Acta Biomaterialia 9 (2013) 8604–8610

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Acta Biomaterialia
journal homepage: www.elsevier.com/locate/actabiomat

The processing of ultrafine-grained Mg tubes for biodegradable stents q

Qiang Ge a, David Dellasega b, Ali Gökhan Demir a, Maurizio Vedani a,⇑
a
Department of Mechanical Engineering, Politecnico di Milano, 20156 Milan, Italy
b
Department of Energy, Politecnico di Milano, 20156 Milan, Italy

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

Article history: An investigation was carried out on equal-channel angular pressing (ECAP) and extrusion processing of a
Available online 17 January 2013 ZM21 Mg alloy to obtain an improved candidate material for the manufacturing of biodegradable Mg
stents. Ultrafine-grain size billets of the ZM21 alloy were obtained by two-stage ECAP aimed at achieving
Keywords: an initial refining of the structure at 200 °C and then reaching the submicrometer grain size range by low-
Biodegradable stent ering the processing temperature down to 150 °C. The investigation revealed a significant improvement
ECAP in the properties of the ECAP-treated samples compared with the starting coarse-grained ZM21 alloy. The
Ultrafine grains
0.2% yield strength rose from 180 to 340 MPa after 150 °C ECAP processing, while maintaining a fairly
Mg alloy
Extrusion
high tensile ductility. The ultrafine ZM21 alloy billets were then used for the extrusion of stent precursors
having the form of small-size tubes. The grain size after extrusion remained in the submicrometer range
while the hardness was revealed to be significantly higher than that of the coarse-grained ZM21 Mg alloy.
It was demonstrated that processing of biodegradable Mg stent having an ultrafine-grained microstruc-
ture by ECAP and low-temperature extrusion is feasible and that the obtained products feature promising
properties.
Ó 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

1. Introduction
Magnesium and its alloys are promising materials for biode-
gradable vascular stents owing to their relatively low corrosion
resistance in human body fluids and their good biocompatibility
[1–4]. However, studies have also revealed that the rapid corrosion
rate of conventional magnesium alloys causes premature loss of
stent mechanical properties. The most effective way to enhance
both the mechanical properties and the corrosion resistance of
engineering magnesium alloys is to add specific alloying elements
such as Li and rare-earth (RE) elements [5–7]. However, the toxic-
ity of these alloying elements in a biomaterial is still a controver-
sial issue among biomedical scientists [2,3,8]. Microstructural
refinement is an alternative effective way for increasing both the
mechanical properties and corrosion resistance of Mg alloys, espe-
cially when exploiting severe plastic deformation techniques to
produce ultrafine-grained (UFG) materials featuring a submicrom-
eter grain size [9–12]. Moreover, the achievement of superplastic
properties induced by the marked grain refinement could enhance
the formability at elevated temperature, allowing easier produc-
tion of miniaturized devices [13,14].
q
Part of the Biodegradable Metals Conference 2012 Special Issue, edited by
Professor Frank Witte and Professor Diego Mantovani.
⇑ Corresponding author. Tel.: +39 02 2399 8230; fax: +39 02 2399 8644.
E-mail address: maurizio.vedani@polimi.it (M. Vedani).
Recent studies by Alvarez-Lopez et al. [10] and Argade et al. [15]
reported that in a AZ31 Mg alloy the best corrosion behavior in
phosphate-buffer solution (PBS) could be achieved after extensive
grain refinement by equal-channel angular pressing (ECAP), as re-
vealed by the lower initial corrosion potential and the higher
charge transfer resistance values at long immersion periods. The
UFG microstructure also showed the highest polarization resis-
tance and the most positive pitting and repassivation potentials
as compared to coarse-grained microstructures.
The experimental investigation described in this paper is fo-
cused on a ZM21 Mg alloy selected with the aim of exploring an al-
loy system preferentially formed by non-toxic elements, thus
preserving the highest levels of biosafety and biocompatibility. It
is reported that Ca, Zn and Mn in fairly low concentrations do
not produce harmful effects (these elements are actually essential
for the human metabolism) [2,8,16], whereas elements such as Al,
Zr, Y and other RE elements that are used in other commercial Mg
alloys to improve strength and corrosion resistance may give un-
wanted effects when released into the human body at high rates
[2–4,17].
The strategy of a significant grain refinement to improve both
strength and corrosion behavior was here exploited by adopting
ECAP to produce an UFG ZM21 alloy. The UFG billets were then di-
rectly used to produce small tubes by a warm extrusion process,
followed by laser cutting to produce UFG Mg stent prototypes.
The microstructure obtained after ECAP and extrusion as well as
the mechanical properties achieved are here investigated to supply

1742-7061/$ - see front matter Ó 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.actbio.2013.01.010
 Q. Ge et al. / Acta Biomaterialia 9 (2013) 8604–8610
information about possible processing routes for improved Mg bio-
degradable stents featuring a UFG structure.
2. Materials and methods
A ZM21 (Mg–1.78Zn–0.89Mn, wt.%) wrought alloy was selected
for this investigation. Cylindrical specimens 10 mm in diameter
and 150 mm long were machined from commercial extruded bars.
The die used for ECAP processing featured two channels intersect-
ing at an angle of 110° with an angle of 20° as the outer arc of cur-
vature. According to the Iwahashi equation [18], this geometry
generates an equivalent plastic strain of 0.76 per pass. The die
was heated by four electrical resistance heaters distributed evenly
around the vertical channel and at the intersection point of the two
channels. The ZM21 alloy samples were subjected to repetitive
pressings by ECAP according to route Bc, which consists of rotating
the samples by 90° in the same direction after each pass [19]. Sam-
ples were sprayed with MoS2 lubricant and pressed into the ECAP
die at a speed of 30 mm min1. A first set of ECAP passes was car-
ried out at 200 °C for up to eight passes. Selected specimens were
additionally subjected to a second set of pressings conducted at a
lower temperature of 150 °C for up to eight passes. For comparison
purposes, some specimens were directly pressed at 150 °C.
Following the stage of microstructure refining by ECAP, extru-
sion was performed to produce small tubes as stent precursors. A
laboratory set-up already described in detail in a previous study
was adopted to perform extrusion under controlled conditions
[20]. The schematic view of the extrusion die is depicted in
Fig. 1. Extrusion was carried out at temperatures ranging from
150 to 350 °C starting from the ECAP-processed billets in order
to study the effects of temperature on formability and grain
growth. The formed tubes had an outer diameter of 4 mm and an
inner diameter of 2 mm, corresponding to a reduction ratio of 8:1.
Microstructure characterization was performed by optical
microscopy (OM) and field emission gun scanning electron
Fig. 1. Schematic set-up of the extrusion die for small-size tubes.
8605
microscopy (FEG-SEM) on samples sectioned along their axial
direction after ECAP and after extrusion. The grain size was evalu-
ated by ASTM E112-96 standard according to the linear intercept
procedure. The structure of the extruded tubes was evaluated con-
sidering samples extracted from the die after interrupted extrusion
trials, where the billet region and the tube region could also be
investigated (see Fig. 1). In the former region the effects related
to high-temperature holding could be assessed, while in the latter
the combined action of temperature and plastic deformation could
be evaluated in a single sample. Mechanical properties after ECAP
treatment were evaluated on tensile test specimens with a gauge
length of 12 mm and a diameter of 4 mm. Due to size limitations,
the properties of the extruded tubes were estimated only by Vick-
ers microhardness tests (load on the indenter of 1 N) on longitudi-
nal sections of the tubes.
To complete our evaluation of the processability of the UFG Mg
alloys for stent applications, the tube outer diameters were re-
duced to 2.4 mm by turning, to achieve a common stent thickness
of 0.4 mm. A stent net was then generated on the ECAP-processed
and extruded tubes by laser cutting under an active fiber laser
source, operating in the nanosecond pulse regime with 7 W aver-
age power and beam spot of 19 lm. This allowed microcutting
with small kerf widths to be produced across the tube walls. Chem-
ical etching was then performed in a HNO3/ethanol solution under
ultrasonic conditions to remove the cutting dross and to obtain a
stent prototype in a semifinished form.
3. Results
In order to generate a very fine microstructure in Mg alloy bil-
lets, the ECAP process has to be performed at as low a temperature
as possible. However, processing the starting billets directly at
150 °C led to extensive cracking due to lack of ductility of the ori-
ginal coarse-grained structure, as shown in Fig. 2. Increasing the
processing temperature to 200 °C significantly improved the alloy
formability and allowed defect-free billets to be obtained. Further
tests showed that, once the alloy structure has been refined,
namely after processing at 200 °C for eight passes, the billet could
be successfully deformed by ECAP even at 150 °C without damage,
thus further improving the refinement effect.
The evolution of the grain size with ECAP processing at the two
temperature levels investigated here is depicted in Fig. 3. The ori-
ginal coarse-grained structure was gradually refined by increasing
the number of passes (from Fig. 3a–d). From these images it can be
inferred that the deformation microstructure after a limited num-
ber of passes was generally heterogeneous since relatively coarse
islands of the original grains were still visible (up to six passes at
200 °C, see Fig. 3b and c). Eventually, a homogeneous fine-grained
microstructure completely replaced the coarse grains after eight
passes (Fig. 3d). The grain size could be further reduced by an addi-
tional set of ECAP passes carried out at a lower temperature of
Fig. 2. View of the ZM21 alloy after ECAP processing at 150 and at 200 °C.
8606 Q. Ge et al. / Acta Biomaterialia 9 (2013) 8604–8610

Fig. 3. Microstructural evolution of ZM21 alloy after ECAP processing at different temperatures and number of passes: (a) starting material; (b) 200 °C, four passes; (c) 200 °C,
six passes; (d) 200 °C, eight passes; (e) 200 °C, eight passes +150 °C, four passes; (f) 200 °C, eight passes +150 °C, eight passes.

Table 1 micrographs of the processed samples. It is demonstrated that a

Average grain size (linear intercept length, in lm) of the ZM21 alloy as a function of
processing conditions.
refining effect down to a grain size of around 500 nm could be
achieved by fine-tuning the processing parameters.
ECAP passes 200 °C 150 °C (after 8 passes at 200 °C) Fig. 4a and b show representative engineering stress–strain
0 15.0 ± (annealed) curves of the materials processed by ECAP. The corresponding val-
4 0.93 0.52 ues of 0.2% yield strength (YS), ultimate tensile strength (UTS) and
6 0.83 Not available
fracture elongation are summarized in Table 2. It is revealed that a
8 0.75 0.52
significant improvement in strength is achieved after four passes
according to the two-step processing route adopted here. The YS
increased from 180 MPa of the starting alloy up to 340 MPa after
150 °C (Fig. 3e and f). From the micrographs it can be observed that four passes at 150 °C, while the UTS reached a value of 353 MPa
by the above-mentioned combination of ECAP passes and temper- in the same condition against the value of 259 MPa of the original
atures, a UFG structure featuring submicrometer-size equiaxed coarse-grained alloy. The tensile ductility corresponding to this
grains could be obtained throughout the billet volume. Table 1 condition remained at fairly good levels while a lower strain hard-
summarizes the average grain size measured on representative ening ability was recorded from the tensile curves.
 Q. Ge et al. / Acta Biomaterialia 9 (2013) 8604–8610
Fig. 4. Engineering stress–strain curves of the ZM21 alloy ECAP processed at 200 °C
(a) and at 150 °C after eight passes at 200 °C (b).
The above-presented trend of YS and UTS as a function of the
number of ECAP passes at the two temperatures investigated is
also reported in Fig. 5 and compared to the Vickers microhardness
evolution. It can be inferred that the modification of the yield and
tensile strength with ECAP passes and processing temperature per-
fectly matches the evolution of hardness. Indeed, hardness and
strength increased with increasing passes and decreasing temper-
ature up to a maximum value corresponding to four passes at
150 °C, followed by a drop measured after six and eight passes at
150 °C.
The processing condition featuring the best tensile properties
(namely eight ECAP passes at 200 °C followed by four ECAP passes
at 150 °C) was therefore considered as the starting condition for
further warm extrusion tests aimed at producing the small size
tubes required for stent manufacturing. The temperature effects
induced by extrusion in the range from 300 to 150 °C on grain
growth is reported in Fig. 6. The tube extruded at 300 °C experi-
enced a significant grain coarsening and reached a grain size close
to the starting coarse-grained alloy (compare Fig. 6a with Fig. 3a).
Grain coarsening was also detected in billets extruded at 250 and
200 °C, even if to a decreasing extent. On the contrary, no apparent
coarsening effect was observed when extruding at 150 °C, thus
Table 2
Tensile properties of the ZM21 alloy ECAP processed according to different conditions.
200 °C
ECAP passes 0 2
YS (MPa) 180 232
UTS (MPa) 259 283
Fracture elong. (%) 20.0 15.7
8607
Fig. 5. Tensile properties and microhardness evolution of coarse-grained and ECAP-
processed ZM21 alloy.
confirming that the achieved ultrafine grains could be kept almost
stable even after the warm extrusion stage.
Due to geometrical limitations, the strength of the extruded
small-size tubes could only be evaluated by microhardness tests.
Profiles measured along the longitudinal sections of samples ex-
tracted from the die after interrupted extrusion tests are reported
in Fig. 7. All the profiles show a gradual increase in hardness during
the extrusion process (moving from the billet region to the tube re-
gion) and a clear increase in hardness as the extrusion temperature
is decreased. It is important to note that when the extrusion tem-
perature was lowered down to 150 °C, holding of the billet into the
die caused a clear hardness drop (compare hardness in billet region
of sample treated at 150 °C to the original hardness of the ECAP bil-
let) which was almost completely counterbalanced by the
improvement generated by the plastic deformation imparted by
extrusion.
The typical surface aspect of a small-size extruded tube after la-
ser cutting and chemical etching is shown in Fig. 8a. The micro-
structure observed near the cutting surfaces, as revealed on
samples sectioned along tube thickness, is reported in Fig. 8b. From
the micrograph it can be suggested that no significant thermal ef-
fects on microstructure stability (e.g. grain coarsening) are gener-
ated by the laser process: the grain size near the cut surface is
reasonably comparable to that of the untreated material.
4. Discussion
According to established theories [21], the mechanism of for-
mation of new grains in metallic alloys deformed by ECAP is char-
acterized by the progressive modification of low-angle cell
boundaries into more stable equiaxed high-angle grain boundaries.
This process is expected to consume a significant fraction of the
mobile dislocations in the material structure with increasing num-
ber of passes, provided that processing is performed at sufficiently
low temperature.
In the low-temperature range, straining of Mg and Mg alloys
mainly occurs by the activation of basal dislocation slip systems
150 °C (after 8 passes at 200 °C)
4 6 2 4 6 8
245 254 285 340 250 239
274 282 312 353 289 268
9.7 11.3 7.8 11.5 5.1 7.2
8608 Q. Ge et al. / Acta Biomaterialia 9 (2013) 8604–8610
Fig. 6. Representative images of the tube grain structure after extrusion at different temperatures: (a) 300 °C; (b) 250 °C; (c) 200 °C; (d) 150 °C.
Fig. 7. Microhardness profiles taken along different regions of samples subjected to
interrupted extrusion tests.
[22] but the large shear strain imparted by ECAP on the coarse
structure often exceeds the fracture limit of the crystals, thus caus-
ing abrupt cracking of billets during processing, as detected in the
present billets processed at 150 °C in a single stage (see Fig. 2). The
strategy of performing a first set of passes at relatively high tem-
perature (e.g. 200 °C) to achieve an initial substantial reduction
in grain size and then completing the refinement in the UFG re-
gime at 150 °C by a second set of passes was revealed to be suc-
cessful. The increased number of crystals after the preliminary
refinement could better accommodate the severe plastic deforma-
tion process at lower temperature, leading to further fragmenta-
tion of the grains into even finer domains (compare Fig. 3e and
f). It should be noted that a similar approach was adopted previ-
ously by other authors [13,14,23]. For instance, Figueiredo and
co-workers [23] successfully processed a ZK60 Mg alloy by hot
extrusion to refine the grain size before ECAP. According to these
researchers, the refinement was accompanied by an increase in
strain-rate sensitivity and a lower tendency for cracking and seg-
mentation during ECAP.
The evaluation of material strength by reduction of the grain
size in polycrystalline metallic alloys is usually performed consid-
ering the Hall–Petch equation:
ry ¼ r0 þ k1 D1=2 ð1Þ
where ry is the resulting yield stress, r0 and k1 are material con-
stants and D is the average grain size. Several studies have already
confirmed that reducing the grain size of Mg alloys results in higher
strength, both in coarse-grained and in ECAP-processed UFG mate-
rials [24,25]. Consistently, in the present study, the yield strength of
the ECAP-treated ZM21 alloy generally improved with increasing
passes and refinement of the grain size. However, it was also re-
vealed that after four passes at 150 °C the strength clearly de-
creased with further passes.
It must be considered that the Hall–Petch relation evaluates
grain size effects supposing that no changes in texture occur during
refining. For a more precise evaluation of tensile properties, texture
effects induced by ECAP should also be evaluated, as already done
by Kim et al. [26]. These authors reported that for an AZ61 alloy the
yield strength decreased significantly after eight ECAP passes (die
channel angle of 90°). The strength drop was attributed to the
development of a new texture that gradually developed starting
from the original extruded material by repetitive ECAP processing.
These authors stated that the dominant texture after eight passes
was (1 0 1 1)[0 1 1 1] +(1 0 1 2)[1 2 1 0], and hence the basal
plane turned out to be more favorably oriented for slip and a lower
stress was therefore required for macroscopic yielding. Also in the
present investigation it could be supposed that the ZM21 alloy pro-
cessed at 150 °C by ECAP is affected by a texture softening effect
after for passes at 150 °C that was apparently dominant over the
grain-size strengthening. Further studies are currently in progress
for a more detailed evaluation of this effect.
The consistency between the hardness and the yield strength
profiles plotted in Fig. 5 suggests that microhardness can reason-
ably approximate the yield stress variation experienced during
processing of the ZM21 alloy, so that the hardness evolution after
extrusion in different regions of the extrudates can supply a reli-
able means to assess the strength of the small-size tubes for
 Q. Ge et al. / Acta Biomaterialia 9 (2013) 8604–8610
Fig. 8. Views of the extruded tube surface after laser cutting and chemical etching (a) and microstructure revealed from a section near the laser-cut surface (b).
Fig. 9. Microstructure of billet material after holding at a set temperature before extrusion: (a) 200 °C; (b) 150 °C.
biodegradable Mg stents. From Figs. 5 and 7 it can be suggested
that the grain refinement of the ZM21 alloy in the UFG range can
bring about an increase in hardness from 50 to 74.8 HVn (after
ECAP) and that this value can be maintained (or better recovered)
even after extrusion at 150 °C to produce high-strength stent pre-
cursors. It is also believed that the higher formability shown by the
recorded lower loads and integrity of the samples during warm
extrusion might be inherited by the contribution of enhanced
superplastic formability induced by the extensive grain refine-
ment. Matsubara and co-workers [13] have already published a
research work on low-temperature and high strain-rate
superplasticity, achieving for a Mg–9%Al alloy tensile elongations
of 800% at 150 °C with a strain rate of 1.0  104 s1 and 360% at
225 °C with a strain rate of 1.0  102 s1.
Finally it must be considered that the UFG microstructure of a
polycrystalline material after ECAP is usually far from the thermal
equilibrium state and that the grains are apt to rapidly grow during
heating. This behavior was also noticed during extrusion. As de-
picted in Fig. 9a, the simple holding time of about 10 min at
200 °C, which corresponds to the heating stage to set temperature
of the billets before extrusion, promoted significant grain growth.
Lowering the temperature down to 150 °C dramatically reduced
this effect but from careful observation of Fig. 9b it can be inferred
that some distinct grains showed evidence of coarsening in the bil-
let region. However, the subsequent extrusion process was able to
counterbalance this process by promoting dynamic recrystalliza-
tion phenomena, as suggested by the microstructure evolution de-
tected in the present study and already confirmed in the literature
by other researchers [27].
5. Conclusions
An investigation was carried out on properties and processing
of UFG ZM21 Mg alloy as a possible candidate material for the
manufacturing of improved biodegradable Mg stents.
8609
1. ECAP was used to achieve a significant grain refining in the sub-
micrometer grain-size range. Processing was performed accord-
ing to a two-step strategy aimed at achieving a first refining of
the structure at 200 °C and then reaching the UFG grain size
range by lowering the processing temperature down to 150 °C.
A homogeneous equiaxed grain structure featuring a submi-
crometer grain size of about 500 nm was successfully achieved.
2. The mechanical characterization revealed a significant
improvement of properties of the ECAP-treated billets com-
pared to the starting coarse-grained ZM21 alloy. The 0.2% yield
strength rose from 180 to 340 MPa after 150 °C ECAP process-
ing, keeping a fairly high tensile ductility.
3. The UFG ZM21 alloy billets were then used for the extrusion of
stent precursors at 150 °C having the form of small tubes with
4 mm outer and 2 mm inner diameters. The grain size after
extrusion was in the submicrometer range owing to low-
temperature processing and to the contribution of dynamic
recrystallization. Consistently, hardness improved from 50 HVn
for the coarse-grained alloy to 74.8 HVn for the UFG extruded
tubes.
4. The stent net was then obtained by using fiber laser cutting
starting from the above UFG precursors. No significant
modification of the microstructure was detected close to the
laser-cut surfaces, thus demonstrating that processing of biode-
gradable Mg stents with a UFG microstructure is feasible and
that the obtained products feature promising properties. In par-
ticular, the improved mechanical properties can offer new
opportunities for the design of stents and the use of UFG metals
could widen the range of alloy compositions that can be
selected for this specific application.
Acknowledgement
The authors would like to thank Fondazione CaRiTRO for par-
tially funding the research under Grant number 2011.0250.
8610 Q. Ge et al. / Acta Biomaterialia 9 (2013) 8604–8610
Appendix A. Figures with essential color discrimination
Certain figures in this article, particularly Figs. 1 and 2, are dif-
ficult to interpret in black and white. The full color images can be
found in the on-line version, at http://dx.doi.org/10.1016/
j.actbio.2013.01.010.
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