Materials Letters 59 (2005) 2267 – 2270

www.elsevier.com/locate/matlet

Mechanical properties and microstructure of AZ31 Mg alloy processed

by two-step equal channel angular extrusion
Li Jina,b, Dongliang Lina,b,T, Dali Maoa,b, Xiaoqing Zenga,c, Wenjiang Dinga,c
a
School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200030, PR China
b
Open Laboratory of the Educational Ministry for High Temperature Materials and Tests, Shanghai Jiao Tong University, Shanghai 200030, PR China
c
National Engineering Research Center of Light Alloys Net Forming, Shanghai Jiao Tong, University, Shanghai 200030, PR China

Received 16 September 2004; accepted 17 September 2004

Available online 28 March 2005

Abstract

A new equal channel angular extrusion (ECAE) processing, two-step ECAE, was applied to control the microstructure and mechanical
properties of AZ31 Mg alloy. The ultra-fine grain size of 0.5 Am has been produced, and both the ductility and yield stress of the alloy were
significantly increased after the processing, which is ascribed to grain refinement as well as incomplete dynamic recovery and
recrystallization during the second-step ECAE at 453 K.
D 2005 Elsevier B.V. All rights reserved.

Keywords: Mechanical properties; Microstructure; Equal channel angular extrusion (ECAE); AZ31 Mg alloy

1. Introduction stress decreased. Similar results about the mechanical

Magnesium alloys have high potential as structural
materials due to their high specific properties. However,
magnesium alloys have poor formability and limited
ductility at room temperature ascribed to their hexagonal
close-packed (HCP) crystal structure. Grain refinement is
an important practice used to improve the mechanical
properties of magnesium alloy. While equal channel
angular extrusion (ECAE) provides a technique for
producing ultra-fine grain sizes in the submicrometer or
nanometer range in bulk materials [1,2]. Mabuchi et al. [3]
reported that fine-grain Mg alloy with a grain size of 1 Am
has been obtained by ECAE. The microstructure and
tensile properties of ECAE AZ31 Mg alloy were studied in
some articles [4–6], and the following common results
were obtained, which were that the grains were refined
effectively, the elongation was improved, but the yield
T Corresponding author. School of Materials Science and Engineering,
Shanghai Jiao Tong University, Shanghai 200030, PR China. Tel.: +86 21
62932544; fax: +86 21 62820892.
E-mail address: dllin@sjtu.edu.cn (D. Lin).
0167-577X/$ - see front matter D 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.matlet.2004.09.061
properties of ECAE AZ61 Mg alloy have also been
obtained [7]. Nevertheless, it is difficult to improve both
the strength and the ductility of the ECAE Mg alloy,
although the grain size can be refined significantly by
ECAE processing.
Zan et al. [4] reported that the grain size of ECAE
AZ31 Mg alloy decreased, the 0.2% proof stress increased,
but the elongation decreased when ECAE processing
temperature decreased. It is suggested that both the
ductility and the yield stress of ECAE AZ31 alloy could
be improved by lowering the processing temperature.
However, it is limited to lowering the ECAE processing
temperature for the Mg alloy. For example, AZ91 [3],
AZ61 [7,8], AZ31B [9], and ZK60 [10] Mg alloys could
only be ECAE-processed at the lowest temperatures of 473
K, 548 K, 473 K, and 433 K, respectively. ECAE has been
investigated by Yoshida et al. [11] for AZ61 at 473 K for
two passes and at 448 K for four passes to lower the
processing temperature and to obtain a finer grain size of
less than 1 Am. However, there was no report on the
mechanical property of subsequent processing at lower
temperature.
2268 L. Jin et al. / Materials Letters 59 (2005) 2267–2270

10µm 10µm 10µm

(a) As-received (b) 523K/4pass (c) 498K/4pass

Fig. 1. The optical photographs of as-received AZ31 alloy and ECAE AZ31 alloy. (a) As-received; (b) 523 K/4 pass; (c) 498 K/4 pass.

In this study, a new ECAE processing procedure, named
two-step ECAE, was applied to improve both the strength
and the ductility of AZ31 Mg alloy. The processing
temperature of the second step could be lower than that of
first step in the two-step ECAE. Emphasis was placed on the
relationship between microstructure evolution and mechan-
ical properties.
2. Experimental
The material used in the present study was a commercial
Mg–Al–Zn alloy, AZ31, and was received as a commer-
cially extruded bar with a grain size of 20 Am. The ECAE
specimen was cut to 10 mm  10 mm  65 mm. ECAE was
carried out on the as-received material through a die made
of H13 steel with an internal angle of 908 between the
vertical and horizontal channels. The strain intensity e n
could be calculated by the equation: e n = 1.15Ncotan (//2)
[12], where N is the pass number, so the strain of each pass
is 1.15. Graphite was used as lubricant. The ECAE
processing was carried out at the temperature ranging from
453 K to 573 K, with a constant processing rate of 16.8
mm/min, All processings were conducted by rotating each
sample about the longitudinal axis by 908 in the same
direction between consecutive passes, designated as route
Bc [13]. Repetitive pressings of the same sample were
performed up to four or five passes, with a strain equivalent
to 4.6 or 5.75. The flat tensile specimens with a gauge
section of 10 mm  3 mm  1.5 mm were cut from the
3. Results and discussion
3.1. The microstructure and mechanical properties of ECAE
AZ31 alloy
ECAE processing was carried out at the temperature
ranging from 473 K to 573 K for the as-received alloy in our
study. However, cracks appeared when the processing
temperature was lower than 498 K. The samples processed
by ECAE at a constant temperature were named ECAE
alloy in this study. Fig. 1 shows the optical photographs of
as-received alloy, four-pass ECAE specimen processed at
523 K and at 498 K, respectively. The average grain sizes of
these AZ31 alloys were determined to be 20, 5, and 2 Am,
respectively. The refinement of the grain size after ECAE
processing proves that the processing temperature is an
important factor used to control the microstructure of AZ31
alloy, lower processing temperature, and finer grain size,
which is similar with the results in the previous reports
[4–6]. The grains in the ECAE AZ31 alloy are equiaxed and
homogeneously distributed, which suggests that recrystalli-
zation took place during ECAE processing.
Fig. 2 shows the stress–strain curves of as-received alloy,
four-pass ECAE specimen processed at 523 K and at 498 K.
300
250
200
stress (MPa)

sample produced by ECAE with electro-discharge machine. B

C
Tensile tests were carried out in 5  10 4 s 1 at room 150
A
temperature. Microstructures of the samples were examined
100
by optical microscope (OM) after mechanical polishing and A As-received alloy
etching at room temperature using a solution of 1% HNO3, 50 B ECAE 4 pass at 523k
24% C2H6O2, and 75% water. For transmission electron C ECAE 4 pass at 498k
microscopy (TEM), disks were thinned at 233 K with a 0
twin-jet polisher under conditions of 10 mA and 75 V using
-5 0 5 10 15 20 25 30 35 40
a solution of 1% HClO4 in ethanol. The thinned specimens
strain (%)
were examined using a JEM-100 electron microscope
operating at 120 kV. Fig. 2. Engineering stress–strain relations for the AZ31 Mg alloy.
 L. Jin et al. / Materials Letters 59 (2005) 2267–2270
5µm
(a) 498K/5pass
Fig. 3. The optical photographs of ECAE AZ31 Mg alloy by two-step ECAE. (a) 498 K/5 pass; (b) 498 K/4 pass–453 K/1 pass.
The elongation of the four-pass ECAE specimen processed
at 523 K and 498 K increased to 35% and 32%, respectively,
from 21% of as-received alloy, but their yield strength
decreased to 113 MPa and 136 MPa from 153 MPa,
respectively. The plots indicate that the ductility of the
AZ31 alloy is enhanced effectively, but its yield strength is
decreased markedly by ECAE processing even with the
grain refined effectively. So the ECAE temperature is an
important factor to control the mechanical properties of the
AZ31 Mg alloy at a given strain intensity e n . The higher is
the processing temperature, the higher is the elongation but
the lower is the yield stress.
3.2. The microstructure and mechanical properties of two-
step ECAE AZ31 alloy
The results in Figs. 1 and 2 indicate that the grain
refinement and the yield stress of ECAE AZ31 alloy have
been improved by lowering the processing temperature. In
this study, a new two-step ECAE was designed to lower the
processing temperature for AZ31 alloy. Repetitive extru-
sions of the sample were performed up to four passes at 498
K and continually performed one more pass at 453 K, and
the sample processed by the procedure was named two-step
ECAE alloy.
(a) (b)
200nm
Fig. 4. The TEM photographs of (a) as-received alloy; (b) AZ31 alloy after ECAE: 498 K/5 passes; and (c) AZ31 alloy after two-step ECAE: 498 K/4 pass–453
K/1 pass.
2269
5µm
(b) 498K/4pass-453K/1pass
Fig. 3 shows the optical photographs of five-pass ECAE
specimen processed at 498 K and two-step ECAE alloy at a
given strain of 5.75. Their grain sizes were determined to be
2 and 0.5 Am, respectively. So ultra-fine grains in
submicrometer range can be produced by the two-step
ECAE by lower processing temperature. It should be noted
that the grains in the two-step ECAE AZ31 are not fully
resolved by OM, indicating that it may not be fully
recrystallized. Further observations by TEM were carried
out to show microstructure evolution of the alloy during the
two-step processing.
Fig. 4 shows the TEM micrographs of as-received ECAE
and two-step ECAE alloys. In Fig. 4(a), there are a few
dislocations in the interior of large grains and careful
observation reveals that the grain boundaries are high angle
grain boundaries. In Fig. 4(b), there were also a few
dislocations in the interior of grains in spite of large
straining by ECAE and effective grain refining. Most of
the grain boundaries are revealed to be high angle grain
boundaries and fully defined subgrain boundaries, which
suggests that dynamic recovery and recrystallization took
place during ECAE at 498 K. In Fig. 4(c), within grains and
on the grain boundaries, many dislocations are visible, and
there are incompletely developed subgrains and cell
structure formed by the tangled dislocations. It suggests
(c)
200nm 200nm
2270 L. Jin et al. / Materials Letters 59 (2005) 2267–2270
350
300
250
200
Stress (MPa)
150
A B
100
50 A: As-received
B: ECAEed AZ31 alloy (498k/5pass)
0 C: Two-step ECAEed AZ31 alloy
(498k/4pass-453k/1pass)
-50
-5 0 5 10 15 20 25
Strain (%)
Fig. 5. Engineering stress–strain relations for the two-step ECAE AZ31 Mg
alloy.
that dynamic recovery and recrystallization do not fully take
place when the processing temperature decreases to 453 K
for the two-step ECAE AZ31 Mg alloy.
Fig. 5 shows the stress–strain curves of as-received alloy,
ECAE alloy, and two-step ECAE alloy. For the ECAE alloy,
the elongation increases to 34% from 21% of as-received
alloy; however, the yield stress decreases to 104 MPa from
152 MPa. For the two-step ECAE alloy, the elongation
increases to 29% from 21% of as-received alloy, and the
yield stress increases to 231 MPa from 152 MPa. It can be
concluded that for the AZ31 alloy, both the ductility and
yield stress can be improved significantly by two-step
ECAE processing.
The mechanical properties of ECAE Mg alloy were
controlled by the microstructure of the alloy, including grain
size, grain boundary structure, dislocation structure, and
texture. At present, a well-accepted idea is that texture
modification plays an important role in increasing the
ductility of ECAE Mg alloy [5,14,15]. However, the factors
affecting the strength of ECAE Mg alloys are not clear and
should be clarified. According to the results in Figs. 4 and 5,
the mechanical properties of AZ31 Mg alloy were affected
by the grain boundary structure and dislocation distribution.
For ECAE AZ31, after five ECAE passes at 498 K, the
ductility was increased but the yield stress decreased
effectively with grain refinement. However, for two-step
ECAE AZ31 alloy, after four ECAE passes at 498 K and
then one pass at 453 K, the grain size was finer than that of
ECAE alloy after four ECAE passes at 498 K, but the yield
stress was improved markedly with a slight decrease of
ductility. Moreover, a lot of incompletely developed
subgrains and cell structure formed in the AZ31 alloy by
two-step ECAE, which probably results in increasing yield
stress of AZ31 Mg alloy. It indicates that the grain boundary
structure and dislocation substructure, besides grain size and
texture, play an important role on the mechanical properties
of AZ31 Mg alloy. It can be concluded that the two-step
ECAE processing could optimize the microstructure and
C
improve the strength and ductility of the alloy.
4. Conclusion
The processing temperature is an important factor that
affects the microstructure and mechanical properties of the
30 35 Mg alloy by ECAE. The two-step ECAE processing was
successfully applied to control the microstructure and
mechanical properties of the AZ31 alloy by lowering the
processing temperature to 453 K. The ultra-fine grain of 0.5
Am has been obtained, and both the ductility and strength of
the alloy were improved significantly after the processing,
which can be explained by grain refinement as well as
incomplete dynamic recovery and recrystallization during
the processing.
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