7. The grain sizes
were measured on the cross-section. The tooth area that
must have experienced the most severe deformation during
micro-extrusion reveals the smallest grain size while the
center area that must have experienced the least deforma-
tion has the largest grain size. The measured grain size also
depended on the extrusion temperature. For 573 K, the
grain size at the tooth area is about equal to that of the
as-ECAPed material and the grain size at the center area
is even larger than this. For the lower extrusion tempera-
ture of 533 K, the grain sizes at the tooth and center areas
are 1.9 lm and 2.6 lm, respectively, which are notably less
than those of the as-ECAPed material. This result indicates
that lower extrusion temperature produces smaller grain
size, which is related to low grain growth rate at a low
temperature. The result of the grain size measurement is
summarized in Fig. 8.
Fig. 3. Photographs of the AZ31 (a) before ECAP and (b) after ECAP at 553 K by 6 passes.
0.0 0.1 0.2 0.3 0.4 0.5 0.6
0
50
100
150
200
250
300
Engineering Strain
6 passes (553K)
unECAPed
E
n
g
i
n
e
e
r
i
n
g

S
t
r
e
s
s
,

/
M
P
a
Fig. 4. Engineering stressengineering strain curves of the unECAPed and
ECAPed AZ31 alloys after 6 passes.
0 6
0
50
100
150
200
T= 573K
T= 533K
L
o
a
d

(
K
g
f
)
Displacement (mm)
AZ31(6 passes)
ram speed = 0.4mm/min
holding time =10min
8 2 4
Fig. 5. Load vs. displacement measured during micro-extrusion at 533
and 573 K.
W.J. Kim, Y.K. Sa / Scripta Materialia 54 (2006) 13911395 1393
The microhardness (H
V
) has been measured before and
after the micro-extrusion and the comparison is shown in
Fig. 9. The hardness diers depending on the position as
well as testing temperature. It was higher at the lower
extrusion temperature and highest at the tooth area. In
order to examine the HallPetch relationship, the micro-
hardness values of the micro-extruded gears in Fig. 9 were
plotted as a function of d
1/2
. This is shown in Fig. 10. The
microhardness data of the as-ECAPed alloy as well as the
ECAPed alloys annealed at several temperatures in the
range between 450 and 750 K for 1.8 ks, with the purpose
of increasing the grain size by static grain growth, were also
plotted. Both the ECAPed and micro-extruded alloys fol-
low the linear relationship described by Eq. (1):
H
V
H
0
K
H
d
1=2
1
Fig. 6. SEM micrographs of a micro-gear shaft extruded from the ECAPed AZ 31 alloy (a) side view (b) front view.
Fig. 7. The cross-section of the gear shaft extruded at 533 K after chemical etching (a) center region and (b) tooth region.
As-ECAPed 533K TOOTH 533K CENTER 573K TOOTH 573K CENTER
0
1
2
3
4
5
G
r
a
i
n

s
i
z
e

(

m
)
Material and Position
Fig. 8. The result of grain-size measurement.
As-ECAPed CENTER TOOTH
60
65
70
75
80
85
90
573 K
533 K
H
a
r
d
n
e
s
s

(
H
v
)
Position
Fig. 9. The microhardness (H
V
) measurement before and after micro-
extrusion.
1394 W.J. Kim, Y.K. Sa / Scripta Materialia 54 (2006) 13911395
with K
H
= 42.2 and H
0
= 40.0 for the ECAPed alloys, and
K
H
= 50.0 and H
0
= 47.4 for the micro-extruded alloys,
where H
0
and K
H
are the material constants. This result
indicates that the micro-extruded alloys are notably harder
than the ECAPed alloys when compared at the same grain
size. The texture dierence between the two groups is be-
lieved to have resulted in the strength dierence. The con-
tribution to H
V
hardness by grain size reduction and
texture modication during micro-extrusion can be evalu-
ated based on the two curves in Fig. 10(a). For example,
the H
V
hardness expected at the tooth area with the grain
size of 1.9 lm in the micro-extruded gear at 533 K is 70
according to the HallPetch relation for the ECAPed
alloys. This is the value obtained when it is assumed that
the H
V
increase after the micro-extrusion is wholly due to
the grain-renement. The experimentally measured H
V
value at the tooth area (=84.7) is, however, considerably
larger than this value, indicating that another strengthen-
ing factor should be taken into considered. Strengthening
caused by texture change during micro-extrusion is
believed to be the factor since texture is known to be very
inuential in the strength of the Mg alloys [4,5]. In fact, the
contribution of strengthening by grain size reduction
(DH
V
= 6.3) to the total strengthening (DH
V
= 21) after
the micro-extrusion is only 30%. This indicates that the
strengthening after the micro-extrusion at 533 K primarily
comes from the texture modication. For the case at
573 K, on the other hand, the strengthening seems to come
entirely from the texture modication since little grain size
reduction is accompanied with the micro-extrusion. It is
worthwhile noting that the hardness datum of the AZ31
alloy that was directly extruded after ECAP under hydro-
static pressure [8], and was proven to almost regain the
ber texture after the extrusion, falls onto the curve estab-
lished based on the data for the micro-extruded gears. This
indirectly supports the proposition that texture restoration
to ber texture takes place during the micro-extrusion
process. Therefore, it can be concluded that application
of micro-extrusion after ECAP to Mg alloys brings out
the normal grain size strengthening eect by restoring the
texture to the original state before ECAP.
The yield stress of the tooth area with the grain size of
1.9 lm (micro-extruded at 533 K), therefore, can be pre-
dicted by knowing the relationship between the yield stress
and grain size in the extruded AZ31 alloy. According to the
HallPetch relation between yield stress and d
1/2
for the
extruded materials shown in Fig. 10(b) [4], a high yield
stress of 380 MPa is predicted at 1.9 lm, indicating that a
very high strength Mg gear can be produced by combining
ECAP and micro-extrusion processes.
4. Conclusion
Micro-gear extrusion was performed on ECAPed AZ31
Mg alloys with ne grain size. High strength gears could be
produced by using ECAP combined with the extrusion
method: ECAP renes the microstructure while direct
extrusion restores the ECAP texture to the original state
before ECAP. It was found that the increase in hardness
during micro-extrusion primarily comes from the texture
restoration eect.
Acknowledgment
This work is supported by 21C Frontier R&D Program
Ministry of Science and Technology.
References
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[2] Mabuchi M, Ameyama K, Iwasaki H, Higashi K. Acta Mater
1999;47:2047.
[3] Lin HK, Huang JC, Langdon TG. Mater Sci Eng A 2005;402:250.
[4] Kim WJ, Jeong HT. Mater Trans 2005;46:251.
[5] Kim WJ, Hong SI, Kim YS, Min SH, Jeong HT, Lee JD. Acta Mater
2003;51:3293.
[6] Yamashita A, Horita Z, Langdon TG. Mater Sci Eng A 2001;300:142.
[7] Chuvildeev VN, Nieh TG, Gryaznov MY, Kopylov VI, Sysoev AN. J
Alloys Compd 2004;378:253.
[8] Kim WJ, unpublished work.
[9] Koike J, Kobayashi T, Mukai T, Watanabe H, Suzuki M, Maruyama
K, et al. Acta Mater 2003;51:2055.
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
0
50
100
150
200
250
300
350
400
Predicted strength
at the tooth area (533K)
=380 MPa
x
AZ31 extruded under
hydrostatic pressure
AZ31(extruded)
AZ31(extruded)
AZ61 (extruded)
0
.
2
%

P
r
o
o
f

S
t
r
e
s
s
,

y

/
M
P
a
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
40
50
60
70
80
90
As-ECAP (AZ31)
AZ31 extruded under
hydrostatic pressure
Micro-extruded gears (AZ31)
As-ECAP (AZ31) + annealing
H
v
d
-1/2
(m
-1/2
) d
-1/2
(m
-1/2
)
(a) (b)
Fig. 10. The microhardness of the micro-extruded gears and the as-ECAPed alloys as a function of d
1/2
.
W.J. Kim, Y.K. Sa / Scripta Materialia 54 (2006) 13911395 1395