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

properties of ECAE AZ61 Mg alloy have also been
Magnesium alloys have high potential as structural obtained [7]. Nevertheless, it is difficult to improve both
materials due to their high specific properties. However, the strength and the ductility of the ECAE Mg alloy,
magnesium alloys have poor formability and limited although the grain size can be refined significantly by
ductility at room temperature ascribed to their hexagonal ECAE processing.
close-packed (HCP) crystal structure. Grain refinement is Zan et al. [4] reported that the grain size of ECAE
an important practice used to improve the mechanical AZ31 Mg alloy decreased, the 0.2% proof stress increased,
properties of magnesium alloy. While equal channel but the elongation decreased when ECAE processing
angular extrusion (ECAE) provides a technique for temperature decreased. It is suggested that both the
producing ultra-fine grain sizes in the submicrometer or ductility and the yield stress of ECAE AZ31 alloy could
nanometer range in bulk materials [1,2]. Mabuchi et al. [3] be improved by lowering the processing temperature.
reported that fine-grain Mg alloy with a grain size of 1 Am However, it is limited to lowering the ECAE processing
has been obtained by ECAE. The microstructure and temperature for the Mg alloy. For example, AZ91 [3],
tensile properties of ECAE AZ31 Mg alloy were studied in AZ61 [7,8], AZ31B [9], and ZK60 [10] Mg alloys could
some articles [4–6], and the following common results only be ECAE-processed at the lowest temperatures of 473
were obtained, which were that the grains were refined K, 548 K, 473 K, and 433 K, respectively. ECAE has been
effectively, the elongation was improved, but the yield 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
T Corresponding author. School of Materials Science and Engineering,
Shanghai Jiao Tong University, Shanghai 200030, PR China. Tel.: +86 21 less than 1 Am. However, there was no report on the
62932544; fax: +86 21 62820892. mechanical property of subsequent processing at lower
E-mail address: [email protected] (D. Lin). temperature.
0167-577X/$ - see front matter D 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.matlet.2004.09.061
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 3. Results and discussion
two-step ECAE, was applied to improve both the strength
and the ductility of AZ31 Mg alloy. The processing 3.1. The microstructure and mechanical properties of ECAE
temperature of the second step could be lower than that of AZ31 alloy
first step in the two-step ECAE. Emphasis was placed on the
relationship between microstructure evolution and mechan- ECAE processing was carried out at the temperature
ical properties. 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
2. Experimental by ECAE at a constant temperature were named ECAE
alloy in this study. Fig. 1 shows the optical photographs of
The material used in the present study was a commercial as-received alloy, four-pass ECAE specimen processed at
Mg–Al–Zn alloy, AZ31, and was received as a commer- 523 K and at 498 K, respectively. The average grain sizes of
cially extruded bar with a grain size of 20 Am. The ECAE these AZ31 alloys were determined to be 20, 5, and 2 Am,
specimen was cut to 10 mm  10 mm  65 mm. ECAE was respectively. The refinement of the grain size after ECAE
carried out on the as-received material through a die made processing proves that the processing temperature is an
of H13 steel with an internal angle of 908 between the important factor used to control the microstructure of AZ31
vertical and horizontal channels. The strain intensity e n alloy, lower processing temperature, and finer grain size,
could be calculated by the equation: e n = 1.15Ncotan (//2) which is similar with the results in the previous reports
[12], where N is the pass number, so the strain of each pass [4–6]. The grains in the ECAE AZ31 alloy are equiaxed and
is 1.15. Graphite was used as lubricant. The ECAE homogeneously distributed, which suggests that recrystalli-
processing was carried out at the temperature ranging from zation took place during ECAE processing.
453 K to 573 K, with a constant processing rate of 16.8 Fig. 2 shows the stress–strain curves of as-received alloy,
mm/min, All processings were conducted by rotating each four-pass ECAE specimen processed at 523 K and at 498 K.
sample about the longitudinal axis by 908 in the same
direction between consecutive passes, designated as route
300
Bc [13]. Repetitive pressings of the same sample were
performed up to four or five passes, with a strain equivalent 250
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 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 2269

5µm 5µm

(a) 498K/5pass (b) 498K/4pass-453K/1pass

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 Fig. 3 shows the optical photographs of five-pass ECAE
at 523 K and 498 K increased to 35% and 32%, respectively, specimen processed at 498 K and two-step ECAE alloy at a
from 21% of as-received alloy, but their yield strength given strain of 5.75. Their grain sizes were determined to be
decreased to 113 MPa and 136 MPa from 153 MPa, 2 and 0.5 Am, respectively. So ultra-fine grains in
respectively. The plots indicate that the ductility of the submicrometer range can be produced by the two-step
AZ31 alloy is enhanced effectively, but its yield strength is ECAE by lower processing temperature. It should be noted
decreased markedly by ECAE processing even with the that the grains in the two-step ECAE AZ31 are not fully
grain refined effectively. So the ECAE temperature is an resolved by OM, indicating that it may not be fully
important factor to control the mechanical properties of the recrystallized. Further observations by TEM were carried
AZ31 Mg alloy at a given strain intensity e n . The higher is out to show microstructure evolution of the alloy during the
the processing temperature, the higher is the elongation but two-step processing.
the lower is the yield stress. Fig. 4 shows the TEM micrographs of as-received ECAE
and two-step ECAE alloys. In Fig. 4(a), there are a few
3.2. The microstructure and mechanical properties of two- dislocations in the interior of large grains and careful
step ECAE AZ31 alloy observation reveals that the grain boundaries are high angle
grain boundaries. In Fig. 4(b), there were also a few
The results in Figs. 1 and 2 indicate that the grain dislocations in the interior of grains in spite of large
refinement and the yield stress of ECAE AZ31 alloy have straining by ECAE and effective grain refining. Most of
been improved by lowering the processing temperature. In the grain boundaries are revealed to be high angle grain
this study, a new two-step ECAE was designed to lower the boundaries and fully defined subgrain boundaries, which
processing temperature for AZ31 alloy. Repetitive extru- suggests that dynamic recovery and recrystallization took
sions of the sample were performed up to four passes at 498 place during ECAE at 498 K. In Fig. 4(c), within grains and
K and continually performed one more pass at 453 K, and on the grain boundaries, many dislocations are visible, and
the sample processed by the procedure was named two-step there are incompletely developed subgrains and cell
ECAE alloy. structure formed by the tangled dislocations. It suggests

(a) (b) (c)

200nm 200nm 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.
2270 L. Jin et al. / Materials Letters 59 (2005) 2267–2270

350
subgrains and cell structure formed in the AZ31 alloy by
300
two-step ECAE, which probably results in increasing yield
stress of AZ31 Mg alloy. It indicates that the grain boundary
250 structure and dislocation substructure, besides grain size and
texture, play an important role on the mechanical properties
200 of AZ31 Mg alloy. It can be concluded that the two-step
Stress (MPa)

ECAE processing could optimize the microstructure and

150 C
A B improve the strength and ductility of the alloy.
100

50 A: As-received 4. Conclusion
B: ECAEed AZ31 alloy (498k/5pass)
0 C: Two-step ECAEed AZ31 alloy
(498k/4pass-453k/1pass) The processing temperature is an important factor that
affects the microstructure and mechanical properties of the
-50
-5 0 5 10 15 20 25 30 35 Mg alloy by ECAE. The two-step ECAE processing was
Strain (%) successfully applied to control the microstructure and
mechanical properties of the AZ31 alloy by lowering the
Fig. 5. Engineering stress–strain relations for the two-step ECAE AZ31 Mg
alloy.
processing temperature to 453 K. The ultra-fine grain of 0.5
Am has been obtained, and both the ductility and strength of
that dynamic recovery and recrystallization do not fully take the alloy were improved significantly after the processing,
place when the processing temperature decreases to 453 K which can be explained by grain refinement as well as
for the two-step ECAE AZ31 Mg alloy. incomplete dynamic recovery and recrystallization during
Fig. 5 shows the stress–strain curves of as-received alloy, the processing.
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 References
152 MPa. For the two-step ECAE alloy, the elongation
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