Beruflich Dokumente
Kultur Dokumente
Original Research
A R T I C L E I N F O A B S T R A C T
Keywords: The effects of Sn addition (0, 0.5, 1.0, 2.0 and 3 wt%) on microstructure of Mg-4Zn-1.5Al alloy in cast and
Magnesium alloys extruded states were investigated, and the mechanical properties of as-extruded Mg-4Zn-1.5Al-xSn studied. The
Sn addition experimental results showed that the as-cast Mg-4Zn-1.5Al alloy was composed of two phases α-Mg and Mg32
Microstructure (Al, Zn) 49, while Sn-containing alloys consisted of α-Mg, Mg32 (Al, Zn)49 and Mg2Sn phases, and Mg32 (Al, Zn)49
Texture
was not detected after extruding due to that the most of them dissolved into the matrix during the homogenized
Mechanical properties
treatment. The addition of Sn refined the grains of as-cast and as-extruded Mg-Zn-Al alloys obviously. It was
noted that the basal texture intensity reduced with increasing Sn content significantly in as-extruded Mg-Zn-Al
alloys. The tensile tests results indicated that Sn addition improve the tensile strength of the extruded alloys,
while it had a harmful effect on the ductility. When the addition of Sn was 2 wt%, the ultimate tensile strength
(UTS), yield strength (YS) and elongation (εf) of the alloy were 280 MPa, 147 MPa and 17.4%, respectively.
https://doi.org/10.1016/j.pnsc.2017.11.002
Received 23 May 2017; Received in revised form 5 November 2017; Accepted 6 November 2017
Available online 06 December 2017
1002-0071/ © 2017 Chinese Materials Research Society. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/BY-NC-ND/4.0/).
B. Wang et al. Progress in Natural Science: Materials International 27 (2017) 695–702
Table 1
Chemical composition of the experimental alloys (wt%).
Zn Al Sn Mg
2. Experimental procedures
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Fig. 3. Optical images showing the microstructures of as-cast Mg-4Zn-1.5Al-xSn alloys. (a) ZAT420, (b) ZAT420.5, (c) ZAT421, (d) ZAT422, (e) ZAT423.
Fig. 4. SEM images of as-cast Mg-4Zn-1.5Al-xSn alloys (a) ZAT420, (b) ZAT420.5, (c) ZAT421, (d) ZAT422, and (e) ZAT423.
consistent with the results from XRD in Fig. 1. The second peak (around obvious effect on grain size, the morphology and the volume percentage
620 °C) is the melting temperature of the α-Mg matrix. The DSC scan of secondary phases. After adding Sn, the grain size decreases and the
results imply that the addition of Sn to ZA42 alloy has no influence on number of secondary phases increase to a certain degree. It can be seen
the low temperature eutectic phase transformation. There is no obvious clearly from Fig. 4, typical SEM images of as-cast Mg-4Zn-1.5Al-xSn
peak for Mg2Sn transformation found in the DSC curves, which may alloys. It reveals that all the experimental alloys are characteristic of
result from that the quantity of Mg2Sn particles is not enough for scan divorced eutectic and the more addition of Sn, the more secondary
detection in the Sn-containing alloys. This is also corresponded with the phases and more continuous of secondary phases. Expect that, most of
results from XRD in Fig. 1. secondary phases are distributed in the vicinity of grain and dendritic
Fig. 3 shows the optical microstructure of as-cast Mg-4Zn-1.5Al-xSn boundaries, which can be seen from Fig. 5 clearly. Fig. 5 shows high-
alloys. All the as-cast alloys show typical dendritic structure with α-Mg magnification SEM micrographs of as-cast ZAT422 alloy. As shown in
matrix and a large amount of intermetallic compounds distributed Fig. 5, two types of intermetallic compounds are observed in the alloy:
along the dendritic boundaries. It is found that the addition of Sn has an the bright block compound (marked as B) and the net-liked compound
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Fig. 6. Optical micrographs of as-extruded Mg-4Zn-1.5Al-xSn alloys (a)ZAT420, (b) ZAT420.5, (c) ZAT421, (d) ZAT422, and (e) ZAT423.
(marked as C and D). Most of the compounds are all mixed with each interface during solidification. Consequently, the refined cast micro-
other. A is mainly composed of Mg, B mainly consists of Mg and Sn structure in the Sn-containing should be related to that Sn addition
elements, with the atomic ration of Mg to Sn is approximately 2, C and induces excessive constitutional supercooling during solidification and
D are rich in Mg, Zn and Al, other than Sn, with the atomic ration of Mg suppresses the formation and growth of Mg32 (Al, Zn)49 intermetallic
to Zn and Al is approximately 1. Combining with Fig. 1 and Fig. 5, B phase due to the precipitation of Mg2Sn phase.
with bright particles and bright block compounds mostly mixing with
the continuous eutectic phases can also be observed in as-cast ZAT422 3.2. As-extruded microstructure
alloy, which are identified as Mg2Sn phase. Both the isolated and
continuous net-liked phases marked as C and D are correspond to β- The optical microstructure of as-extruded Mg-4Zn-1.5Al-xSn alloys
Mg32 (Al, Zn)49 phase with trace Sn content. And A is α-Mg matrix. taken from the parallel plane to the extrusion direction (ED) is shown in
As mentioned above, the addition of Sn plays an important role in Fig. 6. Comparing with as-cast alloys (Fig. 3), the grains are refined
grain refinement and distribution of inter-dendritic intermetallic com- obviously, especially in Fig. 6d. With increasing of Sn addition, grain
pounds, and also makes a contribution to the precipitation of secondary size decreases, especially along ED. The grain sizes of ZAT420,
phases. Based on the observations from Figs. 3 and 4, the grain size ZAT420.5, ZAT421, ZAT422 and ZAT423 are 27 µm,22 µm,22 µm,
decreases and the secondary phase amount increases with increasing Sn 16 µm, and 21 µm, respectively. It indicates that the addition of
content. It is also evident that ZAT422 alloy exhibits the optimal re- 0.5–2 wt% Sn can lead to grain refinement in a certain degree. How-
finement and uniform distribution of the inter-dendritic intermetallic ever, the grain size exhibits the increasing tendency as the addition of
compounds. However, the grains become larger and the inter-dendritic Sn is above 2%, as shown in Fig. 6e. Fig. 7 illustrates the SEM images of
intermetallic compounds get coarser as the Sn addition is up to 3 wt%. as-extruded Mg-4Zn-1.5Al-xSn alloys. There are some small grains
Based on electronegative values of Mg, Al, Zn, and Sn, Mg2Sn has around the large grains obviously, which means that the process of
higher thermal stability as compared to Mg32 (Al, Zn)49 and can inhibit dynamic recrystallization is not completely. And numerous fine parti-
the formation and growth of Mg32 (Al, Zn)49 phase. Yang et al. [16] cles are distributed along grain boundaries and within the grain inter-
found that Mg32 (Al, Zn)49 phase could be refined by forming Mg2Sn, iors, but most of them are on the grain boundaries along the extrusion
which influenced the diffusion kinetics of Al and Mg atoms. Dong et al. direction. And the more fine particles, the finer grain size. It means that
[23] deduced that Sn added to the AZ64 alloy had an effective influence these fine particles play an important role in restricting dynamic re-
on promoting the solute enrichment of Al and Zn at the solid-liquid crystallization grain growth by pinning effect. According to the
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Fig. 7. SEM images of as-extruded Mg-4Zn-1.5Al-xSn alloys (a) ZAT420, (b) ZAT420.5, (c) ZAT421, (d) ZAT422, (e)ZAT423.
following XRD and TEM results in Figs. 8 and 9, the bright particles are
Mg2Sn phases.
From Fig. 6 and Fig. 7, the Sn addition can refine the grains effec-
tively, which is quite well consistent with the as-cast Mg-4Zn-1.5Al-xSn
alloys. And all the extruded alloys exhibit dynamic recrystallized mi-
crostructure with fine and relatively coarse dynamic recrystallized
grains. It implies that there is dynamic recrystallization occurring but
not completely during the extrusion process. The fine-grains are attri-
butable to dynamic recrystallization area and the coarse grains are the
dynamic unrecrystallized region during the extrusion at 300 °C.
Therefore, it can be deduced that Mg2Sn precipitates play an important
role in achieving a fine-grained structure in as-extruded Mg-4Zn-1.5Al-
xSn alloys. Actually, similar phenomenon has been detected by Sasaki
et al. [24]. The Mg2Sn phase is formed by adding Sn, which in large size
as a primary phase. And the Mg2Sn particles in large size have been
broken along the extrusion direction during extrusion process. The
broken Mg2Sn particles are able to be acted as the heterogeneous nu-
cleation sites for recrystallized grains. Besides, the refined cast micro-
structure is important for the dynamic recrystallized microstructure, Fig. 8. XRD patterns of as-extruded Mg-4Zn-1.5Al-xSn alloys.
because the grain boundaries can act as the heterogeneous nucleation
sites for recrystallized grains. However, the growth of recrystallized
grains can also be inhibited by Mg2Sn. This is because that the motion 2%. Compared with the as-cast alloys, Mg32 (Al, Zn)49 phase disappears
of grain boundary will be hindered by Mg2Sn particles, which are dis- in the as-extruded alloys. It may be attributed to that most of Mg 32 (Al,
tributed in the vicinity of grain boundaries [24–27]. In other words, the Zn)49 phases are dissolved into α-Mg matrix during the homogenized
dynamic recrystallization may be promoted by Mg2Sn particles along treatment and the quantity of Mg32 (Al, Zn)49 phase particles are so
extrusion direction and thus the grains are refined obviously in Mg-4Zn- small that XRD can’t detect them. As seen from Fig. 7a, there is some
1.5Al-xSn alloys. fine particles are distributed along the grain boundaries, combined with
The XRD patterns of as-extruded Mg-4Zn-1.5Al-xSn alloys are Fig. 8a, there is only α-Mg in ZAT420 alloy. It can be deduced that the
shown in Fig. 8. As can be seen from Fig. 8, the phase of ZAT420 is only fine particles are the Mg-Zn phase. In order to precisely identify the
composed of α-Mg. However, the diffraction peaks for Mg2Sn phase precipitates, further TEM study was conducted in as-extruded ZAT422
only can be detected in ZAT423 alloy. The ZAT423 alloy consists of α- alloy.
Mg and Mg2Sn. As the addition of Sn is less than 2%, the as-extruded Fig. 9 presents TEM images of the precipitates in as-extruded
alloys only consist of α-Mg, and there is no Mg2Sn phase. The reason is ZAT422 alloy. The extruded ZAT422 alloy shows three kinds of pre-
that the maximum solubility of Sn at 420 °C is about 2.85%. Therefore, cipitates morphologies (Fig. 9a): the typical long and short rod-liked
there are no Mg2Sn diffraction peaks as the addition of Sn is less than precipitates (marked as A and C) and some spherical shaped
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precipitates (marked as B). The size of these rods ranges from 50 nm to Mg4Zn7. However, Mg-Zn phase can’t be detected from the XRD pat-
120 nm in length and their growth direction is parallel to < 01–11 > terns, which should result from that the Mg-Zn precipitates are very
directions. The spherical shaped precipitates are approximately 25 nm few.
in diameter and their growth direction is also aligned to < 01–11 >
directions. According to the results from EDS analysis, these long and 3.3. Texture
short rod-liked precipitates should be Mg-Zn phases, and the spherical-
liked precipitates may be Mg2Sn phase. The further analysis is shown in The pole figures of {0002} plane // ED showing the textures of as-
Fig. 9c-f. As we all known, Mg2Sn is the face-center cubic phase extruded ZAT42x alloys with different Sn contents are shown in Fig. 10.
(a=0.674 nm) with the space group Fm3m. The SAED pattern of the Texture feature is influenced by the addition of Sn obviously. In
spherical shaped phase (marked as D) in Fig. 9d is consistent with that Fig. 10a, the peak intensity is at the center of the {0002} pole figure,
of Mg2Sn phase, and thus the precipitate D should be identified as indicating a strong basal texture. In Fig. 10b and Fig. 10c, the peak
Mg2Sn. Mg2Sn phase has the orientation relationship with α-Mg matrix intensity regions deviated from the center of the pole figures and the
as follows: (0002) Mg/ (−3–11) Mg2Sn, and [01−11] Mg/ [2–33] Mg2Sn. peaks tend to split, especially in Fig. 10c. It indicates that the basal
From Fig. 9e and f, the rod precipitate E can be identified as Mg-Zn texture of the wrought ZAT42x alloy appears to become weaker as the
phase. Mg-Zn phase is parallel to < 01–11 > directions of α-Mg matrix. addition of Sn increases. From ZAT420 to ZAT422, the value of the
For the further calculations from FFT pattern in Fig. 9f, and combined maximum intensity of basal texture reduces notably, from 23.1 to 5.2,
with the reports by Wei [28] and Gao [29], Mg-Zn phase might be β1'- which indicates that basal texture can be weakened by adding Sn
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respective values are given in Fig. 11b. It reveals that the addition of Sn
can improve both yield strength and ultimate tensile strength. In the
contrary, the elongation decreases into a certain degree. With in-
creasing of Sn, both YS and UTS increase, except for the elongation.
When Sn content increases from 0 to 2 wt%, UTS is enhanced from
263 MPa to 280 MPa and YS is improved from 125 MPa to 148 MPa,
while the elongation is reduced from 27% to 17%. However, excessive
Sn addition results in the decrease of YS and UTS values except for the
elongation. The UTS, YS and εf are 270 MPa, 148 MPa and 21%, re-
spectively. This is because the coarsening effect of Mg2Sn precipitates
and grain size. The excessive Sn addition results in the coarsening of
Mg2Sn precipitates and grain size, which are harmful for the mechan-
ical properties. It is obvious that the amount of Sn to ZA42 alloy should
be limited within a certain range to achieve the maximum strength-
ening effect by grain refinement and an increase in the fine precipitates
while suppressing the formation of excessively large undissolved Mg2Sn
phase simultaneously. The improvement of mechanical strength can be
mainly summarized in the following two aspects. On the one hand, the
addition of Sn can give rise to the decrease of grain size. According to
the Hall-Petch relation: σy∝d−1/2, grain size d plays an important role
in improving the tensile strength. The smaller of grain size, the better of
mechanical properties. The refined grains prevent the motion of dis-
locations to increase the strength, and the slip systems can be changed
by the blocked dislocations, resulting in cross slip to maintain good
ductility. And Ma [30] found that lower basal texture intensity tends to
enhance the strength. As shown in Fig. 6, ZAT422 alloy has the smallest
grain size among these alloys, and also with the minimum basal texture
in Fig. 10, which is consistent with the highest strength obtained in
ZAT422 alloy. On the other hand, Mg2Sn precipitates are the effective
barriers to dislocation motion and grain boundary sliding, so they play
an important role in precipitation strengthening effect. With the in-
crease of Sn addition, the Mg2Sn precipitates increase, which can be
seen from Fig. 6, Fig. 7 and Fig. 8 clearly, especially for ZAT423 alloy.
In addition, there are many rod-liked Mg-Zn phase in a-Mg matrix from
Fig. 9, numerous Mg-Zn phase are dissolved into the α-Mg matrix, and
the massive precipitations of Mg2Sn can improve effect of the Mg-Zn
eutectics [17]. Chen et al. [17] and Turen [5] have been reported that
the addition of Sn to the ZA and AZ magnesium alloy lead to the sup-
pression of the eutectics transformation and refinement of the divorced
eutectics, their results is accord with our present results. Based on this,
ZAT422 alloy is considered to offer the optimal strength and elongation
(280 MPa UTS, 147 MPa YS and 17.4% elongation) among the experi-
mental alloys when considering just how much the strength is improved
for what is a relatively large decrease in elongation relative to ZA42
alloy.
Fig. 10. Pole figures of (0002) plane showing the textures of as-extruded ZAT42x alloys 4. Conclusions
with different Sn contents: (a) ZAT420, (b) ZAT420.5, and (c) ZAT422.
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Fig. 11. Tensile engineering stress-strain curves of the as-extruded ZAT42x alloys with various Sn additions. (a) ZAT420, (b) ZAT420.5, (c) ZAT421, (d) ZAT422, (e) ZAT423.
strength, yield strength and elongation are 280 MPa, 147 MPa and 630–635.
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