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C.

Remillat
Department of Aerospace Engineering,
University of Bristol,
Queens Building,
University Walk,
BS8 1TR, UK
M. R. Hassan
Department of Mechanical Engineering,
University of Shefeld,
S1 3JD Shefeld, UK
F. Scarpa
1
Department of Aerospace Engineering,
University of Bristol,
Queens Building,
University Walk,
BS8 1TR, UK
e-mail: f.scarpa@bris.ac.uk
Small Amplitude Dynamic
Properties of Ni
48
Ti
46
Cu
6
SMA
Ribbons: Experimental Results
and Modelling
This work illustrates viscoelastic testing and fractional derivative modelling to describe
the thermally induced transformation equivalent viscoelastic damping of NiTiCu SMA
ribbons. NiTiCu SMA ribbons have been recently evaluated to manufacture novel honey-
combs concepts (conventional and negative Poissons ratio) in shape memory alloys for
high damping and deployable sandwich antennas constructions. The dynamic mechanical
thermal analysis (DMTA) test has been carried out at different frequencies and tempera-
tures, with increasing and decreasing temperature gradients. Thermally induced trans-
formations (austenitic and martensitic) provide damping peaks at low frequency range
excitations. On the opposite, the storage moduli are not affected by the harmonic pulsa-
tion. As the SMA ribbon increases its stiffness, the damping capacity reduces, and the loss
factor drops dramatically at austenite nish temperature. The fractional derivative mod-
els provide a compact representation of the asymmetry of the peak locations, as well as
the storage modulus change from martensite to austenite phases.
DOI: 10.1115/1.2204949
Introduction
Shape memory alloy SMA materials have always attracted
signicant interest in damping applications. Opposite to classical
polymer-type materials, SMAs have signicant stiffness proper-
ties and are relatively insensitive to environmental hazard. One of
the advantages of using SMAs in austenitic or superelastic state is
related to the restoring force provided to return to the original
position after an imposed deformation. From a general point of
view, damping properties of SMAs are due to thermally-induced
and stress-induced transformations, as well as intrinsic damping
generated in the coexisting phases. Dissipation originated by tem-
perature variation occurs during heating and cooling. The intrinsic
damping of the martensite phase is signicantly high due to the
reorientation of the martensite twin variants under stress. In the
austenite phase, intrinsic damping is low, although a martensite-
induced phase transformation can be produced by high-applied
stress, leading to high-energy dissipation. Shape memory alloys
can be extremely useful in applications where damping capacity is
sufciently elevated and damping stability is also required. Super-
elastic damping capacities of SMAs have been studied by De-
jonghe et al. 1 on copper SMA. Piedboeuf and Gauvin 2 evalu-
ated the dynamic properties of austenitic Nitinol wires under
uniform strain rate and sinusoidal loading at different levels of
vibration amplitudes 2%, 3%, and 4% strain and four decades of
frequency up to 10 Hz, at 25C and 35C. Using an Anova and
F ratio analysis, they could verify the cross correlation and the
nonlinear viscoelastic properties of the SMA wire, and propose
semiempirical FFT models to describe the dynamic stress re-
sponse and loss factor for the material. Gandhi and Wolons 3
performed a similar analysis for NiTi wires subjected to a maxi-
mum of 5.48% cyclic peak-to-peak strain, at 50F, 90F, and
130F, with sinusoidal excitation up to 10 Hz. The results were
postprocessed in terms of the complex modulus approach, a for-
mulation extensively used in vibration damping applications to
identify the viscoelastic material and structure combination to in-
crease modal damping ratios close to resonance behaviour 4.
While a consistent bulk of literature in damping of SMAs is
devoted to applications of pseudoelasticity or during superelastic
phase, less attention has been drawn on the damping behavior at
small amplitude harmonic vibrations with varying temperature
ranges. Small amplitude vibration damping in SMAs can be im-
portant for example in aerospace applications, where combined
random broadband excitations typical of boundary layer ow and
acoustic fatigue loading and thermal excitation spectra are
present in a typical operational environment. Recently, Biscarini
et al. 5 have identied extremely low values of Q
1
factors for
thin lms of Ni
30
Ti
50
Cu
20
produced by vacuum induction melting
when doped with hydrogen, in the range of 0.045 for temperatures
from 275 K to 318 K. The samples were subjected to maximum
strains of 110
7
to 310
5
at excitation frequencies of
0.48 kHz and 1.5 kHz, respectively using a resonance technique
based on clamped-free beam testing. A recent work on the small
amplitude dynamic properties of SMA ribbons has been illustrated
by Lu et al. 6, where Ti
44
Ni
47
Nb
9
have been tested on a DMTA
IV type instrument, at harmonic pulsations between 0.1 Hz and
10 Hz, with strain amplitudes ranging from 510
6
to 110
4
.
The samples were subjected to heating and cooling between
140C full martensite and 40C at complete austenite phase.
A peak loss factor of 13% was measured during the transition
phase between 105C and 80C, with no signicant depen-
dence over the frequency excitation, in a similar manner recorded
for high frequency ranges in 5.
Several authors have performed the modelling of damping char-
acteristics of SMAs. As already mentioned, the determination of
equivalent storage modulus and tan for pseudoelasticity has
been considered by Gandhi and Wolons 3, while Piedboeuf and
Gauvin used a FFT modelling approach 2. Malovrh and Gandhi
7 have proposed piecewise linear, multiple friction chains and
nonlinear spring models with and without offset to simulate the
hysteresis loops at different dynamic strain amplitudes and ther-
mal loading of NiTi wires. Oberaigner et al. 8 adapted their
micromechanical model for NiTi alloys to simulate the behavior
1
Corresponding author.
Contributed by the Materials Division of ASME for publication in the JOURNAL OF
ENGINEERING MATERIALS AND TECHNOLOGY. Manuscript received September 7, 2005;
nal manuscript received January 24, 2006. Review conducted by Mohammed
Cherkaoui.
260 / Vol. 128, JULY 2006 Copyright 2006 by ASME Transactions of the ASME
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of a vibrating rod between elastic and inelastic regions. After sim-
plications like the presence of a spatial constant stress distribu-
tion, combined dissipation, and latent heat and assuming constant
several parameters related to the thermal conduction and mechani-
cal properties, the mechanical energy ratios versus time and tem-
perature and therefore the dissipation levels can be determined
using a nonlinear nite difference scheme.
All the models described so far consider the elastic and inelastic
behaviour of the shape memory material. Classical micromechani-
cal models in SMAs like the ones proposed by Tanaka 9, Liang
and Rogers 10, and Brinson 11 should only be used to predict
the superelastic behavior of NiTinol materials 12, although at
full martensite phase the Brinson model provides more accurate
results. The complex modulus approach 3,4 is related strictly to
the equivalent viscoelastic properties of a solid, and its use on
pseudoelastic behavior of SMA provides an overall indication of
damping levels and storage stiffness values of the alloy.
In this work the small amplitude dynamic properties of a
Ni
48
Ti
46
Cu
6
ribbon storage modulus and loss factor: are mea-
sured using a dynamic mechanical thermal analyzer over a tem-
perature range from 10C to 150C, subjected to several har-
monic excitation over a decade, from 1 Hz to 60 Hz. The SMA
ribbons are subjected to a tension-tension loading with a constant
offset and constant dynamic strain of 510
6
. Both the offset
value and the dynamic strain are contained within the elastic range
of the SMA phases. The type of ribbon tested is used to manufac-
ture a new concept of SMA honeycomb structures 13 to be used
as high-capacity damping core for sandwich structures and de-
ployable antennas. The results are then prostprocessed in terms of
complex modulus using a fractional derivative model using a re-
duced frequency parameter where the temperature is the solely
variable. The fractional derivative modelling allows a very com-
pact notation of the real and imaginary part of the complex modu-
lus for viscoelastic materials. Although closed-form solution mod-
els have been proposed in the past for polymers 14, the
fractional derivative model allows avoiding the identication of
linear combinations of the Standard model or Prony series 15, a
procedure often used in viscoelastic polymer modelling.
The paper is organized as follows: The rst part describes the
properties of the SMA ribbon and the types of mechanical and
dynamic testing performed. The second part describes the results
acquired during heating and cooling process, as well as the stor-
age modulus and loss factor values obtained during the frequency
sweep of the mastercurve approach. The third part of the manu-
script describes the fractional derivative model developed to simu-
late the heating and cooling of the SMA ribbon.
SMA Properties and Testing
Ni
46
Ti
48
Cu
6
Properties. The SMAmaterial used consisted on a
ribbon manufactured by @Medical Technologies n.v. product
code: SME NTC05 OX 0.206.40 mm using a thin rolling
process technique. The transformation temperature of the ribbon
was determined by differential scanning calorimeter DSC and
given as data specication for the material batch. The martensite
temperatures M
f
and M
s
were, respectively, 38C and 50C,
while the austenite phase was dened by the temperatures A
s
and
A
f
being, respectively, 58C and 76C. At room temperature, the
material therefore behaved in full martensite structure. Mechani-
cal tensile tests conducted with a Testometric M350 machine with
a 5 kN load cell allowed to identify the Youngs modulus and
yielding points of the martensite and austenite phases. At room
temperature full martensite the Youngs modulus was 13 GPa,
with a yield stress
0
of 170 MPa at 1.1% of strain. At 105C
full austenite phase the Youngs modulus was 30 GPa, with yield
stress
0
of 320 MPa at 1.8% of strain. The samples were trained
loading up to 8% of strain at room temperature. After load release,
the residual strain was around 4%. The ribbons were heated then
until full austenite phase, and the whole process repeated 30
times. The training process was performed on the same DMTA
used for the equivalent viscoelastic testing.
DMTA Testing. The DMTA machine consisted in a ME-
TRAVIB VA2000 Viscoanalyser equipped with a load cell of
100 N, able to support a maximum sinusoidal excitation fre-
quency of 250 Hz ranging from 0.001 Hz. Three types of test
were performed with the DMTA: progressive heating while the
the ribbon was subjected to sinusoidal excitation at 5 Hz, progres-
sive cooling at the same cyclic loading, and a master curve test for
frequency range from 1 Hz to 60 Hz.
For the rst test, the ribbon was tested under tension-tension
loading at the prescribed harmonic pulsation within a temperature
range between 10C and 110C. The ribbon was placed in the
test chamber and xed with a custom-made aluminium clamp. To
ensure an improved xture and thermal insulation between the
aluminium of the clamp and the ribbon itself, a coat of epoxy
resin glue has been applied 6. The ribbon was preloaded at room
temperature with a 5 N tensile load, corresponding to a tensile
strain of 0.03% at full martensite phase. The temperature was then
brought down to 10C at a rate of 5C/ min. The data were col-
lected for the test from 10C to 110C maintaining the same con-
stant heating rate of 5C/ min. The ribbon was constantly excited
with sinusoidal excitation of 5 Hz and constant dynamic strain of
5.6e-4% during the whole test. The dynamic strain was also moni-
tored, showing a constant behavior with maximum It has to be
pointed out that the test chamber temperature was kept uniform
across the volume using a fan device, while the temperature au-
tomatically monitored and controlled through thermocouple.
The second test was started immediately when the heating pro-
cess stop at 110C. It must be done using the same sample in
order to get the complete cycle of heating and cooling process of
the ribbon. Also in this case, the data were collected using a cool-
ing rate of 5C/ m from 10C to 110C. The third test was per-
formed to obtain a master curve for the SMA ribbon. From the
previous tests, it was noticed a signicant increase in the loss
factor during transition phase, between 50C and 60C. It was
therefore decided to narrow the mastercurve temperature range
between 10C and 75C, with discrete frequency values at 1 Hz,
1.5 Hz, 2.26 Hz, 3.41 Hz, 5.14 Hz, 7.74 Hz, 11.66 Hz, 17.56 Hz,
26.4 Hz, 39.84 Hz, and 60 Hz. The values were selected because
frequency was measured in log value. At each temperature step
5C the ribbon was subjected to that frequencies. Between each
sinusoidal loading there was in interval of 1 min between fre-
quency steps before the new mechanical loading started.
The values of the storage modulus were then evaluated using:
E
S
= k F
c
F
f
1
where k is the measured stiffness N/m, F
c
is the correction fac-
tor,
F
c
= cos 2
where is the phase angle. F
f
is the stress concentration factor,
F
f
= h/S
e
3
where h is the specimen height and S
e
=b t is the specimen cross
section. The loss factor or tangent modulus has been computed
using the classical formulation 4
tan =
E
I
E
S
4
where E
I
is the imaginary part of the SMA complex modulus, and
E
S
the storage modulus. The results were postprocessed using the
DYNATEST software associated to the DMTA facility.
Results and Discussions
Figures 1 and 2 shows the quasistatic tensile tests performed on
the ribbon at full martensite Fig. 1 and austenite Fig. 2 phases.
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The linear elastic portion of the curves during the loading phase
shows Youngs moduli of 8.7 GPa 25 C and 23.1 GPa
105 C for the martensite and austenite of the SMA ribbon con-
sidered, respectively. These values are signicantly lower com-
pared to the ones provided in the data specs, with a percentage
decrease of 42% and 23%, respectively. The stiffness ratio be-
tween austenite and martensite phase assumes now the value of
2.65, from the value of 2 provided by the data sheet.
Figure 3 shows the storage modulus and loss factors of the
ribbon during heating process and subjected to a sinusoidal load-
ing of 5 Hz. The storage modulus and loss factors values have
been calculated using Eqs. 1 and 4; the storage modulus, in
particular, is proportional to the effective Youngs modulus of the
SMA material by a factor of 0.64. It can be noticed that the stor-
age modulus tends to decrease after the A
s
temperature, with a
signicant drop during the transformation phase. In particular, two
peaks of the storage modulus are present around A
s
and A
f
tem-
peratures. The storage modulus tends to increase further until full
austenite, with a gradual build up of the real part of the complex
modulus until 150C. The loss modulus features some interesting
characteristics. The loss factor shows an almost constant damping
value of 2%, with a subsequent steep increase at around 6% at
austenite start. In principle, a second smaller peak could be ar-
guably identied around A
f
temperature. The loss factor at full
austenite has average values around 1%, well below the ones of
the martensite phase, as illustrated in literature 2,5,6,9. A step
increase of loss factor up to 6% is recorded during the transition
phase, while a smaller peak could be identied always around A
f
temperature. The ratio of storage modulus between austenite and
martensite phase is 2.6, well in line with the ratio of Youngs
Fig. 1 One-cycle quasistatic test on SMA ribbon-full martensite
Fig. 2 One-cycle quasistatic test on SMA ribbon-full austenite
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modulus between austenite and martensite phase recorded during
the quasistatic tests. Figure 4 shows the same type of test of Fig.
3 during cooling. The storage modulus is almost constant for all
the austenite phase, starting to decrease between A
f
and M
s
tem-
peratures, with a steep reduction in martensitic transition from M
s
to M
f
temperature. At full martensite phase, the storage modulus
is constant, giving a modulus ratio of 5. The loss factor present an
average value of 1% in the austenite phase, with a gradual de-
crease during austenitic transformation and steep peak during
martensitic one, with maximum value around 6% as in the heating
phase. During martensite form, the loss factor assumes an average
value of 2% over the temperature range. It is worth noticing that
the presence of the peak loss factor coincides with the temperature
point approximately corresponding to the zero second derivative
versus temperature of the storage modulus, as it occurs in classical
viscoelasticity 15,16. Figure 5 shows the results of the master
curve test on the storage modulus of the ribbon during the heating
process at different frequencies of excitation. As it can be
noticedand expected to a large extendthe storage modulus is
almost independent of the frequency excitation, also during the
austenitic transition phase. We show for completeness the behav-
ior of the loss factor in a master curve approach in Fig. 6. The loss
factors corresponding to the rst six frequencies from
1 Hz to 7.74 Hz are shown with a star mark, while the other
values are represented with a round mark. The behavior of the loss
factor for the rst six frequencies of excitation is quite similar,
with a major peak around transition phase, and decreased value at
the austenite form. For the subsequent frequencies, the loss factor
at martensite increases signicantly, while not presenting clear
peak behavior during the transformation phase.
The presence of storage modulus and loss factors peaks Figs. 3
and 6 during heating have been recorded as transition peaks P
H1
and P
H2
in other NiTiCu alloys 5, although transition effects
tend to disappear above frequencies of 1 Hz. In this case, not only
the peaks are present at higher frequency of excitation Fig. 3,
but also they exist in the storage modulus for higher harmonic
pulsations Fig. 5. The behavior of the loss factor during heating
is quite similar for the rst ve frequencies of excitation, with the
presence of a peak during austenitic transition. However, for
higher pulsations this behavior is not respected, with increase of
the loss factor during martensite and no presence of peaks during
transition, while the curves do not show regular patterns as in the
lower frequency range. This behavior would suggest that transient
Fig. 3 Storage modulus and loss factor versus temperature-heating process
Fig. 4 Storage modulus and loss factor versus temperature-cooling process
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effects effectively generate the peaks during transition. However,
above 10 Hz the DMTA used experienced some resonance prob-
lems due to the dynamic stiffness of the head designed to test
softer materials. While this resonance behavior does not particu-
larly affect the real part of the complex modulus extracted using
Eq. 1, the phase shift between real and imaginary part of the
mechanical response is affected. In fact, the loss factor changes
signicantly even during full martensite, opposite to the stable
behavior shown at excitation frequencies up to 7.74 Hz. This fact
suggests that the measurements taken from 11 Hz, especially for
the loss factor, could be prone to experimental error, and should
be considered with care.
Although the cooling curve shown in Fig. 4 features all the
characteristics of regularity and smoothness typical of classical
viscoelastic testing, the nal storage modulus corresponding to
full martensite is signicantly lower compared to the one present
in Fig. 3, with a decrease of almost 50%, although the dynamic
strain applied was constantly monitored and did not show any sign
of clamp slip. We are not able to provide explanation of this
phenomenon at this stage. We observe that, considering the con-
stant harmonic cycling and the temperature rate applied, the rib-
bon was subjected to a total of 12,000 cycles at the end of the
martensite phase during cooling, leading to a possible modica-
tion of residual stresses on the sample at the end of the heating/
cooling process. However, the average loss factors at martensite
and austenite phase are substantially the same for the two pro-
cesses, indicating that motions of twin boundaries for the high
damping in martensite was still present both after heating and
cooling 5. However, the curves shown in Fig. 6 feature an
equivalent viscoelastic characteristic of the storage modulus
Fig. 5 Storage modulus versus temperature and frequency-heating process
Fig. 6 Storage modulus and loss factor versus temperature and frequency-
heating process. - frequencies from 1 Hz to 7.74 Hz. , frequencies from
11.4 Hz to 60 Hz.
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equivalence temperature/frequency, and the presence of a loss
factor peak that would suggest the possible use of modelling tech-
niques used for classical polymeric viscoelastic materials.
Fractional Derivative-Based Model
A basic fractional derivative model used in temperature/
frequency equivalence is given by 15
E
*
=
a
1
+ b
1
i2 fT

1 + c
1
i2 fT

5
In this relation, E
*
is a complex number, while a
1
, b
1
, and c
1
are
quantities, not necessarily complex. The quantity fT is the re-
duced frequency of the master curve model 15. When the re-
duced frequency approaches to zero, the term a
1
represents the
lowest fT asymptote of the complex modulus for the lowest
frequency and/or highest temperature. In a similar way, when the
reduced frequency approaches innity, the ratio b
1
/ c
1
approaches
the upper asymptote of fT viscoelastic response, corresponding
to high frequency and/or low temperature. In the case of the
equivalent viscoelastic properties of the SMA ribbon, the fre-
quency dependence is negligible, therefore Eq. 5 can be recast in
terms of pure temperature reliance. Typical values of the coef-
cient vary between 0.4 and 0.7 15. The standard viscoelastic
model 15 features a value of equal to 1. Other typical values
of the coefcients a
1
and b
1
for polymeric materials range from
200 to 700, while the coefcient c1 is always well below the unity
15. To consider the specic loss factor behavior for the SMA,
i.e., the nonsymmetric performance at full martensite around 2%
and austenite phase 1%, the fractional derivative model pro-
posed is the following:
E
*
= E
0
1 + 0.02i

1 + m
r
1 + im
a

i10
T
10
T
0

1 +
i10
T
10
T
1

6
In this case, E
0
is the value of the storage modulus at full marten-
site phase, with a loss of 2% corresponding to that specic crystal
lattice structure. It has to be noticed that the term E
0
1+0.02i
corresponds to a
1
in Eq. 5. The term b
1
,
Fig. 7 Fractional derivative representation of storage modulus and loss factor
for the SMA ribbon-cooling process
Fig. 8 Fractional derivative representation of storage modulus and loss factor
for SMA ribbon-heating process
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b
1
=
m
r
1 + im
a

E
0
1 + 0.02i
7
is complex, and allows us to represent the nonsymmetric peak
location of the loss factor. The values for m
r
and m
a
are, respec-
tively, 0.042 and 0.01 for the cooling process. The temperatures
T
0
and T
1
represent the transition temperatures, being, respec-
tively, 38C and 50C. To simulate the heating process, the co-
efcient should be decreased by one order of magnitude to
0.0045, and the transition temperatures to 58C and 76C, re-
spectively. The coefcient is equal to 0.15. Figure 7 shows the
plot of the storage modulus ratio and loss factor from Eq. 6
versus a temperature range for cooling, considering a stiffness
ratio of 2.6 similar to the one from the quasistatic tests. The curve
for heating process is represented in Fig. 8. One can notice the
change of transition temperatures, and the substantial physical
similarities that the fractional derivative models allow us to simu-
late in a compact form with the experimental results. Figure 9
provides a direct comparison between the experimental and ana-
lytical values related to the heating process, showing a consistent
agreement between the fractional derivative approach and the
mastercurve data.
Conclusions
In this work small amplitude master-curve-type tests have been
performed on a NiTiCu ribbon to extract equivalent viscoelastic
characteristics for broadband low amplitude damping applications
up to 60 Hz of excitation, and heating/cooling from
10C to 150C. The storage modulus and loss factors measured
using DMTA equipment did not show frequency dependence,
while changes in stiffness of ratios similar to the ones recorded
during quasistatic tests were observed from full martensite to aus-
tenite phase. The loss factors showed signicant peak increase
during transition, under harmonic pulsations up to 7.74 Hz. A
compact fractional derivative-based model has been developed to
simulate the equivalent viscoelastic properties of the SMA ribbon.
The storage modulus peaks present during transition were re-
corded during the whole frequency sweep in the master curve test.
However, the results related to the loss modulus are not conclu-
sive, because of the irregularities given by resonance of the test
equipment used above 10 Hz. Further analysis is needed to im-
prove the testing at higher frequency ranges, to improve the as-
sessment of SMA ribbons to enhance possible implementations in
broadband white noise excitation applications 17,18.
Acknowledgment
This work has been partially supported by the Engineering and
Physical Science Research Council Grant No. EPSRC GR/R/
97313. The authors would like to thank Mr. Les Morton for his
assistance during the DMTA testing. Special acknowledgement
goes also to several colleagues: Dr. M. Collet from CNRS
FEMTO-ST of University of Besanon, France, Professor F. Maz-
zolai from University of Perugia, Italy, Dr. Farhan Gandhi from
Penn State, and Professor R. Lakes from University of Wisconsin-
Madison, for their useful suggestions and discussions.
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