Materials Letters 245 (2019) 155–157

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Materials Letters
journal homepage: www.elsevier.com/locate/mlblue

Enhanced plasticity of magnesium alloy micro-tubes for vascular stents

by double extrusion with large plastic deformation
Wenlong Lu a, Rui Yue a, Hongwei Miao a, Jia Pei a,b, Hua Huang a,b,⇑, Guangyin Yuan a,b,⇑
a
National Engineering Research Center of Light Alloy Net Forming and Key State Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, School of Materials Science
and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China
b
Shanghai Innovation Institute for Materials, Shanghai 200444, China

a r t i c l e i n f o a b s t r a c t

Article history: Double extrusion with a large plastic deformation was conducted to fabricate Mg-Nd-Zn-Zr (JDBM)
Received 20 November 2018 micro-tubes (3.5 mm in outer diameter and 0.25 mm in thickness) with high plasticity for biodegradable
Received in revised form 19 February 2019 vascular stents application. After double extrusion, the grain size was greatly decreased to one seventh of
Accepted 23 February 2019
the original size and the basal texture intensity was enhanced slightly. The elongation increases from
Available online 2 March 2019
about 23% for the as-extruded JDBM alloy bar to about 48.8% for the as-extruded micro-tubes, which
is a 112% increase by double extrusion. The high elongation is attributed to the enhanced activation of
Keywords:
non-basal slips contributed by the significant grain refinement.
Biomaterials
Double extrusion
Ó 2019 Elsevier B.V. All rights reserved.
Microstructure
Texture
Plasticity

1. Introduction extrusion and compression (CEC), equal channel angular process-

Mg alloys are considered as the very promising candidate of
biomaterials due to their outstanding biocompatibility, biodegrad-
ability and appropriate mechanical properties [1]. The plasticity is
very important especially for biodegradable vascular stents which
need to crimp on a balloon and then expand with large deforma-
tion during implantation. But generally, Mg alloys exhibit poor
ambient temperature deformability because of the hexagonal
close-packed (HCP) crystal structure, which only two independent
basal slip systems can be activated normally. That leads to signifi-
cant difficulty to fabricate Mg alloys micro-tubes with high plastic-
ity for biodegradable stents applications.
One effective way to improve the plasticity of Mg alloys is to
facilitate the non-basal slips. Firstly, non-basal slips could be
greatly affected by alloy constitution. Trace Zn addition for Mg-
Nd-Zn-Zr alloy was beneficial for non-basal slips [2]. Hence, Mg-
Nd-Zn-Zr (denoted as JDBM) shows good mechanical properties
and great potential as the next generation vascular stent material
[3,4]. In addition, non-basal slips also could be improved by grain
refinement. Severe plastic deformation processing such as cyclic
⇑ Corresponding authors at: National Engineering Research Center of Light Alloy
Net Forming and Key State Laboratory of Metal Matrix Composites, Shanghai Jiao
Tong University, School of Materials Science and Engineering, Shanghai Jiao Tong
University, Shanghai 200240, China.
E-mail addresses: huangh@sjtu.edu.cn (H. Huang), gyyuan@sjtu.edu.cn (G. Yuan).
ing (ECAP) and double extrusion is very effective on grain refine-
ment [5–9]. And double extrusion for JDBM alloy has been
studied to obtain an alloy bar [9]. The research results confirmed
that the microstructure of JDBM alloy bar was refined significantly,
which contributed to the enhanced strength and plasticity. There-
fore, in this study, double extrusion with a large plastic deforma-
tion was conducted to fabricate JDBM alloy micro-tubes with
high plasticity for vascular stents.
2. Experimental procedure
JDBM (Mg-2.1Nd-0.2Zn-0.5Zr in wt. %) alloy ingot with a
dimension of 100 mm in diameter was produced by the semi-
continuous casting technology (casting temperature 700 °C and
casting speed 90 mm/min). The ingot was solution treated at
540 °C for 8 h and then machined into the billets with the dimen-
sion of 90 mm in diameter and 300 mm in height. These billets
were insulated at 350 °C for 30 min and then extruded at this tem-
perature by the 800 T horizontal extruder with an extrusion ratio
of 36:1 to obtain cylindrical bars with a diameter of 15 mm. The
as-extruded bars were further cut into small billets with the
dimension of 14 mm in diameter and 17 mm in height with a hole
in the center. The dimension of the hole is 3.1 mm in diameter.
These billets were insulated at 380 °C for 30 min. Finally, seamless
micro-tubes could be fabricated successfully by the 80 T vertical

https://doi.org/10.1016/j.matlet.2019.02.114
0167-577X/Ó 2019 Elsevier B.V. All rights reserved.
156 W. Lu et al. / Materials Letters 245 (2019) 155–157

extruder with second extrusion at 380 °C. The dimension of the
micro-tubes is 3.5 mm in outer diameter and 0.25 mm in thickness.
The second extrusion ratio is about 57:1. Hence, there is a large
plastic deformation during the fabrication of micro-tubes.
The specimens for electron backscattered diffraction (MIRA3
scanning electron microscope (SEM) & QXFORD NordlysMax3
EBSD) analysis were cut from the cross sections and mechanically
polished and chemically etched with acid solution (5 ml nitric acid,
15 ml acetic acid, 60 ml ethanol and 20 ml distilled water). The
texture data was analyzed by CHANNEL5.0 software. Tensile spec-
imens with an overall length of 70 mm and a gauge length of
20 mm as a function of ASTM standard (ASTM E8M-04) were pre-
pared from the as-extruded bar and micro-tubes. The tensile test
was performed on a Zwick/Roell Z100 material test machine at
an initial strain rate of 1  10 3 s 1 at ambient temperature. The
tension axes were kept parallel to the ED. The surface morpholo-
gies of fractured tensile specimens were examined by VEGA 3
XMU (LaB6) SEM and the surfaces of observed specimens were pol-
ished and etched before the tensile test.
for the prismatic and pyramidal slips tends to increase after double
extrusion (0.26–0.38 and 0.27–0.36, respectively), which indicates
that non-basal slips became more easily activated for micro-tubes.
Fig. 2 shows the representative ambient temperature tensile
engineering stress versus strain curves of the as-extruded bar
and micro-tubes. Yield strength (YS), ultimate tensile strength
(UTS) and elongation increase by 146%, 52% and 112% after double
extrusion, respectively. In addition, the tensile curve of the as-
extruded micro-tubes shows a more obvious yield phenomenon
than the as-extruded bar. According to the previous study, the
stress-drop phenomenon is associated with rapid increase of the
density of mobile dislocation, which is ascribed to the enhanced
activation of non-basal slip systems [10,11]. The double-extruded
JDBM alloy bar with finer grains also shows a more obvious yield
plateau [9]. Grain refinement can inhibite twinning and facilitate
activation of non-basal slips [10,12]. Hence, the obvious yield pla-
teau on the tensile curve of the as-extruded bar may be resulted

3. Results and discussion

Fig. 1a shows the products of fabrication process, including as-

extruded bar, hollow billets and as-extruded micro-tubes. The
inverse pole figure (IPF) maps (Fig. 1a and b) indicate that both
the as-extruded bar and micro-tubes obtain a nearly homogeneous
microstructure. The average grain size of the as-extruded bar and
micro-tubes are 14 lm and 2 lm, respectively, indicating the
great grain refinement after double extrusion. The Schmid factor
 > basal slip, (1100)
(SF) distribution of the (0001) <1120  
<1120>
prismatic slip and (1122) <1 123>
 pyramidal slip for the as-
extruded bar was shown in Fig. 1c–e, and for the as-extruded
micro-tubes was shown in Fig. 1f–h, respectively. The average SF
value of basal slip is 0.42 and 0.27 for the as-extruded bar and
micro-tubes, respectively. The (0001) pole figures (inserted in
Fig. 1c and f) also indicate that typical basal texture was formed
and the intensity tends to be strengthened after double extrusion Fig. 2. The representative engineering stress vs strain curves of as-extruded bar and
(3.46–4.59), which is not beneficial to basal slip. However, the SF micro-tubes and the list of the mechanical properties.

Fig. 1. (a) The photos of as-extruded bar, hollow billets and as-extruded micro-tubes; IPF map for the as-extruded (b) bar and (i) micro-tubes; SF of (c) basal slip (d) prismatic
slip and (e) pyramidal slip for the as-extruded bar; SF of (f) basal slip (g) prismatic slip and (h) pyramidal slip for the as-extruded micro-tubes.
 W. Lu et al. / Materials Letters 245 (2019) 155–157
Fig. 3. Surface morphologies of fractured tensile specimens for as-extruded (a) bar and (b) micro-tubes.
from the more suffcient activation of non-basal slips during the
deformation.
According to the reported critical resolved shear stresses (CRSS)
data for different slip systems in single crystal Mg, the CRSS of pris-
matic and pyramidal planes is approximately 100 times than that
of a basal slip system at ambient temperature [13–16]. However,
only two independent basal slip systems are available at ambient
temperature while five independent systems are needed for homo-
geneous deformation according to von Mises criterion [17]. Twin-
ning and/or non-basal slip may be activated. In this study, the
surface morphologies of fractured tensile specimens were
observed, and the results were shown in Fig. 3. Basically no twin-
ning can be found and the crack originated from the grain bound-
aries for the both tensile samples. Numerous slip lines can be
observed, and more intensive slip lines for the micro-tubes indi-
cated that slips become more sufficient after double extrusion. In
addition, most of the slip lines kinking reveals the activation of
numerous non-basal slips. Therefore, the excellent plasticity
of the as-extruded micro-tubes is attributed to the activation of
numerous non-basal slips.
Generally, the non-basal slips activation is mainly affected by
the grain size and orientation for a particular Mg alloy. Grain
refinement was reported to be able to enhance the activition of
non-basal slip systems [10]. In this study, the grain size is greatly
decreased to one seventh of the original size after double
extrusion, which can be contributed to the more activation of
non-basal slips. And for grain orientation, the SF for non-basal slip
systems become higher after double extrusion (Fig. 1), which
indicates that the non-basal slips become easier to be activated.
Therefore, the enhanced plasticity of the as-extruded micro-tubes
can be largely ascribed to the easier activation of non-basal slips.
4. Conclusions
JDBM micro-tubes with high plasticity were successfully fabri-
cated by double extrusion with a large plastic deformation. The
elongation increased from 23% for as-extruded JDBM bar to about
48.8% for as-extruded JDBM micro-tubes because of the enhanced
activation of non-basal slips contributed by the significant grain
157
refinement. This achievement of high-ductile micro-tubes is of
great significance for Mg alloy used as the next-generation
biodegradable cardiovascular stents material.
Conflicts of interest
The authors declare no conflict of interest.
Acknowledgements
This work was supported by the National Key Research and
Development Program of China (2016YFC1102401), the National
Natural Science Foundation of China (No. 51501110, and
51501115), the Science and Technology Commission of Shanghai
Municipality (No. 17XD1402100, 17440730700, 18441908000)
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