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Abstract
Constitutive laws for shape-memory alloys subjected to multiaxial loading, which are based on direct experimental
observations, are generally not available in the literature. Accordingly, in the present work, tensiontorsion tests are
conducted on thin-walled tubes (thickness/radius ratio of 1:10) of the polycrystalline superelastic/shape-memory alloy
Nitinol using various loading/unloading paths under isothermal conditions. The experimental results show signicant
variations in the mechanical response along the two loading axes. These are attributed to changes in the martensitic
variants nucleated in response to the directionality of the applied loading, as well as to microstructural texture present
in the parent material. Numerical simulations suggest that the characterization and modeling of the microstructure is
of paramount importance in understanding the phenomenology of shape-memory alloys.
2002 Elsevier Ltd. All rights reserved.
Keywords: Shape-memory alloys; Phase transformation; Superelasticity; NiTi; Nitinol; Constitutive behavior; Multiaxial loading
0167-6636/$ - see front matter 2002 Elsevier Ltd. All rights reserved.
doi:10.1016/S0167-6636(02)00310-1
970 J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986
biomedical devices such as endovascular stents, The organization of the article is as follows: the
vena cava lters, dental les, archwires and guide- experimental protocol and the testing setup are
wires, etc. described in Section 2. The experimental results
Both the superelasticity and shape-memory are documented in Section 3. These are followed
eects are induced in Nitinol by reversible, displa- by discussion and comparison to numerical simu-
cive, diusionless, solidsolid phase transforma- lations in Section 4 and concluding remarks in
tions from a highly ordered austenitic (simple cubic, Section 5.
B2) crystal structure to a less ordered martensitic
(B190 , monoclinic) structure. The stress-induced
austenite-to-martensite transformation is eected 2. Experimental procedure
by the formation of martensitic structures which
correspond to system energy minimizers. Although 2.1. Materials
24 variants of the less symmetric martensitic phase
can be formed by the same crystal of parent aust- Nitinol tubing (Ti 49.2 at.%, Ni 50.8 at.%) was
enite, it has been experimentally observed that only received from NDC (Fremont, CA), with a 4.64
a few variants are typically active and fully resolve mm outer diameter and 0.37 mm thickness. The
the stress/shape change (Miyazaki et al., 1989; Gall tubing was cut into 75 mm long specimens and
and Sehitoglu, 1999). During the martensite- ground down along the 25 mm long center test
to-austenite (reverse) transformation, all variants section to an outer diameter of 4.3 mm in order to
transform back to the same parent phase. obtain an hourglass shape and minimize end-
Most of the mechanical testing on polycrystal- eects during testing (Fig. 1). Thus, the wall thick-
line Nitinol found in the literature has been per- ness in the gauge section was reduced to 0.2 mm,
formed on wires and is thus one-dimensional. As a resulting in a thickness-to-radius ratio of approx-
result, most phenomenological constitutive models
are based on uniaxial data, oftentimes extended to
three-dimensions in an ad hoc fashion. Hence,
there is little condence that three-dimensional
models can accurately describe the material re-
sponse under complex loading experienced in
Nitinol devices. Very little information exists on
the multiaxial loading/unloading of Nitinol and
even less on tubes which are used as the starting
material in the manufacture of critical devices such
as endovascular stents; to our knowledge, only
three previous studies, all on thick-walled tubing,
are available (Miyazaki et al., 1989; Lim and
McDowell, 1999; Helm and Haupt, 2001).
The present work focuses on the biaxial testing
of thin-walled tubes chosen to minimize the gra-
dient in the torsional strain along the radial di-
rection. Three distinct biaxial stress-loading paths
are explored under isothermal conditions. The re-
sulting data are compared to the results obtained
by numerical simulation of polycrystalline Nitinol
response based on an extension to polycrystalline
response and to nite deformations of a three-
dimensional single-crystal model by Siredey et al. Fig. 1. Schematic illustration of the NiTi specimen (not to
(1999). scale).
J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986 971
Fig. 3. X-ray diraction analysis of the as received NiTi material showing an essentially fully austenitic structure.
972 J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986
hardened steel pin was inserted into the tube used to determine the rotation in the reduced
throughout the grip region which allowed appli- (gauge) section of the tube:
cation of sucient lateral gripping force to inhibit
slippage during testing. ii(i) The total angular rotation /t of the specimen
Strain rates in the range 105 104 s1 were was measured.
used for both the tensile and torsional loading i(ii) The elastic rotation /e of the thick-walled sec-
in order to avoid rate eects. Due to the two- tion of tubing between the gauge section and
dimensional nature of the loading paths, the strain the grip was calculated based on the length
rates could not be xed for the entire test. For pure of the thick-walled section and the calibrated
tension and pure torsion segments, the strain rate response of a straight thick-walled tube.
during loading/unloading was 104 s1 . During (iii) The rotation of the gauge section / of the
mixed-mode proportional loading/unloading tests, tube was found by subtracting the elastic rota-
the tensile strain rate was xed at 104 s1 , while tion of the (thick-walled) tube section from
the shearing strain rate was adjusted to main- the total measured angular rotation, namely
tain the prescribed loading path. For the material / /t /e .
used in this study, preliminary uniaxial tests using
slower loading rates conrmed that the range of It is noted that when loading in pure torsion
strain rates employed did not aect the measured under xed tensile displacement, a tensile clip
stressstrain response. gauge response was presumed to be due to torsion
All testing was performed at an ambient tem- (i.e., as the tube twists, the gauge might slip
perature of 22 C that was maintained to within slightly). In addition, a constant value of tensile
1 C during any single test. The loading rates strain during pure torsional loading was assumed.
used in the experiments were shown to be su- All axial and torsional loads were measured
ciently low to suppress signicant temperature using a tensiontorsion load cell (Key Transducers
variations during testing (Lim and McDowell, Inc., model 610410, capacity 28 Nm/4500 N for
1995). Indeed, a surface-mounted resistance tem- torsiontensile, respectively).
perature detector used in a tensile loading test at
strain rate of 5 104 s1 recorded a temperature 2.3. Loading program
rise of less than 1.5 C. Hence, all experiments
were deemed to be taking place under essentially In order to investigate thoroughly the complex
isothermal conditions. nature of the forward and reverse transformation
Using thin-walled tubes, three measurements process and its eect on the constitutive properties
are necessary in order to fully characterize the of polycrystalline Nitinol, three specic loading/
strain state of the material: tensile elongation, unloading programs (referred to as Types IIII)
radial elongation, and angle of twist. Tensile were investigated, as outlined below:
elongation was measured using a standard ex-
tensometer mounted over a 13 mm gauge length in Type I (Load in tension followed by torsion, un-
the reduced section of the tube. The extensometer load in reverse orderFig. 6(a))
was attached to the specimen using elastomeric 1. Tensile loading to a particular strain level;
bands. Radial elongation was measured in the re- hold during segments 2 and 3.
duced section using a spring-loaded clip gauge 2. Torsional loading to 2% shear strain.
outtted with a semicircular clamping region. At- 3. Unload shear axis to zero strain.
tempts to mount an angular measurement device 4. Unload tensile axis to zero strain.
directly on the reduced section of the tube were Type II (Load in torsion followed by tension, un-
unsuccessful due to excessive gauge slippage dur- load in reverse orderFig. 6(b))
ing the austenite-to-martensite transformation. 5. Torsional loading to 2% shear strain;
Consequently, angular rotation of the tube was hold during segments 2 and 3.
measured at the grip. The following procedure was 6. Tensile loading to a particular strain level.
974 J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986
3. Results
Fig. 7. Equivalent stressstrain plot showing the repeatability of four separate uniaxial tension tests up to 6% strain.
Fig. 8. X-ray diraction analysis of NiTi material after a complete tension cycle, showing the presence of a small proportion of
residual martensite.
forward transformation occurs under increasing sults in elastic deformation of the fully trans-
strains. Upon completion of the transformation at formed martensite matrix. Unloading of the
approximately 5.75% strain, further loading re- transformed material is initially elastic, followed
976 J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986
by a second plateau region, during which most of posed to equivalent) stressstrain diagram in Fig.
the reverse transformation occurs. Finally, elastic 10, where closure is accurately reproduced.
unloading of the regenerated austenite phase takes
place. The repeatability of the tests appears to be 3.2. Tension followed by torsion (Type I)
adequate with the onset of the transformation
varying between 1.1% and 1.2% strain and the Results of Type I loading experiments involving
transformation plateau stresses lying between 355 tension up to a maximum of 6% strain, followed by
and 380 MPa. These variations may be attributed torsional loading of 2% strain and reverse-order
to the sensitivity of the material to small ambient unloading are presented in Fig. 11. Even with this
temperature changes. Fig. 8 shows typical X-ray relatively simple loading path, the material response
diraction data, for a specimen that has been is quite complex. A number of qualitative features,
loaded and unloaded in tension, which reveal the however, are evident. At low tensile strains (<1%),
presence of a small proportion of residual mar- the overall behavior is similar to that of pure tor-
tensite. sion; at higher tensile strains, a sharp increase is
Under pure torsional loading (Fig. 9), the observed in the stress upon superposition of torsion,
transition from the elastic loading region to the which is indicative of the generation of a new set of
transformation plateau region is less sharp. Notice martensitic variants which are energetically prefer-
that the lack of closure in the loading/unloading able for torsional (rather than the tensile) defor-
curve is due to the slippage of the axial extens- mation. In addition, the hysteresis in the torsional
ometer. This conclusion is deduced by a simple loading/unloading loop appears to decrease pro-
comparison with the corresponding shear (as op- gressively with increasing applied tensile strain
Fig. 9. Equivalent stressstrain plot showing the repeatability of two separate uniaxial torsion tests up to 2.3% equivalent strain.
J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986 977
Fig. 10. Shear stressstrain plot showing the repeatability of two separate uniaxial torsion tests up to 2.0% shear strain.
Fig. 11. Equivalent stressstrain plots in tension (0%, 0.7%, 1.10%, 1.5%, 2%, 3%, 6%), followed by torsion (2%) and reverse unloading
(Type I).
978 J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986
Fig. 12. Equivalent stressstrain plot showing the repeatability of tensiontorsion tests at two dierent sets of tensile strain (1.05%,
3%) and 2% shear strain.
Fig. 13. X-ray diraction analysis of NiTi material after a complete tensiontorsion cycle, showing the presence of a small proportion
of residual martensite.
which is consistent with the decreasing volume levels of applied tensile strain, the end of the tor-
fraction of variants associated with torsion. At all sional unloading segment is marked by a increasing
J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986 979
Fig. 14. Equivalent stressstrain plots in torsion (2%), followed by tension (0%, 0.7%, 1.05%, 3%, 5.8%) and reverse unloading
(Type II).
Fig. 15. Equivalent stressstrain plots in simultaneous tension (0%, 0.7%, 1.5%, 3%, 6%) and torsion (2%) with simultaneous
unloading (Type III).
980 J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986
equivalent stress with decreasing applied equivalent torsional loading occurs at monotonically decreas-
strain. The micromechanical origin of this me- ing stress levels. In addition, upon unloading, the
chanical response is not presently understood. elastic region is followed by reverse transforma-
However, it does qualitatively indicate that the tion along a plateau at monotonically increasing
material has retained memory of its tensile stress levels up to the point that corresponds to the
transformation state. end of the tensile unloading. Again, the material
A representative set of measurements in Fig. 12 appears to exhibit memory of the transition from
illustrates the degree of repeatability for two par- proportional to non-proportional loading.
ticular Type I loading programs. As in the case of
pure tension, X-ray diractometry data on the 3.4. Simultaneous tensiontorsion (Type III)
unloaded specimens indicate the presence of re-
sidual martensite at small proportions (Fig. 13). The results of simultaneous proportional ten-
siontorsion at up to 6.0% tensile strains and at
3.3. Torsion followed by tension (Type II) 2.0% shear are depicted in Fig. 15. All loading
paths produce curves which are qualitatively sim-
In this case, torsion is applied corresponding to ilar to those obtained under pure tension or tor-
2% strain, followed by tension up to 5.8% strain. sion. In particular, smooth loading and unloading
Unloading is subsequently eected in the reverse transformation plateaus are obtained at approxi-
order. Type II loading paths dier substantially mately constant stresses. This observation appears
from Type I paths, as readily seen in Fig. 14. Indeed, to support the conjecture that sharp changes in
here the transformation plateau that follows the the stresses during non-proportional loading are
Fig. 16. Comparison of equivalent stress and strain behavior between loading paths at peak strains of 0.7% in tension and 2.0% in
torsion.
J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986 981
Fig. 17. Comparison of equivalent stress and strain behavior between loading paths at peak strains of 3.0% in tension and 2.0%
in torsion.
eected by the generation of new sets of marten- smooth stressstrain curves, owing to the sharp
sitic variants, while existing variants lead to higher transitions in variant formation at the transfor-
stresses due to their energetic incompatibility with mation plateau. At a high tensile strain level (Fig.
the current loading state. Additionally, it is ob- 18), the Types II and III paths yield remarkably
served that both the forward and reverse trans- similar curves, which can be explained by the
formation stresses decrease with increasing predominantly proportional nature of both paths
proportion of the tensile loading, as expected. during the transformation process.
Figs. 1618 compare Types IIII loading paths The main features of the mechanical response of
for various maximum tensile strains and at con- the tested polycrystalline Nitinol alloy are sum-
stant maximum shearing strain of 2%. At low marized and discussed in this section. In addition,
tensile strain levels (Fig. 16), the loading paths are the experimental results are reproduced using a
quite similar, although a small deviation is evident proposed constitutive model for superelasticity.
for the case of torsion followed by tensile loading.
This apparent path-independence is not surprising 4.1. Qualitative features
considering the low level of applied tensile strain.
At moderate tensile strains (Fig. 17), Type I and The experiments conrm that Nitinol produces
Type II loading generates widely diering non- essentially perfect stressstrain loops under cyclic
982 J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986
Fig. 18. Comparison of equivalent stress and strain behavior between loading paths at peak strains of 6.0% in tension and 2.0%
in torsion.
loading in both tension and torsion. They also the tensile stress reached the plateau value of ap-
demonstrate that the development of a load- proximately 400 MPa at 1% tensile strain, as
dependent microstructure is responsible for the shown in Fig. 6(a) (see also (Shaw and Kyriakides,
non-smooth stressstrain curves under non- 1998)); the bands remained visible during the tor-
proportional loading of Types I and II. In addi- sion cycle, where the tensile strain is held xed.
tion, the alloy appears to exhibit memory of However, no L uders bands were observed during
its forward transformation history throughout Type II loading. It is conjectured that L uders band
the loading process, as illustrated by the re- formation during the tensile cycle facilitates the
verse transformation paths followed in the non- deformation, consistent with the higher stresses in
proportional loading cases. torsion, where such bands do not appear to form,
Another important feature observed in the ex- at least up to 2% shear strain. This is also sup-
periments is that the forward transformations in ported by the simultaneous loading tests (Type
tension and torsion follow markedly dierent III), where the plateau stress decreases with in-
paths. In particular, and contrary to the case of creasing tensile strain (Fig. 6(c)). These observa-
initial yielding in metals, the transformation stress tions are consistent with the so-called yield drop
in torsion is consistently higher than in tension. In in Nitinol (Eucken and Duerig, 1989). Another
order to investigate further the dierent deforma- interesting qualitative characteristic of the stress
tion mechanisms in tension and torsion, electro- strain curves is that in the case of tension, there is a
polished specimens were loaded according to the signicant reduction in the elastic modulus at very
Types I and II protocol. During Type I loading, low strains (approximately 0.3%), shown in Fig. 7,
Luders band formation was observed as soon as which may be attributed to the presence of the so-
J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986 983
X
24
Et na Eta 2
a1
Fig. 20. Comparison of equivalent stress and strain plots between experiments and numerical simulation for uniaxial loading.
Fig. 21. Comparison of equivalent stress and strain plots between experiments and numerical simulation for Type I loading path.
J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986 985
Fig. 22. Comparison of equivalent stress and strain plots between experiments and numerical simulation for Type III loading path.
longitudinal axis. The sheet texture assumption is clusion of dierent martensitic variants that can
also supported by the X-ray diraction analysis nucleate under non-proportional, non-simulta-
(Fig. 3), in which B2 (1 1 0) phase is dominant. In neous tensile and torsional loading shown in Fig.
real materials, a statistical variation from the tex- 21. This feature, which is clearly exhibited in the
ture within a deviation (wobble) is present, de- experiments and replicated in the numerical sim-
pending on the manufacturing process and ulation, has been dicult to capture using phe-
geometric properties of the material. However, in nomenological constitutive models.
this simulation, only the idealized texture eect has
been considered in generating a polycrystal ap-
proximation. 5. Conclusions
A novel computational method for solving the
constitutive equations associated with the above Tensiontorsion experiments on thin-walled
model is discussed in a companion paper (Jung superelastic Nitinol tubes have demonstrated a
et al., 2002). The nite element mesh of the spec- rich mechanical behavior involving signicantly
imen used in the experiments is shown in Fig. 19. dierent characteristics in each of the two loading
The model predicts reasonably well the stress re- axes. The observed behavior provides important
sponse in both tension and torsion, as illustrated in insights to the stress-induced phase transformation
Figs. 2022. Notice that the presence of R-phase is under multiaxial loading commonly encountered
not included in the model, which results in a devi- in a wide array of engineering applications in-
ation of the numerically computed linearly elastic volving superelastic materials. The experiments
loading curve from the corresponding experimen- and simulations suggest that the characterization
tal one. Also, notice that the ear-shaped curve and modeling of the microstructure is of para-
produced in the torsional loading/unloading stage mount importance in understanding the phenom-
is reproduced by the model, due to the latters in- enology of shape-memory alloys.
986 J.M. McNaney et al. / Mechanics of Materials 35 (2003) 969986