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Optimization of Mn content for high strengths in high-speed extruded Mg-

0.3Al-0.3Ca(wt.%) dilute alloy

Article  in  Materials Science and Engineering A · July 2016

DOI: 10.1016/j.msea.2016.07.098

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 Materials Science & Engineering A 673 (2016) 443–449

Contents lists available at ScienceDirect

Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Optimization of Mn content for high strengths in high-speed extruded

Mg-0.3Al-0.3Ca (wt%) dilute alloy
T. Nakata a,n, C. Xu a, Y. Matsumoto b, K. Shimizu b, T.T. Sasaki c, K. Hono c, S. Kamado a
a
Nagaoka University of Technology, 1603-1, Kamitomioka, Nagaoka 940-2188, Japan
b
Sankyo Tateyama, Inc. Sankyo Material-Company, 8-3, Nagonoe, Imizu, Toyama 934-8515, Japan
c
National Institute for Materials Science, 1-2-1 Sengen, Tsukuba 305-0047, Japan

art ic l e i nf o a b s t r a c t

Article history: The effect of Mn content on mechanical properties and microstructure of Mg-0.3Al-0.3Ca-xMn (wt%,
Received 27 June 2016 x¼ 0, 0.2, 0.4, 0.8) dilute alloys extruded at a high die-exit speed of 60 m/min has been investigated. The
Received in revised form strengths of the as-extruded samples increased with increasing Mn content, and Mg-0.3Al-0.3Ca-0.8Mn
22 July 2016
(AXM030308) alloy exhibited the highest 0.2% proof stress of 190 MPa. This is due to the formation of
Accepted 23 July 2016
fine and strongly textured grain structure as well as the dispersion of high number density of Al-Mn
Available online 25 July 2016
particles. Subsequent solution treatment and peak aging resulted in further increase in strength. High
Keywords: number density of Guinier Preston zones (G.P. zones) were dispersed within fine grains with their [0001]
Mg-Al-Ca-Mn alloy axis normal to the extrusion direction in the peak aged Mg-0.3Al-0.3Ca-0.4Mn (AXM030304) alloy, ex-
High-speed extrusion
hibiting the highest 0.2% proof stress of 220 MPa with reasonable tensile ductility of 22%, which are
Particle pinning
superior to those of a peak aged 6063 aluminum alloy.
Aging
Tensile property & 2016 Elsevier B.V. All rights reserved.

1. Introduction 0.5Al-0.1Mn [12–15]. Although the Mg-0.5Al-0.1Mn dilute alloy

Achieving high strengths in wrought magnesium (Mg) alloys
receives intense research interest because the application of
lightweight magnesium alloys to transportation vehicles is ex-
pected to reduce the emission of greenhouse effect gas through
their weight reduction. Although high tensile 0.2% proof stress
(hereafter, proof stress) over 300 MPa has been demonstrated in
Mg-Al, Mg-Zn, and Mg-Sn based alloys [1–11], such high strength
was obtained through the grain refinement by severe plastic de-
formation or extrusion at very low die-exit speeds. Because these
processing routes are industrially unfavorable due to their high
processing cost, there is a strong demand for the development of
high strength wrought Mg alloys, which has the hot workability
equivalent to those of 6000 series aluminum (Al) alloys.
The extrudability of Mg alloys can be improved by dilution of
the alloying elements. This is mainly because of the elimination of
the secondary phases with low melting temperature that sig-
nificantly deteriorate the extrudability of Mg alloys. The maximum
die-exit speed could be increased from 20 to 70 m/min by diluting
the alloy compositions from Mg-2.0Al-0.5Zn-0.2Mn (wt%) to Mg-
n
Corresponding author.
E-mail address: s123055@stn.nagaokaut.ac.jp (T. Nakata).
has comparable hot workability to 6000 series Al alloys, such high-
speed extrusion leads to the formation of the coarse grain struc-
ture causing the low strength [15]. The Mg-0.5Al-0.1Mn alloy ex-
truded at high speed exhibited much lower proof stress of only
140 MPa than those of peak aged 6063 Al alloy extruded at high-
speed, 215 MPa [16], and commercial Mg-3Al-1Zn alloy, 160 MPa
[15]. To overcome this problem, we have recently developed a
precipitation hardenable Mg-0.30Al-0.21Ca-0.47Mn alloy, which is
extrudable at a high die-exit speed of 60 m/min. By a peak aging
right after the extrusion, the proof stress of this particular alloy
can be increased to 206 MPa, which is higher than that of com-
mercial Mg-3Al-1Zn alloy (AZ31) [17]. However, the strength is
still lower than that of the aged 6000 series Al alloys due to its
coarse grain structure and deficient age hardening [16,17]. The
addition of Mn leads to the formation of Al-Mn particles, which are
known to work as grain growth inhibitor [18,19]. However, the
formation of the Al-Mn particles would degrade the age hardening
response in the Mg-Al-Ca-Mn dilute alloy since Al atoms that are
used to form G.P. zones are decreased by the Mn addition.
Therefore, the Mn content should be optimized to obtain a rea-
sonable age hardening response and fine grain structure in the
Mg-Al-Ca-Mn dilute alloy system. In this work, we have in-
vestigated the effect of Mn on the age-hardening response, tensile
property, and microstructure of high-speed extruded Mg-0.3Al-

http://dx.doi.org/10.1016/j.msea.2016.07.098
0921-5093/& 2016 Elsevier B.V. All rights reserved.
444 T. Nakata et al. / Materials Science & Engineering A 673 (2016) 443–449
0.3Ca-xMn (AXM0303xx) alloys.
2. Experimental procedure
Alloy ingots with 55 mm in diameter were prepared by a direct
chill casting. The alloy nomenclatures and chemical compositions
are summarized in Table 1 in both wt% and at%. These alloys were
homogenized at 450 °C for 1 h in an electronic furnace under an Ar
atmosphere, followed by water quenching. An indirect extrusion
was carried out at 400 °C at a die-exit speed of 60 m/min with an
extrusion ratio of 20 without any lubricant. The as-extruded
samples were subjected to a solution treatment at 500 °C for
10 min in an electronic furnace, followed by water quenching. An
artificial aging was done at 200 °C in an oil bath, and the variations
in the hardness were measured by a Vickers hardness tester
(Mitsutoyo, HM-221). Mechanical properties of the as-extruded
and peak-aged samples were evaluated by room temperature
tensile tests at an initial strain rate of 10  3 s  1 along the extrusion
direction using specimens with 4 mm in diameter and 22 mm in
gage length. Microstructure and texture were characterized by a
scanning electron microscope (SEM), JSM-7000F and TSL EBSD
apparatus. Transmission electron microscope (TEM) analyses were
done using FEI Tecnai 20, JEM-2100F, and Titan G2 80-200 with
energy dispersive spectroscopy (EDS) detector. Thin foils for the
TEM observations were prepared by punching 3 mm diameter
discs and twin-jet electro polishing using a solution of 5.3 g LiCl,
11.16 g Mg(ClO4)2, 500 ml methanol, and 100 ml 2-butoxy-ethanol
at about 45 °C with a voltage of 90 V. The thickness of the thin
foils were determined by the convergent beam electron diffraction
method [20].
3. Results
Fig. 1 shows surfaces of the (a) AX0303, (b) AXM030302,
(c) AXM030304, and (d) AXM030308 extruded bars. While the
surface of the Mn-free AX0303 alloy is severely cracked after the
extrusion (Fig. 1(a)), the surface quality is substantially improved
by the trace addition of Mn; the addition of 0.2% Mn improves the
surface quality, and the crack-free surface is formed by the addi-
tion of 0.8%Mn. Hereafter, the results of the AXM030302,
AXM030304 and AXM030308 alloys will be presented.
Fig. 2 shows variations in Vickers hardness of the AXM030302,
AXM030304, and AXM030308 alloys as functions of aging time at
200 °C. Note that As-ext. and S.T. in Fig. 2 stand for the as-extruded
and solution-treated conditions. The AXM030302 alloy reaches its
peak hardness of 5971 HV with a hardness increment of 16 HV.
Although the AXM030304 alloy reaches the similar peak hardness
of 59 71 HV as the AXM030302 alloy, the hardness increment is
8 HV, which is lower than that in the AXM030302 alloy. The ad-
dition of 0.8% Mn results in further decrease in the age hardening
response. The AXM030308 alloy shows hardness increment of
only 2 HV. However, all samples reach their peak hardness at 8 h,
which means that the Mn addition does not affect the time to
reach the peak hardness.
Table 1
Nomenclatures and chemical compositions of the alloy ingots [wt% (at%)].
Alloy Al Ca Mn
AX0303 0.32 (0.29) 0.32 (0.19) – Bal.
AXM030302 0.33 (0.30) 0.34 (0.20) 0.24 (0.11)
AXM030304 0.34 (0.32) 0.32 (0.19) 0.43 (0.19)
AXM030308 0.30 (0.27) 0.31 (0.19) 0.84 (0.37)
Fig. 3 shows tensile stress-strain curves of the (a) as-extruded
and (b) peak-aged AXM030302, AXM030304, and AXM030308
alloys, and Table 2 summarizes the proof stresses, ultimate tensile
strengths, and ductility. In the as-extruded condition, the proof
stress and ultimate tensile strength increase with increasing the
Mn content while the ductility decreases. The AXM030302 alloy
shows the lowest proof stress and ultimate tensile strength of
136 MPa and 203 MPa while it exhibits the largest ductility of 29%.
The as-extruded AXM030304 alloy shows the 0.2% proof stress of
167 MPa and the ultimate tensile strength of 220 MPa, and the as-
extruded AXM030308 alloy exhibits the highest 0.2% proof stress
of 190 MPa and ultimate tensile strength of 229 MPa. The ductility
of both AXM030304 and AXM030308 alloys are 24%, which are
slightly lower than that of the AXM030302 alloy. The peak-aging
increases the proof stresses and the ultimate tensile strengths in
the AXM030302 and AXM030304 alloys (Table 2); the
AXM030302 alloy exhibits the proof stress of 188 MPa and the
ultimate tensile strength of 247 MPa, and the AXM030304 alloy
shows the highest proof stress and ultimate tensile strength of 220
and 264 MPa, respectively. The peak-aged AXM030302 and
AXM030304 alloys show the satisfactory ductility of 27% and 22%,
respectively. However, the AXM030308 alloy shows only a slight
increase in proof stress and ultimate tensile strength by the peak
aging due to the small hardness increment; the proof stress and
ultimate tensile strength are 199 and 243 MPa, which are low
compared to those of the peak-aged AXM030304 alloy. The duc-
tility of the peak-aged AXM030308 alloy is almost the same as that
of the peak-aged AXM030304 alloy, 22%.
Fig. 4 shows inverse pole figure maps of the (a) as-extruded
and (b) solution-treated AXM030302, AXM030304, and
AXM030308 alloys taken from the planes parallel to the extrusion
direction. In the as-extruded samples, the microstructure mainly
consists of recrystallized grains with equi-axed shape. The grain
size of the AXM030302 alloy is about 22 mm, while the
AXM030304 and AXM030308 alloys have finer grain size of 11 mm
and 13 mm, respectively. In the AXM030308 alloy, there is a small
volume fraction of unrecrystallized grains, which are elongated
along the extrusion direction. Interestingly, all the alloys do not
show significant grain growth even after the solution treatment at
500 °C. The grain sizes of AXM030302, AXM030304 and
AXM030308 alloys are 21, 10 and 12 mm.
Fig. 5 shows inverse pole figures of the (a) as-extruded and
(b) solution-treated AXM030302, AXM030304, and AXM030308
alloys analyzed from the planes normal to the extrusion direction.
The texture observed in the as-extruded conditions did not change
by the solution treatment. In the as-extruded condition, the
AXM030302 alloy has o10 1̄1 4 and o11 2̄2 4 components,
which are often observed in extruded Mg alloys containing rare
earth elements and/or Ca [21–24]. The o10 1̄0 4 and o11 2̄0 4
components are observed in the inverse pole figures of the
AXM030304 and AXM030308 alloys. This means that the [0001]
directions in the AXM030304 and AXM030308 alloys are more
strongly aligned normal to the extrusion direction compared to the
AXM030302 alloy [24,25], and the texture developed in the
AXM030304 and AXM030308 alloys is similar to that of conven-
tional extruded Mg alloy such as AZ31 alloy. Schmid factors for
basal slip under tensile loading along the extrusion direction are
0.31, 0.26, and 0.25 for the AXM030302, AXM030304, and
AXM030308 alloys, respectively. The Schmid factors did not
change by the solution treatment.
Mg Fig. 6 shows bright field TEM (BF-TEM) images taken from the
as-extruded (a) AXM030302, (b) AXM030304, and (c) AXM030308
alloys. Nanoscale particles with diameter of less than 100 nm are
Bal. observed within the grains and along the grain boundaries. EDS
Bal.
Bal.
analyses (Fig. 6(d)) suggest that these particles are β-Mn phases
having the FCC structure since these particles mainly consist of Al
 T. Nakata et al. / Materials Science & Engineering A 673 (2016) 443–449
Fig. 1. Surfaces of the (a) AX0303, (b) AXM030302, (c) AXM030304, and (d) AXM030308 extruded bars.
Fig. 2. Variations in Vickers hardness of the AXM030302, AXM030304, and
AXM030308 alloys as a function of aging time. As-ext. and S.T. stand for the as-
extruded and solution-treated condition.
and Mn with their mole ratios of 40:60 [26]. A few percent of Ca is
also included in these particles. The number density of the β-Mn
particle increases with increasing Mn content; the number den-
sities in the as-extruded AXM030302, AXM030304 and
AXM030308 alloys are 1.8  1020 m  3, 3.3  1020 m  3, and
5.6  1020 m  3, respectively. These nanoscale particles are ob-
served at the grain boundaries even after the solution treatment as
shown in the BF-TEM image of the solution treated AXM030304
alloy (Fig. 6(e)), suggesting these particles pin grain boundaries.
Fig. 7 shows BF-TEM images and selected area diffraction (SAD)
patterns of the peak-aged (a) AXM030302, (b) AXM030304, and
(c) AXM030308 alloys recorded from the zone axis of [101̄0] of the
Mg matrix. The BF-TEM images of the AXM030302 and
AXM030304 alloys show linear contrasts along the trace direction
of the (0001) planes. Continuous and faint streaks are observed
along the [0001] direction in the SAD patterns of the AXM030302
and AXM030304 alloys, implying the formation of fine plate-
Fig. 3. Tensile stress-strain curves of the (a) as-extruded and (b) peak-aged AXM030302, AXM030304, and AXM030308 alloys.
445
shaped Guinier Preston (G.P.) zones on the (0001) planes as re-
ported in previous reports [27,28]. The number densities of the G.
P. zones in the AXM030302 and AXM030304 alloys are estimated
to be 4  1022 m  3 and 2.5  1022 m  3, respectively. However, in
the AXM030308 alloy, the BF-TEM image shows coffee-bean like
strain contrasts, and continuous streaks are not observed in the
SAD pattern, which means that G.P. zones are not formed in the
AXM030308 alloy. Fig. 8 shows HAADF-STEM and EDS elemental
maps of Ca, Al and Mn of the (a) solution-treated and (b) peak-
aged AXM030308 alloys. Ca-enriched particles are clearly visible
in a superimposed elemental map of Al and Ca (Fig. 8(b)) in the
vicinity of Al-Mn particles in the peak-aged sample while only Al-
Mn particles which dissolve a little amount of Ca are observed in
the solution treated sample. Considering the similar features in the
BF-TEM image reported by Oh-ishi et al. [28] and the EDS results
(Fig. 8(b)), the Ca enriched compounds should be Mg2Ca phases.
4. Discussion
In this work, we have investigated the role of Mn on the me-
chanical properties and microstructure in the Mg-0.3Al-0.3Ca-
xMn (wt%, x ¼0, 0.2, 0.4, and 0.8) alloys extruded at high die-exit
speed of 60 m/min. The addition of Mn substantially improved the
extrudability, and the peak-aged AXM030304 alloy showed the
highest strength with reasonable ductility in the peak-aged con-
dition (Fig. 3(c)), which are comparable to those of 6000 series Al
based alloys.
The strengths of the as-extruded samples increased with in-
creasing the Mn content (Fig. 3 and Table 2). The proof stress in-
creases from 136 to 167 MPa with increasing the Mn content from
0.2% to 0.4%. This is mainly attributed to the grain refinement
[30,31], strong alignment of (0001) planes [19,29,32,33], and the
dispersion strengthening effect by Al-Mn particles [19]. As shown
in Fig. 6, the Mn addition lead to the formation of Al-Mn particle,
446 T. Nakata et al. / Materials Science & Engineering A 673 (2016) 443–449

Table 2
0.2% Proof stresses, ultimate tensile strengths, and ductility of the as-extruded and peak-aged AXM030302, AXM030304, and AXM030308 alloys.

As-extruded Peak-aged

Alloy 0.2% Proof stress [MPa] Tensile strength [MPa] Elongation (%) 0.2% Proof stress [MPa] Tensile strength [MPa] Elongation (%)

AXM030302 136 ± 2 203 ±2 29 ± 1 188 ±0 247 ± 0 27 ±0

AXM030304 166 ±1 220 ±1 24 ± 0 220 ± 2 264 ±0 22 ± 2
AXM030308 190 ± 3 229 ±1 24 ± 3 199 ± 1 243 ± 0 22 ± 3

Fig. 4. Inverse pole figure maps of the (a) as-extruded and (b) solution-treated AXM030302, AXM030304, and AXM030308 alloys.

Fig. 5. Inverse pole figures of the (a) as-extruded and (b) solution-treated AXM030302, AXM030304, and AXM030308 alloys.

and the number density was 1.8  1020 m  3, 3.3  1020 m  3 in
AXM030302 and AXM030304 alloys. This means that a larger
dispersion strengthening effect is expected in the AXM030304
alloy. Al-Mn particles also worked as grain growth inhibitor since
they pin the grain boundaries (Fig. 8). Therefore, we can under-
stand the formation of finer grain structure in the AXM030304
alloy than in the AXM030302 alloy, and the inhibition to the static
grain growth leads to the strongly aligned feature of the (0001)
planes [29]. However, the grain size and strongly aligned feature of
the (0001) planes do not change even if the Mn content is in-
creased to 0.8%. This is probably because the pinning effect by the
Al-Mn particle is saturated as reported by Khan et al. [18]. The
increase in the number density of Al-Mn particle to 5.6  1020 m  3
lead to a larger dispersion strengthening effect, giving rise to the
 T. Nakata et al. / Materials Science & Engineering A 673 (2016) 443–449
Fig. 6. BF-TEM images of the as-extruded (a) AXM030302, (b) AXM030304, and (c) AXM030308 alloys, (d) a BF-TEM image and EDS point analyses obtained from the as-
extruded AXM030302 alloy, a BF-TEM image of the solution-treated AXM030304 alloy.
Fig. 7. BF-TEM images and selected area diffraction (SAD) patterns of the peak-
aged (a) AXM030302, (b) AXM030304, and (c) AXM030308 alloys.
447
proof stress of 190 MPa.
The proof stresses and ultimate tensile strengths increased
without significant loss of the ductility by the peak-aging, and the
AXM030304 alloy exhibited the highest strength; the proof stress
and ultimate tensile strength of the AXM030304 alloy were 220
and 264 MPa. The strength increment by the peak-aging is at-
tributed to the precipitates since the grain structure and texture
feature do not change by the solution treatment (Figs. 4–6). The
AXM030302 and AXM030304 alloy show similar increases in the
proof stresses by 52 and 53 MPa although the number density of
the precipitate in the AXM030302 alloy, 4  1022 m  3, is higher
than that in the AXM030304 alloy, 2.5  1022 m  3. The increase in
the proof stress, Δs, by the dispersion of the precipitates can be
understood by considering an increment of critical resolved shear
stress by precipitation hardening, Δτ, and Schmid factor, M, as
follows [19];
Δτ
Δσ = .
M (1)
The Δτ increases with increasing the number density of pre-
cipitates, and is described as follows [34];
Gb d
Δτ = ln .
2πλ 1 − ν r0 (2)
where G is the shear modulus, b is the magnitude of burgers
vector, λ is the effective planar inter-obstacle spacing (¼ 1/ N⋅t .
[35], where N is the number density of precipitates per unit vo-
lume and t is the thickness of precipitates), ν is the Poisson's ratio,
d is the uniform diameter of precipitates, and r0 is the core radius
of dislocations ( ¼b [34]). Assuming that the size of the G.P. zones
is the same for the AXM030302 and AXM030304 alloys , the re-
lation between the Δs for the AXM030302 alloy, ΔsAXM030302, and
the Δs for the AXM0303004 alloy, ΔsAXM030304, can be written as
follows;
448 T. Nakata et al. / Materials Science & Engineering A 673 (2016) 443–449
Fig. 8. STEM-EDS images and EDS elemental maps of the (a) solution-treated and (b) peak-aged AXM030308 alloys.
MAXM 030304 NAXM 030302
ΔσAXM030302 = ΔσAXM 030304 . ability and the optimization of Al content in the Mg-Al-Ca-Mn
MAXM 030302 NAXM 030304
where MAXM030302 and MAXM030304 are the Schmid factor of the
AXM030302 and the AXM030304 alloys, and NAXM030302 and
NAXM030304 are the number density of the G.P. zones in the
AXM030302 and AXM030304 alloys. As the Schmid factor, M, the
one for basal slip should be considered because initial tensile de-
formation along extrusion direction in Mg alloys is predominantly
governed by basal slip [36]. Using Schmid factors and the number
density of the precipitates as MAXM030302 ¼0.31, MAXM030304 ¼0.26,
NAXM030302 ¼4.0 ×1022 m  3, and NAXM030304 ¼2.5 ×1022 m  3, fol-
lowing relationship is derived;
ΔσAXM030302 = 1.1ΔσAXM 030304.
This result suggests that the increase in the proof stress by the
peak aging, Δs, in the AXM030302 and AXM030304 alloy should
be almost the same since the proof stress can be effectively in-
creased by dispersing the G.P. zones within the grains whose
[0001] directions are strongly aligned normal to the extrusion.
Although the grains in the AXM030308 alloy had similar textured
feature to those in the AXM030304 alloy, the excessive addition of
Mn to 0.8% resulted in the significant decrease in the strength
increment by the peak-aging; the proof stress and ultimate tensile
strength are 199 and 243 MPa after the peak-aging (Figs. 2 and 3).
This is because the strengthening precipitate changed from the G.
P. zone to sparsely dispersed coarse Mg2Ca phase in the peak-aged
AXM030308 alloy (Figs. 7 and 8). The Mg2Ca phase is formed since
most of Al element is used to form the Al-Mn particles, and there is
almost no Al left to form the G.P. zones in the AXM030308 alloy
[27].
As demonstrated in this work, we found that the optimum Mn
content in the Mg-0.3Ca-0.3Al alloy was 0.4% to achieve the high
strength with reasonable ductility. This is because high number
density of G.P. zones are dispersed within the fine grains in the
AXM030304 alloy. The effect of precipitation hardening was
maximized by dispersing the precipitates within the grains with
their [0001] direction strongly aligned to the normal direction to
the extrusion direction. Since the strength is expected to be fur-
ther increased by increasing the number density of the G.P. zones,
the optimization of Al content is expected to increase the strength
further. Although the Mn addition is also found to improve the
extrudability, the reason still remains unclear. Future work will
shed light on to the clarification of the role of Mn on the extrud-
(3)
dilute alloy system.
5. Conclusions
In this work, we investigated the mechanical properties and
microstructure of the Mg-0.3Al-0.3Ca-xMn (wt%, x ¼0, 0.2, 0.4 and
0.8) dilute alloys. We found that the high speed extrusion at die-
exit speed of 60 m/min was impossible without Mn addition, and
the optimum Mn content was 0.4%. Ideal microstructure for
strengthening was formed in the AXM030304 alloy; high number
density of G.P. zones were dispersed, and the Al-Mn particles led
(4)
to the formation of the fine grains whose [0001] directions were
strongly aligned normal to the extrusion direction. The
AXM030304 alloy exhibited the highest proof stress of 220 MPa
and ultimate tensile strength of 264 MPa that are superior to those
of an aged 6063 aluminum alloy. Therefore, the AXM030304 alloy
is a promising candidate as a light alternative to the 6000 series Al
based alloys.
Acknowledgment
This work was supported by JSPS KAKENHI Grant Number
25249101, Grant-in-Aid for JSPS Research Fellows Grant Number
15J12688, and Advanced Low Carbon Technology Research and
Development Program (ALCA), 12102886.
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