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org
Medical Device Materials III
Proceedings of the Materials & Processes for Medical Devices Conference (#05153G)

MICROSTRUCTURAL CHARACTERIZATION OF Ni-Ti VASCULAR STENTS

A. Toro
National University of Colombia, Medellin, Columbia

W. Van Geertruyden
EMV Technologies, LLC, Bethlehem, PA USA

W.Z. Misiolek
Institute for Metal Forming, Lehigh University, Bethlehem, PA USA

X.D. Han
Institute of Microstructure & Property for Advanced Materials, Beijing University of Technology, Beijing, P.R. China

M.H. Wu
Memry Corporation, Bethel, CT USA

Abstract
A detailed study of the microstructural features in Ni-Ti stents
was performed, which included TEM examination to
determine the grain structure and precipitation kinetics after
heat treatment of the stent tube. The samples were extracted
from vascular stents, as well as from the tubes used in early
stages of the production process. The Focused Ion Beam (FIB)
equipment was used for preparation of TEM samples.
The specimens were analyzed at different stages of the stent
production process, such as laser cutting and shape setting,
and correlations between the microstructure and the
manufacturing process were established. Characterization of
the main morphologic features of the material was based on
TEM imaging, and the effect of the different processing steps
on the crystallographic texture was determined by adequate
selection of different sample locations.
Introduction
Ni-Ti alloys have been successfully used for manufacturing
self expanding vascular stents, which assist the vessel
expansion in superficial artery applications and behave more
reliably than balloon expandable stents made with stainless
steel [1]. The advantages of Ni-Ti alloys are related not only
to superelasticity and shape memory effect, but also to their
tissue and blood biocompatibility, corrosion resistance, stress-
strain behavior similar to that of hard living tissues, the
possibility of applying a constant stress for a wide range of
strain levels, assistance to fracture healing without application
of undue forces, among others [2,3].
Self expanding stents are “crush resistant”, which means that
there is an extended limit to the deformation they can undergo
as a consequence of the application of radial strength, since
they are able to recover to the original shape. On the other
hand, balloon expanding stents are designed for a maximum
radial strength they can endure without collapsing or buckling
[1]. These exceptional deformation properties of Nitinol stents
are related to the selective habit plane variants and twinning
modes that are possible during the stress induced-martensitic
transformation, as well as to the low elastic anisotropy, very
small grain size and the constant critical tensile stress for the
stress induced martensitic transformation [4].
It has been claimed by several authors that the <011> type II-
twinning mode is the dominant one in monoclinic B19’
martensite, which is characterized by rotational symmetry
with respect to a 2-fold axis in the parent phase [5,6].
{011}Type I-twinning mode, in which mirror symmetry with
respect to one invariant plane is observed, as well as (001)
compound twinning are also commonly found in Ni-Ti
martensite [7-9]. Furthermore, de-twinning of these variants
occur when the martensite is deformed, and usually only one
remains after high strain levels.
Since vascular stents are designed to remain permanently in
the human body, their microstructure has to be carefully
controlled to assure that mechanical properties and
biocompatibility will be maintained. Unfortunately, any
manufacturing procedure causes microstructural changes that
have to be considered in order to keep the stent properties. In
the case of laser cutting, a heat affected zone (HAZ) and a
recast layer with micro-cracks have been observed [10], but no
systematic study of the relationship between the processing
parameters and microstructure has been published.

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Medical Device Materials III
Proceedings of the Materials & Processes for Medical Devices Conference (#05153G)

The microstructural changes induced in the recast layer and
HAZ will depend on the chemical composition of the stent, the
cutting parameters and the thermal and mechanical history of
the alloy. The R-phase has also been found in Ni-Ti alloys
with a high density of rearranged dislocations in the parent
phase, which can be formed after cold working of the material
followed by annealing at proper temperatures, and in Ni-rich
Ti-Ni alloys containing Ti3Ni4 precipitates [6].
remove the thin foils from the tubes (Figure 1a), while in the
stents the specimens were extracted from regions of maximum
curvature (Figure 1b), since a significant effect of laser cutting
on the microstructure is expected in this area. An SEM image
showing the extraction process is shown in Figure 1c.

The analysis of diffraction patterns from areas in which the

parent phase and the martensite coexist have led several
authors to affirm that there is a lattice instability preceding the
B2-B19’ transformation, and in some cases this pre-
martensitic stage has been associated to the formation of R-
phase. However, recent developments have led to the
conclusion that the formation of R-phase from parent phase
B2 is a martensitic transformation itself [6]. Generally
speaking, the presence of R-phase is related to the occurrence
of reflections along the 1/3<110>B2 and 1/3<111>B2 directions a) b)
of the parent phase in reciprocal space, and the B2-R-phase
transformation is characterized by a sharp increase of
electrical resistivity with a very small temperature hysteresis.

In this work, a study of the effect of laser cutting on the

microstructure of vascular stents is performed. The analysis is
focused on the microstructure in the region close to the laser-
cut surface, which includes the recast layer and the heat
affected zone.

Procedure

Stent samples were laser machined from cold drawn and heat
treated NiTi tube of Ti-55.8wt.%Ni composition using a Nd c)
YAG pulse laser of 1062nm in wave length.
Figure 1: a) TEM sample location from a tube b) TEM sample
Optical Microscopy Analysis location from a stent and c) SEM image of sample extraction.
Pre-cut tubes as well as laser cut and expanded stents were
prepared metallographically for Light Optical Microscopy
(LOM). The samples were etched (10% HF, 40% H2SO4, Results
50% H20) to reveal the microstructure. An LOM image from the surface of the as-cut stent is shown
in Figure 2. It can be seen that the surface revelas the recast
TEM Examination layer where small microcracks are present (Figure 3). These
microcracks were primarily present at the apex of the strut
Ni-Ti tubes and stents were analyzed in a JEOL 2000FX TEM rather than along the strut itself. Additionally, the microcracks
(LaB6 electron source) operating at 200 KV. The specimens generally extended within the recast region.
were prepared in a FEI Focused Ion Beam Microscope, in
which high-energy Ga-ions (30 KV acceleration voltage)
strike the sample in a controlled manner. The process allowed
homogeneous samples with less than 100 nm in thickness,
with no thermal or mechanical stresses induced to be
produced.

The samples were extracted from tubes as well as from as-cut

and expanded stents. No preferential location was selected to

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© 2006 ASM International. All Rights Reserved. www.asminternational.org
Medical Device Materials III
Proceedings of the Materials & Processes for Medical Devices Conference (#05153G)

a)

Figure 2: LOM micrograph showing micro-cracks (arrows)

within the recast layer after laser cutting.

Tube Microstructures

Figure 3 shows a typical microstructure in the as-drawn tube

while Figure 4 represents the typical microstructure of the
tube at higher magnification via the TEM technique.
Deformation bands, 20 to 100 nm in width can be observed,
although in some areas a sub-grain structure is also present
(Figure 5). The diffraction patterns obtained revealed the b) [111]B2
presence of cubic parent phase B2 and possibly monoclinic
martensite B19’. Neither 1/3 <110> reflections (which are
associated to R-phase formation) nor Ti3Ni4 diffraction spots
Figure 4: a) Tube microstructure showing B2 austenitic
were observed in the patterns.
grains and b) its corresponding diffraction pattern.

100 Pm
Figure 3: LOM micrograph showing a ttypical tube
microstructure. Figure 5: LOM micrograph showing a typical tube
microstructure.

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© 2006 ASM International. All Rights Reserved. www.asminternational.org
Medical Device Materials III
Proceedings of the Materials & Processes for Medical Devices Conference (#05153G)

As-cut Stent Microstructure

The results of the as-cut stent tube microstructures at the edge

and greater than 10Pm from the edge can be summarized as
follows:

For distances to the edge smaller than 3 µm (within the recast

layer) the microstructure is composed of recrystallized,
almost-equiaxed grains of parent phase B2 with mean size up
to 400 nm. Figures 6 and 7 show the typical microstructure of
this region.

For distances to the edge between 4 and 8 µm the

microstructure is also composed of smaller austenite grains a)
and there is a marked contrast due to dislocations. Figure 8
shows the characteristic morphology and a diffraction patterns
for the parent phase found in this area. 002
For a distance to the edge larger than 10 µm, B2 parent phase
and possibly B19’ martensite were identified. Bands were
also observed inside the grains, which are most likely caused
by plastic deformation. 110

Figure 9 shows the typical microstructure of this region. It is 000

unclear based on this image and its diffraction pattern whether
the structure is B2 austenite or B19’ martensite. Further
examination of the diffraction pattern is needed to confirm the
lattice structure.
b) [110]B2
Expanded Stent Microstructure
Figure 6: a) As-cut stent microstructure less than 3 Pm from
Figure 10 shows the microstructure of the expanded stent in a the edge and b) its corresponding diffraction pattern showing
region located 5 µm far from the edge of the sample. Parent B2 parent phase grains.
phase B2 and austenite were observed. The diffraction patterns
in 10a corresponds to the areas I and II in figure 10b,
respectively. The diffraction pattern shown in Fig. 10b can be
indexed as type II twins. The electron beam was parallel to
[112]Matrix || [121]Twin. Figure 11 shows the microstructure of
the expanded stent far from the cutting surface. The structure
consists of B2 Austenite with high strain levels related to high
density of dislocations.

Figure 7: As-cut stent microstructure less than 3 Pm from the

edge showing an equiaxed microstructure of B2 austenitic
grains.

66
© 2006 ASM International. All Rights Reserved. www.asminternational.org
Medical Device Materials III
Proceedings of the Materials & Processes for Medical Devices Conference (#05153G)

a)
a)

011
021M

000 101 111M,T

000
101T

b) [111]B2 b) [112]M //[121]T

Figure 8: As-cut stent between 4 and 8Pm from the edge

Figure 10: a) Expanded stent 5Pm from the edge and b) its
showing B2 austenitic grains with high levels of strain.
corresponding diffraction pattern.

Summary and Conclusions

The microstructures found within the analyzed material can be

summarized as follows. The as-drawn tube contained
primarily B2 austenite microstructure with a high dislocation
density likely resulting from cold work. Within the as-cut
stent, the edge of the sample contained strain free B2
austenitic grains In the region greater than 10 Pm from the
edge the microstructure consisted of B2 austenite or possibly
B19’ martensite structure while bands were also observed
inside the grains, which are most likely caused by plastic
deformation. Within the region of 4 to 8 Pm from the edge, a
B2 austentic structure with high dislocation density was
observed.

Figure 9: As-cut stent greater than 10Pm from the edge

showing either B2 austenite or B19’ martensite.

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© 2006 ASM International. All Rights Reserved. www.asminternational.org
Medical Device Materials III
Proceedings of the Materials & Processes for Medical Devices Conference (#05153G)

References

1. Duerig, T.W. and Pelton, A.R., Materials Science Forum

Vols. 394-395 (2002) 1-8.

2. Trepanier, C., Pelton, A.R., Proceedings of the Materials &

Processes for Medical Devices Conference, 8-10 Sept 2003,
Anaheim, CA, ASM International, p. 176-179.

3. Shabalovskaya, S.A., Bio-medical materials and

engineering 12 (2002) 69-109

4. Otsuka, K., Ren, X., Intermetallics 7 (1999) 511-528.

a)
5. Nishida, M., Yamauchi, K., Itai, I., Ohgi, H., Chiba, A.,
Acta Materialia 43 (1995) 1229.

6. Otsuka, K., Ren, X., Progress in Materials Science 50

(2005) 511-678.

7. Kim, J.I., Liu, Y., Miyazaki, S., Acta Materialia 52 (2004)

487-499

8. Liu, Y., Xie, L., Van Humbeeck, J., Delaey, L., Acta
Materialia Vol. 47 N. 2 (1999) 645-660.

9. Xie, Z., Liu, Y., Van Humbeeck, J., Acta Materialia Vol. 46
N. 6 (1998) 1989-2000.

b) 10. Dickson, T.R., Moore, B., Toyama, N., Materials Science

Forum Vols. 394-395 (2002) 309-312.

Figure 11: a) Expanded stent 10Pm from the edge and b) its
corresponding diffraction pattern.

In this study, it was found that a there is a significant

microstructure gradient in the vicinity of the laser cut in
Nitinol stents.

There is a need for more quantitative microstructure analysis

for typical laser cuts in order to establish exact distance from
the cut, which must be removed via electro-chemical means.
This treatment is critical in providing improved fatigue
properties of the Nitinol stents.

Acknowledgements

The authors thank Memry Corporation for donating samples

for this study. Partial support of Dr. Misiolek and funding for
the Loewy Visiting Professorship of Dr. Toro was funded by
the Loewy Family Foundation. Additionally, the authors wish
to thank Mr. Shengcheng Mao for helping indexing part of the
electron diffraction patterns.

68
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