Roy Bangalore
Roy Bangalore
a r t i c l e i n f o a b s t r a c t
Article history: An investigation into the thermo-mechanical response of trained Ni–Ti shape memory alloy (SMA) wires
Received 6 March 2008 with two-way shape memory effect (TWSME) induced into them was conducted in order to examine the
Received in revised form 16 April 2008 influence of the cold work on quasi-static and fatigue behavior of SMAs. Use of dynamic mechanical ana-
Accepted 21 April 2008
lyzer (DMA) for such tests on thin wires was examined and successfully utilized. Quasi-static stress–strain
responses of the wires at different temperatures were obtained to determine the critical stresses for for-
Keywords:
ward as well as reverse transformations. Mechanical stress-controlled fatigue tests were conducted on
Shape memory alloys
the wires in the austenitic state (130 ◦ C). They showed a two-stage deterioration of fatigue life—a rapid
Fatigue life
Austenite
decay when the maximum stress of the fatigue cycle is higher than the critical transformation stress, and
Martensite a more gradual deterioration at stress levels considerably lower than the critical stress. The fatigue life of
Dynamic mechanical analyzer the wires was found to increase with the load ratio, R, whereas the frequency of cyclic loading had only
a marginal effect. Differential scanning calorimetry (DSC) of the fatigued austenite specimens indicated
the presence of residual stress-induced martensite in the austenitic state. The high concentration of the
austenite–martensite interfaces act as potential sites for stress-concentration and are the main source of
the drastic decrease of the fatigue life in the two-phase region.
© 2008 Elsevier B.V. All rights reserved.
0921-5093/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2008.04.052
430 D. Roy et al. / Materials Science and Engineering A 494 (2008) 429–435
Fig. 2. A schematic of the grips used for testing the wires. All the dimensions are in
mm.
3. Results
Fig. 4. Quasi-static tensile stress–strain response of the thermally cycled wires at
3.1. DSC various temperatures.
Comparison of DSC scans of the AR and HT wires is made in 200 MPa. The two, however, have different plateau strains (owing
Fig. 1. Both the A → M and M → A transformation start at a higher to martensite variant reorientation), larger in the heat-treated wire
temperature for the HT wire as compared to the AR wire. However, (∼4.5%) in comparison to the thermally cycled wire (∼2.5%).
the HT wire shows a distinct R-phase transformation while cooling, Quasi-static stress–strain responses during loading and unload-
much in contrast to the AR wire wherein the R-phase transforma- ing of the TC wires at different temperatures above Af are shown in
tion is suppressed almost entirely. (Only a small hump in the curve Fig. 4. The curves depict ideal pseudo-elastic behavior with a dis-
corresponding to the R phase formation was seen.) tinct stress plateau during loading owing to SIM transformation.
Data obtained from these curves are summarized in Table 2. It is
3.2. Quasi-static tensile tests seen that the transformation stress increases with increasing tem-
perature whereas the transformation strain remains approximately
Quasi-static tensile stress–strain response of the trained (AR) constant at ∼7.5%.
wire at room temperature is shown in Fig. 3. It does not show a The critical stress for inducing forward transformation, SIM ,
distinct plateau at a constant stress owing to martensite variant ori- as well as that for inverse transformation, b , both increase with
entation (lack of detwinning). However, the stress–strain response increase in temperature as shown in Fig. 5. The stress–temperature
at room temperature of both the HT and TC wires (Fig. 3) show a relationship is approximately linear with d/dT of ∼7 MPa/◦ C, as
distinct plateau behavior with the detwinning stress, DT , of around per the Clausius–Clapeyron relation that describes the thermo-
Table 2
Summary of the data obtained from the qausi-static tensile tests performed at various temperatures
Temperature (◦ C) Starting stress (MPa) End stress (MPa) Starting strain (%) Plateau strain range (%) UTS (MPa)
Fig. 5. Variation of the stress-induced martensite start stress on loading and the
reverse transformation stress during unloading as a function of the testing temper-
ature. Fig. 7. Variation of elastic modulus of the as-received wire with temperature.
Fig. 8. S–N curves generated on the TC wires with different load ratios, R. Here,
for comparison purposes, fatigue life is plotted against the maximum stress of the
Fig. 6. Variation of elastic modulus of the as-received wire with stress at 130 ◦ C. fatigue cycle, max .
D. Roy et al. / Materials Science and Engineering A 494 (2008) 429–435 433
4. Discussion
forward as well as reverse transformation increases with increase macroscopic critical stress of the wire at 130 ◦ C) is clear evidence
in temperature. of the formation of stress-induced martensite during these tests
The disappearance of the plateau corresponding to the reverse (Fig. 10a). Also, the pre-existing residual martensite present in the
(martensite to austenite) transformation with increase in temper- microstructure of the trained wire grows with continued cycling.
ature can be attributed to the introduction of dislocations into the The high concentration of the austenite–martensite interfaces act
matrix as the material is stressed to higher levels with increase in as potential sites for stress-concentration and are the main source
temperature. of the drastic decrease of the fatigue life in the two-phase region.
The rapid degradation rate when the wire is cycled at stresses
4.3. Variation of secant modulus higher than the critical stress of the material is in agreement with
the observations of Tabanli et al. [16] who found that the fatigue
The Young’s modulus of SMAs is phase dependant, with the life of NiTi was shorter in the super-elastic plateau regime, which
modulus of the austenite and martensite differing as much as a few they suggest is a consequence of the coexistence of austenite and
times in some SMAs [12]. The V-shaped variation of secant modulus martensite. The slower degradation of the wires cycled at maxi-
(instantaneous slope of the stress–strain curve) with strain (Fig. 6) mum stresses considerably lower than the critical stress (so that
indicates that the SMA initially becomes more complaint before microscopic stress-induced transformation during cycling can be
regaining the stiffness. This can be explained as following. The ruled out) can be explained on the basis that the population of
stress-induced phase transformation from austenite to martensite austenite–martensite interfaces is much lower. In this case, only the
in polycrystalline SMAs is not instantaneous, but occurs gradu- stationary interfaces between austenite and pre-existing residual
ally, i.e., initial phase transformation from austenite to martensite martensite in the trained wire exist as compared to the wires cycled
followed by reorientation of the martensite variants so formed. at high maximum stresses where stress-induced transformation
The stiffening in the later stage is the result of growth of partic- does take place. Thus the magnitude and extent of permanent dam-
ular martensite variants favorable to the applied stress state at age accumulation will be lower and hence higher fatigue life is seen
the expense of the others. The formation and dissolution of inter- for these conditions of cycling.
faces of various variants and their relative motion influences the The improvement in fatigue life with increase in R can be
stress–strain behavior during transformation. The DMA was found explained on the basis that for the same maximum stress, the wire,
to be particularly suited to examine modulus variations as it pro- which has been fatigued at a lower R, has to go through a wider
vides information to obtain the modulus at every load increment stress range in an entire fatigue cycle and hence the extent of micro-
during the quasi-static tensile test. scopic deformation accumulated in it in a cycle is much larger than
the case of a wire fatigued at a higher R.
4.4. Fatigue life The marginal improvement of fatigue life with increase in fre-
quency is possibly because of the higher critical stress (due to
As mentioned earlier, the TWSME generated by training is basi- increased temperature as a result of exothermic SIM transforma-
cally a consequence of a dislocation structure generated during the tion) and hardening rate at high strain rates, which decreases the
training cycle, which provides local stress and favors the forma- transformation and associated microstructural effects that influ-
tion of a preferred orientation to a net shape variation [10]. The ence fatigue degradation.
oriented residual stresses associated with dislocation arrangement
during training are relaxed by the nucleation and growth of cer- 5. Summary
tain preferential martensite variants. The presence of dislocations
does not allow complete martensite–austenite transformation dur- The thermo-mechanical response of thin trained NiTi wires was
ing unloading or heating. Hence, with cycling, there is a progressive examined employing a DMA. The quasi-static tensile stress–strain
increment of residual martensite, leading to permanent damage response of the trained wires with pre-existing residual marten-
accumulation and a deterioration of pseudo-elasticity [13–15]. The site is different from annealed wires in a sense that in the trained
trained wires used in this study therefore had some residual per- wires, owing to the presence of stabilized martensite a priori, there
manent deformation associated with them a priori in the form of is no closure of the super-elastic loop (at temperatures above Af )
dislocations as well as certain fraction of stabilized martensite vari- in contrast to annealed wires where complete closure of the super-
ants. elastic loop is observed. As a result, the extent of the plateau regime
Mechanical cycling of the trained wires at high stresses (owing to martensite re-orientation in case of the trained wires in
( max > 400 MPa) would lead to the generation of dislocations their martensitic state and stress-induced transformation in their
within the wires and dislocation mediated plastic deformation austenitic counterparts) is less in the trained wires compared to
would change the internal stress-fields associated with the trained the annealed ones. An interesting feature, which came up along-
wires. The stress-fields associated with the newly formulated dis- side the stress–strain response of the wires, with the aid of the
locations would possibly aid the nucleation of variants different dynamic mechanical analyzer, was the V-shaped variation of the
from those formed during training cycles and hence are unfavorable secant modulus with strain.
for TWSME. The annihilation and rearrangement of the disloca- Fatigue loading of the wires in their austenitic state revealed a
tion structure impedes the formation of the variants of martensite two-stage deterioration of fatigue life with a rather rapid decay at
responsible for the two-way effect, and with continued cycling, for- maximum stresses higher than the critical stress of the material
mation and stabilization of other martensite variants occurs leading which slows down to a more gradual deterioration at maxi-
to permanent damage accumulation and final failure of the wires. mum stress levels considerably lower than the critical stress for
Although 400 MPa is lower than the critical stress of the material at inducing martensitic transformation. A possible explanation is the
130 ◦ C (around 600 MPa), as mentioned earlier, pockets of marten- population of austenite–martensite interfaces which act as stress
site start forming in the material as a consequence of microscopic concentrators and dislocation mediated plastic deformation which
stress-induced transformation prior to macroscopic transforma- interferes with the two-way memory effect and leads to the func-
tion. The broadening of the peaks and the decrease in latent heat of tional fatigue of the wires. Other interesting feature which came
transformation corresponding to the cooling curves for the wires up with the fatigue test is the improvement of fatigue life with
cycled at a maximum stress of 450 and 550 MPa (lower than the increase in the stress ratio. The frequency of loading had only a
D. Roy et al. / Materials Science and Engineering A 494 (2008) 429–435 435