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Article history:
Received 16 February 2012
Accepted 27 August 2012
Available online 12 September 2012
Keywords:
Magnesium alloy
Squeeze casting
Cyclic properties
Low cycle fatigue
High cycle fatigue
a b s t r a c t
Cyclic deformation behavior and fatigue life of squeeze-cast AZ31 magnesium alloy was studied under
stress amplitude-control at room temperature. Low and high cycle fatigue tests with engineering stress
amplitudes in the range from 40 to 110 MPa were conducted. Analysis of hysteresis curves was performed. Tensioncompression asymmetry of hysteresis loops was not observed; the alloy exhibited cyclic
hardening in tension and compression. The fatigue life in the low cycle fatigue region was expressed by
Whler and derived MansonCofn curves. Experimental data in both, the low and high cycle fatigue
regions were tted by means of regression functions. SN curves exhibited a smooth transition from
the low to the high cycle fatigue regions and signicant scattering of experimental points was observed.
Furthermore, metallographic and fractographic analyses were performed. Crack initiation occurred from
the specimen surface or on clusters of secondary particles; the region of nal fracture was characterized
by a transgranular ductile fracture.
It can be concluded that the fatigue properties of squeeze cast magnesium alloy AZ31 are signicantly
improved comparing to materials prepared by common methods of casting. Squeeze casting also enables
the cost-effective fabrication of complicatedly shaped parts.
2012 Elsevier Ltd. All rights reserved.
1. Introduction
Magnesium alloys are increasingly used in the automotive and
aircraft industries. Reducing the weight of components while
maintaining good mechanical properties leads to reduced fuel consumption and more economical and environmentally-friendly
operation. To predict the behavior of the material under cyclic
loading, it is essential to describe the fatigue behavior of magnesium alloys in the low and high cycle regions.
The fatigue behavior of AZ31 magnesium alloy in the low and
high cycle regions has already been investigated in the literature.
However, there have only been limited studies on the fatigue
behavior of cast magnesium alloys. The low cycle fatigue behavior
of extruded AZ31 was studied using strain controlled pushpull
tests [1] and rotating bending fatigue tests [2]. Hasegawa et al.
[3] investigated the low cycle fatigue behavior of extruded AZ31
magnesium alloy using both, stress and strain controlled tests.
The authors examined the effect of mean stress and analyzed cyclic
stressstrain behavior. Stress and strain controlled fatigue tests of
different die cast magnesium alloys were alos performed by Sonsino and Dieterich [4]. The inuence of notches, mean stress, and
elevated temperatures was evaluated and compared to other structural materials. Zberov et al. [5] studied the tensile, low and high
cycle fatigue behavior of AZ31 magnesium alloy fabricated by
Corresponding author. Tel.: +420 54114 3147.
E-mail address: horynova@fme.vutbr.cz (M. Horynov).
0261-3069/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2012.08.079
squeeze casting (SC), hot rolling (HR), and equal channel angular
pressing (ECAP). The average grain size for SC was 450 lm; the
grain size for HR ranged from 3 to 20 lm, and the grain size for
ECAP ranged 12 lm; yield strength was 50 MPa for SC, 175 for
HR, and 115 for ECAP. The strong inuence of production procedure on fatigue properties was found. The fatigue limit of SC material was 40 MPa; HR and ECAP materials exhibited about 95 MPa.
Chamos et al. [6] investigated the tensile and fatigue behavior of
hot rolled AZ31 and AZ61 magnesium alloys. Longitudinal and
transverse directions were evaluated and the fracture surfaces of
specimens were examined. Matsuzuki and Horibe [7] studied the
inuence of heat treatment on the fatigue behavior of extruded
AZ31 magnesium alloy. Plastic strain controlled tests were conducted on as-extruded and annealed specimens. The fatigue life
of as-extruded material, was slightly longer than that of heat treated material. No other signicant difference was found in the
fatigue behavior of the experimental materials.
Casting is the most economical way to transform material into
shaped components. The major drawback of casting techniques is
the formation of defects such as porosity or segregation defects
that can be potential crack initiation sites during the life of the
component. New casting techniques such as squeeze casting have
been developed to minimize casting defects and related problems
[8,9].
Squeeze casting is a technique in which the material solidies
under high pressure and has signicant advantages such as an
improvement in mechanical properties and the possibility to
254
Nomenclature
a ()
tion behavior, and low and high cycle fatigue life were investigated
and compared to available data on AZ31 magnesium alloys prepared by different technologies.
2. Experimental details
2.1. Material and specimens
The experimental material used was AZ31 magnesium alloy
fabricated by squeeze casting at ZFW GmbH in Clausthal. The direct squeeze casting method was used: molten metal was
squeezed and solidied at a pressure of 150 MPa. The material
was supplied in the form of billet 200 mm in diameter and
40 mm in height. As squeeze casting is a method producing a ner
grain and more homogeneous structure than other casting methods, no additional heat treatment was performed. The chemical
composition measured by a Spectrumat GDS 750 optical emission
spectrometer with glow discharge is shown in Table 1. The basic
mechanical properties (Young0 s modulus, ultimate tensile strength,
proof stress and elongation), strain hardening coefcient and strain
hardening exponent established by means of tensile tests are given
in Table 2. Tensile tests were performed according to EN ISO 68921 [14] on a PC controlled testing device with a strain rate of
0.00025 s1 using cylindrical specimens with a diameter of 6 mm
and gauge length of 30 mm. Strain was measured by an axial
extensometer with a gauge length of 30 mm. A representative
engineering stressstrain curve is given in Fig. 1.
As shown in Fig. 2, cylindrical specimens of two different geometries were machined from experimental material and used for fatigue tests. The test specimens were machined so that the axes of
the samples were perpendicular to the axis of the billet. The surface of the gauge section was 0.4 Ra ground to remove the machining marks and to achieve a smooth surface.
2.2. Experimental procedure
Specimens for metallographic assessment were prepared in the
usual way and etched with a mixture of picric acid (5 ml acetic acid,
6 g picric acid, 10 ml water, and 100 ml ethanol). Microstructural
Table 1
Chemical composition of AZ31 alloy (wt.%).
Al
Zn
Mn
Si
Fe
Zr
Mg
2.86
1.07
0.35
0.005
0.004
0.01
Bal.
255
Table 2
Tensile properties of AZ31 alloy.
E (GPa)
Rp0.2 (MPa)
Rm (MPa)
A (%)
K (MPa)
40.66
55
174
8.8
404.8
0.32
3. Experimental results
3.1. Microstructure of AZ31 magnesium alloy
Fig. 3 shows the secondary electron micrograph of AZ31 magnesium alloy and elemental maps measured by energy-dispersive Xray spectroscopy. According to the results of local analysis of
chemical composition (Table 2), the structure of AZ31 alloy is
formed by the solid solution d phase, the intermetallic c phase
(Mg17Al12) and the intermetallic u phase (Mg21(Al, Zn)17), eutectic
(d + c), and AlMn-based particles.
Several differently shaped AlMn particles were analyzed.
According to the AlMn binary phase diagram [17], a Mn content
of between 34 and 39.5 at.% corresponds to the c2 phase (Al8Mn5). The calculated Al/Mn ratio of 1.7 0.2 also indicates that
these particles are most likely Al8Mn5.
The material is heterogeneous; it is evident from the analysis of
element distribution (Fig. 3) that there is an Al- and Zn-rich d phase
along the grain boundaries. The difference in aluminum content
between the d phase and enriched d phase was about 3 at.%. The
average grain size of the material was about 50 lm.
3.2. Cyclic plasticity and low-cyclic fatigue
Fig. 2. Shape and dimension of specimens for (a) high-resonance pulsator and (b)
servo-hydraulic testing system.
VH
W
4eap ra
Fig. 6 shows the evolution of plastic strain amplitude with number of cycles at different stress amplitudes; the evolutions of total
and mean strain are illustrated in Figs. 7 and 8, respectively. A
change of 5% in the effective modulus was used as a criterion for
determining Nf.
256
Fig. 3. (a) Secondary electron micrograph of AZ31 magnesium alloy and elemental distribution maps measured by energy-dispersive X-ray spectroscopy: (b) Al, (c) Mn, (d)
Zn, (e) EDX spot analysis of AlMn based particle.
257
Fig. 4. Hysteresis loops for (a) 65 MPa and (b) 110 MPa. Cycle No. 20000 (65 MPa)
and 800 (110 MPa) roughly correspond to Nf/2.
Fig. 7. Evolution of total strain in engineering stress controlled low cycle fatigue
tests.
Fig. 5. Dependence of hysteresis loop area W, plastic strain amplitude eap and loop
shape parameters VH on number of cycles. Each set of symbols represents different
stress amplitude.
ra K 0 enap
2
0
R0p0:2 K 0 0:002n
r
r
er
r0
E
m
4
Fig. 8. Evolution of mean strain in engineering stress controlled low cycle fatigue
tests.
eat, plastic strain amplitude eap, and elastic strain amplitude eae
on the number of cycles to failure (Fig. 11). The material parameters found by the tting procedure are summarized in Table 5. Furthermore, the transition number of cycles was also established
(Nt = 1025). The intersection of plastic and elastic strain amplitude
dependence on number of cycles is located in the region that is not
covered by experimental data. The amplitudes of elastic and plastic
strain were therefore extrapolated to Nf = 200. The value of the
plastic strain amplitude eap = 6 106 for 107 cycles was obtained
from Eq. (6).
ra r0f 2Nf b
258
ra a Nbf r1
ra r1
Fig. 9. (a) Cyclic deformation curve in loglog coordinates (b), comparison of static
tensile curve and cyclic stressstrain curve tted to RambergOsgood function.
Table 3
Composition of constituent phases in squeeze cast AZ31 magnesium alloy (at.%).
d phase
c phase Mg17Al12
u phase Mg21(Al, Zn)17
AlMn particle
Mg
Al
Mn
Zn
98.72
77.11
75.22
63.46
1.14
21.42
19.24
24.02
0.04
12.52
0.10
1.47
5.54
Table 4
Summary of material parameters.
Power law
0
RambergOsgood function
0
K (MPa)
445.1
0.23
R0p0:2
(MPa)
106
r0 (MPa)
R00p0:2 (MPa)
469
4.03
101
r0 f
E
6
7
Nf
Nf C
8
b
9
Fig. 11. Dependence of total strain amplitude eat, plastic strain amplitude eap, and
elastic strain amplitude eae on the number of cycles in loglog coordinates.
Table 5
Low cycle fatigue parameters.
r0f (MPa)
e0f
410.52
0.169
1.45
0.729
a
b
C
r1 (MPa)
S
Stromayer
Kohout-Vechet
1075.3
0.38
43.3
1473.5
0.17
2.03 105
45.8
1531.5
259
260
Fig. 13. Inuence of stress amplitude on characteristics of fracture surface of AZ31 magnesium alloy. Initiation sites are marked by arrows, dashed line indicates the
transition between propagation area and area of nal fracture.
c-axis is parallel to the tensile axis or perpendicular to the compression axis [3640].
As only pyramidal slip, which is in magnesium alloys activated
at about 200 C [38,41,42], can fulll the Von Misses criterion without the activation of other deformation modes, various primary
and secondary slip and twinning mechanisms can and have to be
activated at the same time at room temperature [4345]. Evidence
of pyramidal slip at room temperature was found for MgLi single
crystal by Agnew et al. [36] and Ando and Tonda [46]. As single
crystal was strained along the direction, the Schmid factors for basal and pyramidal II slip were nearly identical and pyramidal slip
occurred at room temperature. For polycrystalline magnesium
and its alloys, combinations of other deformation modes were observed at room temperature. Gharghouri et al. [37] observed basal
slip and tensile and compressive twining for Mg7.7Al. Basal slip
with tensile twinning was reported for AM60 [42], AZ31 [47] and
also for pure Mg [40]. Basal slip and tensile twining were considered as major deformation modes for extruded AZ31 magnesium
alloy [39]. Only in the case that the c-axis was nearly perpendicular
to the loading direction, the Schmid factors of the three basal slip
systems is so small, that prismatic and pyramidal I slip system
could be additionally activated. Basal slip and twining can therefore be considered as the most important deformation modes at
room temperature for polycrystalline magnesium alloys with randomly oriented grains.
Symmetric hysteresis curves with respect to tension and compression are typical for deformation predominantly accomplished
by means of dislocation slip [48]. On the other hand, asymmetric
and sigmoidal-shaped curves are the result of mechanical twining
[49].
At all stress amplitudes, except for the rst cycles at higher
stress amplitudes, hysteresis loops were symmetric, which suggests slip-dominated plastic deformation. Hasegawa et al. [3] reported asymmetric hysteresis curves until half-life using the
stress control mode and asymmetry until the end of the test for
the strain control mode. Since stress control mode tests are not frequently used, the shape of hysteresis curves were further discussed
with strain control mode fatigue test results.
261
Fig. 14. (a) Secondary electron micrograph of fatigue fracture surface with initiation site on cluster of secondary particles, (b) back-scattered electron micrograph of initiation
site, (c) more detailed back-scattered electron micrograph of area with AlMn based particles, and (d) EDX spot analysis of area with AlMn based particles.
Fig. 15. Secondary electron micrographs of fatigue fracture surfaces of sample loaded with stress amplitude of 65 MPa. (a) Initiation site, (b) beginning of propagation area,
(c) striations, and (d) region of nal fracture.
262
Fig. 16. Secondary electron micrographs of fatigue fracture surfaces of sample loaded with stress amplitude of 110 MPa (a) initiation site, (b) beginning of propagation area
with secondary crack, (c) striations, and (d) region of nal fracture.
The values of fatigue limits for 108 cycles were basically the
same when tted to each function. The value of the fatigue limit
(rc = 45 MPa) and the fatigue ratio (rc/Rm = 0.26) were slightly
higher than those reported for squeeze-cast AZ31 magnesium
alloy by Zberov et al. [5]. Comparing to AZ type magnesium
alloys prepared by common methods of casting, the value of
fatigue limit of our experimental material is signicantly higher
263
The fracture surfaces of selected specimens were examined. Fatigue cracks initiated from the specimen surface or from the clusters of AlMn based particles. Those clusters were observed along
the longitudinal section of the fatigued specimen and because
there was no evidence of fatigue cracks near the non-surface clusters, we can conclude, that those clusters act as initiation sites only
when placed at specimen surface. This is in agreement with nding
of Patel et al. [32] who reported near surface AlMn particle in
AZ91 magnesium alloy which did not act as an initiation site. Documented fatigue crack initiated at a free surface and changed its
direction when reached AlMn particle.
Initiation sites of examined samples were mostly similar, characterized by cleavage-like facets and in some cases by ratchet
marks. As ratchet marks indicate relatively high stresses, its presence was observed only for specimen tested at 110 MPa.
Ridges parallel to the crack propagation direction which have
been observed at the beginning of the crack propagation areas
are most probably formed by local shears that merge plateaus corresponding to different fracture plains in individual grains [58].
5. Conclusions
Low and high cycle engineering stress controlled fatigue tests
were conducted on AZ31 magnesium alloy fabricated by squeeze
casting. The microstructure, cyclic deformation behavior, and low
and high cycle fatigue life were investigated and compared to
available data on AZ31 magnesium alloys prepared by different
264
Acknowledgments
The work was nanced by the Czech Science Foundation, Project No. 101/09/P576 and was also carried out in the frame of the
NETME centre supported by the European Regional Development
Fund and CEITEC Central European Institute of Technology with
research infrastructure supported by the Project CZ.1.05/1.1.00/
02.0068 nanced from the European Regional Development Fund.
The authors would also like to thank Prof. Tom Kruml for
helpful discussion.
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