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A R T I C L E I N F O A B S T R A C T
Keywords: In the present investigation, microstructure, texture and mechanical properties of Mg-3Mn alloys fabricated by
Magnesium‑manganese alloys hot extrusion process with the extrusion temperatures of 250 °C and 300 °C were investigated. The results re-
Microstructure vealed that the samples exhibited the refined microstructure and weakened basal texture. Refined microstructure
Texture of the samples was attributed to the dynamic precipitates suppressing the recrystallization grain growth during
Mechanical property
extrusion process. Weakened basal texture of the samples was explained as a result of particle stimulated nu-
PSN
cleation (PSN) promoted by coarsened Mn precipitates altering the texture of extruded profiles during re-
crystallization by orienting the c-axis of grains at an angle that favors basal slip activity. As a result, the samples
exhibited the high tensile elongation and good yield strength at room temperature.
⁎
Corresponding authors at: Chongqing University, Chongqing, PR China.
E-mail addresses: zwyu@zmc.edu.cn (Z. Yu), tat@cqu.edu.cn (A. Tang).
https://doi.org/10.1016/j.matchar.2017.12.029
Received 19 July 2017; Received in revised form 22 November 2017; Accepted 19 December 2017
Available online 20 December 2017
1044-5803/ © 2017 Elsevier Inc. All rights reserved.
Z. Yu et al. Materials Characterization 136 (2018) 310–317
Table 1 are found in this paper. The result is consistence with the previous work
Chemical composition of M3 alloy (wt%). [24]. In addition, extrusion process, such as temperature, strain rate,
extrusion ratio et al., rarely changes the phase components of Mg alloys
Alloys Mn Fe Si Others Mg
[25]. Therefore, cross section of M3 alloy extruded at 300 °C are se-
M3 2.971 0.001 0.002 < 0.010 Bal. lected to examine the XRD pattern shown in Fig. 1b. The result de-
monstrates that the main phases of as-extruded M3 alloy are α-Mg and
α-Mn phases. Due to the limited solid solubility of Mn alloying element
2. Experimental Procedure in Mg matrix shown in Fig. 1c, none of the intermetallic compounds are
formed between magnesium and manganese in M3 alloy extruded at
Commercial pure magnesium (99.98 wt% Mg) and Mg-Mn master both 250 °C and 300 °C. Fig. 1d shows the DSC cooling curve of as-cast
alloy containing 4.04 wt% manganese were applied to synthesize the M3 alloy in this paper. As clearly observed, the alloy has four main
experimental samples. The testing alloy Mg-3.0Mn, hereafter named peaks at about 687.2 °C, 678.0 °C, 659.7 °C and 640.1 °C, respectively,
M3 alloy, was melt in an electric resistance furnace under a mixed at- corresponding to the pseudo peritectic reaction or phase transformation
mosphere of CO2 and SF6. Molten metal was stirred and held on about temperatures.
20 min at 740 °C. Then it was poured into a preheated (300 °C) steel
mold. The dimensions of the ingots were 100 mm in diameter and 3.2. Microstructure
150 mm in length. The billets covered with graphite were homogenized
at 500 °C for 24 h and then water quenching immediately. The billets Fig. 2 shows the microstructure of both as-cast and as-extruded al-
were preheated to 250 °C and 300 °C, respectively, for 2 h and extruded loys in the present work. In Fig. 2a, as-cast pure Mg shows the ex-
in an XJ-500 horizontal extruder. Solid rods, approximately 16 mm in tremely coarsened microstructure with the average grain diameter of
diameter, corresponding to an extrusion ratio of 25:1, were extruded at ~1481.5 μm. Previous investigation [26] figured out that Mn exhibited
the extrusion rate of 4 mm s− 1 and air cooled. the extremely poor grain refinement effect on as-cast Mg alloys with its
As to confirm whether the high melting point metal Mn has been lowest grain growth restriction factor (GRF) value of ~0.15, compared
added into the M3 alloy, X-ray fluorescence spectrometry (XRF) was with those alloying elements, Ti [27], Fe [28], Zr [26] et al., showing
employed to inspect the actual chemical composition of the experi- the obvious effect on refining the microstructure of as-cast Mg alloys.
mental samples shown in Table 1. XRF result indicated that Mn alloying However, microstructure of as-cast M3 alloy has been refined compared
element was successfully added into the experimental samples. with as-cast pure Mg, and the average grain diameter is ~741.8 μm
Phase constitution and texture were determined by Rigaku D/max- shown in Fig. 2b.
2500 X-ray diffraction (XRD), using Cu Kα radiation (wave length Metallography of deformed, e.g. extruded, rolled, forged, Mg-Mn
λ = 0.15406 nm) at 45 kv and 150 mA with a sample tilt angle ranging alloys is difficulty to be revealed due to their poor response to etching
from 20° to 80°. Texture analyses of the extrusion bars were carried out [29]. According to the previous investigation [30], there were no sig-
for the (0002), (1010 ), (1011) and (1012 ) planes. The measurements were nificant change in average grain size of Mg-Mn alloys when annealing
performed on the cross sections of the specimens. Differential scanning at 300 °C for 1 h. As to clearly reveal the microstructure of the samples
calorimetry (DSC) was tested by NETZSCH STA 449C system. Samples in the present work, therefore, both of the extruded samples are an-
weighted around 30 mg were heated in a flowing argon atmosphere nealed at 300 °C for 1 h, and microstructure of the samples are shown in
from room temperature to 700 °C for 5 min before being cool down to Fig. 2. The samples exhibit a bimodal microstructure, consisting of
100 °C. The cooling curve was recorded at a controlling speed of 10 °C/ equiaxed recrystallized grains and unrecrystallized regions indicated by
min. the arrows in Fig. 2c and Fig. 2d. The volume fraction of un-
Samples were ground and polished by standard metallographic recrystallized regions in M3 alloy extruded at 250 °C is ~7.8% shown in
preparations. Afterwards, specimens were etched in a solution con- Fig. 2c, and the average recrystallized and unrecrystallized grain sizes
taining 20 ml acetic acid, 6 g picric acid, 2 ml H2O and 100 ml ethanol. are 1.1 μm and 4.8 μm, respectively. With the extrusion temperature
Zeiss optical microscope was applied to observe the microstructure of increasing to 300 °C, the volume fraction of unrecrystallized regions,
extruded profiles. average recrystallized and unrecrystallized grain sizes are ~ 9.2%,
Transmission electron microscopy (TEM) foils of the samples were 5.3 μm and 9.4 μm shown in Fig. 2d, respectively.
prepared by twin-jet electro polishing using a solution of 5.3 g LiCl, Fig. 3 shows the SEM images of both as-cast and as-extruded M3
11.6 g Mg(ClO4)2, 500 ml methanol and 100 ml 2-butoxy-ethanol at alloys. Obviously, both of the samples show the similar phase con-
approximately − 50 °C and 90 V. The specimens were surface cleaned stitutions. In Fig. 3a and Fig. 3b, an amount of coarsened Mn-enriched
by ion milling using a Gatan Precision ion Polishing System (PIPS) at an particles, identified by EDS inset of Fig. 3a and marked by the arrows in
operating voltage of 2 kV. Fig. 3b, are observed locating among the matrix and along the grain
Room temperature mechanical properties of the samples were tested boundary. Fig. 3c and Fig. 3d show the SEM morphologies of M3 alloy
using a universal material testing machine for tension and compression extruded at 250 °C. As clearly seen from the figures, a large number of
(SANS CMT-5100). Tensile (5 mm diameter and 25 mm gauge length) finer Mn-enriched particles confirmed by EDS inset of Fig.3d are ob-
and compressive (8 mm diameter and 12 mm height) test specimens served, and only a small quantity of coarsened particles containing Fe
were machined parallel to the extrusion axis from the extruded rods and and Si are observed in Fig. 3c. The coarsened particles have been
pulled to failure with a strain rate of 3 mm/min. At least three samples commonly observed in Mg alloys [18]. This can be estimated as the
were taken from different locations of the extruded rods. The tension major factor of Mn addition on removing the impurities, and then im-
and compression axes were kept parallel to the extrusion axis. proving the corrosion resistance of Mg alloys [31].
3.1. Phase Component Texture in forms of (0002), (1010 ), (1011) and (1012 ) pole figures of
M3 alloys extruded at both 250 °C and 300 °C are analyzed to assess the
XRD patterns of both as-cast and as-extruded M3 alloys have been grain orientation evolution shown in Fig. 4. Both of the samples exhibit
examined shown in Fig. 1. XRD pattern of as-cast M3 alloy shown in the unusual fiber texture. In Fig. 4a, M3 alloy extruded at 250 °C shows
Fig. 1a indicates that phase constitutions are α-Mg matrix and Mn the texture with 〈0001〉 axis of the Mg matrix tilting nearly 40° away
precipitates, respectively. None of the Mg-Mn intermetallic compounds from the radial direction, and a maximum texture intensity of 1.606.
311
Z. Yu et al. Materials Characterization 136 (2018) 310–317
With the extrusion temperature increasing to 300 °C, the intensified both as-cast and as-extruded M3 alloys are shown in Fig. 5, and room
texture is with < 0001 > axis of the Mg matrix tilting about 10° away temperature mechanical properties are listed in Table 2. Obviously, as-
from the radial direction, and an increased intensity of 1.712 is ex- cast M3 alloy shows a yield strength (YS) of 34.2 ± 3 MPa, an ultimate
amined shown in Fig. 4b. Previous investigations [32–36] illustrated tensile strength (UTS) of 97.7 ± 5 MPa and a tensile elongation to
that the recrystallized grains usually corresponded to a relatively weak rupture (EL) of 5.6 ± 0.6%. The poor performance of as-cast alloy can
texture. In other words, grains nucleated by the particle stimulated be attributed to the coarsened microstructure shown in Fig. 2b, poor
nucleation (PSN) mechanism are proved to be random in orientation, solid solution strengthening behavior [40] and unsatisfied precipitation
leading to the weakened texture of M3 alloys in this paper [37–39]. The hardening effect [41]. However, M3 alloy, after hot extrusion de-
lower texture intensity of M3 alloys might be attributed to the higher formation, exhibits the excellent mechanical performance shown in
volume faction of recrystallized grains shown in Fig. 2. Fig. 5. The sample extruded at 250 °C exhibits the highest YS of
212.6 ± 6 MPa, excellent UTS of 248.3 ± 8 MPa and outstanding EL
property of 29.9 ± 0.3%. With the extrusion temperature increasing to
3.4. Mechanical Properties
300 °C, YS, UTS and EL properties of the alloy decrease slightly to be
205.4 ± 5 MPa, 241.6 ± 7 MPa and 26.7 ± 0.5%, respectively.
The typical nominal tensile and compressive stress-strain curves of
312
Z. Yu et al. Materials Characterization 136 (2018) 310–317
Fig. 3. SEM morphologies of (a), (b) as-cast and (c), (d) as-
extruded Mg-3Mn alloys extruded at 250 °C.
Simultaneously, the alloy extruded at 250 °C also shows the higher that have the obvious effect on pinning the grain growth during the
compressive properties than that extruded at 300 °C. Furthermore, the extrusion process. Most of previous investigations proved that Mn ele-
samples extruded at 250 °C and 300 °C also exhibit the improved yield ment had the obvious effect on refining the microstructure of as-ex-
strength asymmetry (YSA) properties, and the values of YSA are ~0.91 truded Mg alloys, e.g. Mg-Zn [45], Mg-Gd [13] and Mg-RE-Zn [12] al-
and ~0.89, respectively. Therefore, M3 alloys in the present work show loys. In addition, our previous work [23] found that Mn addition can
the better comprehensive mechanical properties, including YS, EL and significantly refine the microstructure of pure Mg as well, leading to an
YSA, than commercial AZ31 and ZK60 alloys [9,42–44]. obvious enhancement of tensile properties. Fig. 6 shows the bright filed
TEM image of M3 alloy extruded at 250 °C. A high density of nanoscale
4. Discussion heterogeneous phases lying among the matrix and along the grain
boundary are observed Fig. 6a. Together with the EDS analyzes, second
4.1. Effect of Mn Addition on Microstructure phases marked as “1”, “2” and “3” located in the red circles A, B and C
in Fig. 6a, respectively, are verified to be Mn-enriched phases. Ac-
In general, microstructure of as-extruded Mg alloys can be refined cording to the previous investigation [24], an amount of Mn-enriched
by a high quantity of fine precipitates located along the grain boundary particles are only Mn precipitates in M3 alloy because Mn phase is the
313
Z. Yu et al. Materials Characterization 136 (2018) 310–317
Table 2
Mechanical properties of M3 alloys and samples reported in literatures.
TYS (MPa) UTS (MPa) El (%) CYS (MPa) UCS (MPa) EC (%)
314
Z. Yu et al. Materials Characterization 136 (2018) 310–317
combining with an amount of nanoscale Mn heterogeneous lying 1. Mn additions effectively refine the microstructure of M3 alloys ex-
among the matrix and along the grain boundary, could considerably truded at both 250 °C and 300 °C due to the high density of na-
contribute to the strength of Mg alloys by providing barriers for gliding noscale Mn precipitates locating among the matrix and along the
dislocations. In addition, a high density of faults are also observed in grain boundary, pinning the recrystallized grains growth of α-Mg
M3 alloy extruded at 250 °C shown in Fig. 8a and b. According to the matrix during extrusion process. M3 alloy extruded at 250 °C shows
result of Fast Fourier Transformation (FFT) pattern presented as “C” in the refined grains with mean grain size of 1.5 μm by averaging re-
Fig. 8, the high density of faults in this paper are parallel to the basal crystallized and unrecrystallized grains.
planes of α-Mg matrix, implying that the faults can impede the basal 2. Both of M3 alloys show the weakened basal texture attributed to the
slip and resulting in an enhancement of YS of the sample [56]. particle stimulated nucleation (PSN) effect.
Therefore, microstructure of both M3 alloys have been refined from 3. The improvement of mechanical properties of M3 alloys can be at-
the dynamic recrystallization [57], and the alloy extruded at 250 °C tributed to the combined effects of refined microstructure, wea-
shows the refined microstructure. The dynamic precipitates of na- kened basal texture and high density of nanoscale Mn precipitates
noscale Mn phases among the matrix and along the grain boundary locating among the matrix and along the grain boundary, disloca-
shown in Fig. 6 play the vital role in refining the microstructure of α-Mg tions and faults.
grains of the extruded binary M3 alloys in Fig. 2. Moreover, since an
amount of nanoscale Mn precipitates disperse among the matrix and
along the grain boundary in Fig. 6 and a high density of faults are in- Acknowledgements
troduced during extrusion process in Fig. 8, the precipitates and defects
can provide the barriers for gliding dislocation, and thus contributing to The present work is supported by the National Key Research and
an improvement of strength in M3 alloy. Development Program of China (2016YFB0301100), National Natural
Science Foundation of China (Project 51501045 and 51474043), Youth
5. Conclusions Talent Project of Department of Education of Guizhou Province (KY
[2016] 207), Natural Science Foundation of Guizhou Province (J
In the present work, M3 alloys are processed by an extrusion pro- [2015] 2067), Research Foundation for Advanced Talents in Guizhou
cedure in which different extrusion temperatures are applied. The Institute of Technology (XJGC20141102) and Foundation of Talent
major conclusions are summarized as follows: Team (Guizhou (2015) 4008).
315
Z. Yu et al. Materials Characterization 136 (2018) 310–317
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