Sensors and Actuators A 254 (2017) 28–35

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Sensors and Actuators A: Physical

journal homepage: www.elsevier.com/locate/sna

Investigations on the life cycle behavior of Cu-Al-Ni/polyimide shape

memory alloy bi-morph at varying substrate thickness and actuation
conditions
Akash K a , Mani Prabu S S b , Ashish K. Shukla b , Tameshwer Nath a , Karthick S a ,
I.A. Palani a,b,∗
a
Mechatronics and Instrumentation Lab, Discipline of Mechanical Engineering, Indian Institute of Technology Indore, Madhya Pradesh, India
b
Metallurgy Engineering and Material Science, Indian Institute of Technology Indore, Madhya Pradesh, India

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

Article history: In this work, a two-way displacing Cu-Al-Ni/Polyimide shape memory alloy bi-morph without any post
Received 24 June 2016 processing has been developed. The forward stroke was achieved with shape memory effect and the
Received in revised form return stroke was due to the influence of flexible polyimide substrate. A custom made setup with electrical
26 November 2016
heating was developed to investigate the life cycle of the bi-morph at different voltages, ranging from
Accepted 7 December 2016
2 V to 3 V. The austenite transformation temperatures of the bi-morph, was found to be As = 215 ◦ C and
Available online 8 December 2016
Af = 240 ◦ C. Shape recovery ratio was calculated and the shape memory alloy deposited on 75 ␮m thick
polyimide sheet exhibited better recoverability than 50 ␮m thick sheets. Further, maximum displacement
Keywords:
Shape memory materials
of 19 mm was observed from the edge of the bi-morph through plate heating. The effect of substrate
Cu-Al-Ni thickness on the life cycle behavior of the bi-morph was investigated. The bi-morph showed minor signs
Bi-morph of deformation when actuated at 0.5 Hz after 500 cycles. In addition the structural, morphological and
Phase transformation thermal behavior of the SMA bi-morph has been investigated in detail.
Life cycle © 2016 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction MEMS devices. Although there are reports on thermomechanical

behavior and fatigue life analysis of bulk SMA’s [12–17], very few
Shape memory alloys (SMA’s) are smart material which can papers discuss the fatigue life of thin film shape memory alloys.
recover its original geometry on the application of heat. Twin- Silicon wafers are widely used for developing thin films, where
ning is an important microstructural process responsible for the the film is peeled off after deposition process. Recently Kapton
shape memory effect. The SMA’s can remember up to three differ- Polyimide (PI) substrates are considered for the development of
ent shapes while transforming from low temperature martensite thin composite structures, where the substrate acts along with the
phase to high temperature austenite phase [1,2]. MEMS devices deposited material. SMA/Polyimide composite-film actuators are
which use thin film shape memory alloys have a work output that flexible films, which has SMA on one face and the polyimide sub-
often exceeds the other actuating mechanisms such as piezoelec- strate on the other. These bi-morph structures are more suitable for
tric, pneumatic. Further, these alloys can recover strains up to 8% the development of SMA thin films, as the return stroke during the
[3–6] and owing to their exceptional properties, these alloys have thermomechanical cycle is accomplished by the bias force of the
been widely used in micro-actuators such as micro-grippers, micro- flexible substrate. Further the flexible substrates can be obtained
pumps and micro-cantilevers [7–11]. However, thin film SMA has in several other shapes according to the requirement, thus avoid-
very less practical usage as the training process after fabrication to ing the training performed after deposition. Cantilever made out
obtain two way shape memory effect, hindering its applicability in of SMA/PI bi-morphs developed through sputtering was studied in
detail [18,19]. Recently NiTi/Polyimide composite actuated using a
1.5 V battery as a wing of dragonfly, has paved way for further more
microactuators [20,21].
∗ Corresponding author at: Mechatronics and Instrumentation Lab, Discipline of
Cu-Al-Ni can be an attractive and cost effective solution and it
Mechanical Engineering, Indian Institute of Technology Indore, Madhya Pradesh,
has the potential to replace the conventionally used NiTi [22,23].
India.
E-mail addresses: [email protected] (A. K), [email protected], In addition to this, copper based shape memory alloys can be
[email protected] (I.A. Palani). used in high temperature applications as the transformations tem-

http://dx.doi.org/10.1016/j.sna.2016.12.008
0924-4247/© 2016 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/
4.0/).
 A. K et al. / Sensors and Actuators A 254 (2017) 28–35 29

Fig. 1. (a) Thermal evaporation setup, (b) Life cycle analysis setup.

perature are beyond 200 ◦ C. Cu-Al-Ni shape memory alloys has Scanning Electron Microscope analysis, Thermogravimetry analysis
been proved to show 18% recoverable strain which is much higher and Temperature vs. resistance measurements.
when compared to conventionally demonstrated Ni-Ti [24,25]. To probe the suitability of the developed bi-morph in MEMS
Their properties such as good machinability, ease in forming pro- micro-actuator application, electrical actuation setup was utilized
cess, high thermal stability, rapid heating and cooling rate, less as shown in Fig. 1(b). Life cycle of the bi-morph has to investi-
hysteresis and higher Young’s modulus acts as major advantage gated thoroughly before considering it for potential applications
[26,27]. Further the transformation temperatures of these alloys [16,28,29]. It consist of K-type thermocouple, data acquisition sys-
can be altered by changing the percentage of Ni in the alloy. tem with 22 channels (Model: 34970A, Agilent) and programmable
In this work, an attempt has been made to develop Cu- power supply. The heating and cooling cycles was recorded by a
Al-Ni/Polyimide bi-morph at different substrate thickness and laser displacement sensor (Model: HLG108-A-C5, Panasonic). Three
investigate its life cycle behavior at different actuation conditions. different voltages 2 V, 2.5 V and 3 V were used for the analysis.
The influence of substrate thickness on thermal properties and the Fig. 1(b) shows the life cycle analysis setup. Using the setup two
fatigue life of the composite film have been studied in detail and different frequencies of 0.05 Hz and 0.5 Hz was exercised. In order
the suitability to use the as developed bi-morph as micro-actuator to obtain the maximum displacement of the bi-morph at different
has been explored. voltages 0.05 Hz was utilized and 0.5 Hz was used for fatigue life
analysis. The fatigue life was tested for 500 cycles and the results
2. Experimental procedure are summarized.

Wires of Copper, Aluminum and Nickel were precisely measured 3. Results and discussion
using a precision balance and made into 100 mg pellets with Cu-
14Al- 4Ni wt.% (Sigma Aldrich, purity 99.9%) composition. These Fig. 2(a) shows the detwinned martensite shape of the deposited
pellets were loaded on to a tungsten boat (crucible) placed in material and Fig. 2(b) shows the transformation to austenite phase
the system chamber and high vacuum of 10−5 Pa was maintained during the application of heat. During deposition, the polyimide
throughout the evacuation process. The deposition was carried out sheet is clamped to a substrate holder and the deposited mate-
using a large area thermal evaporation system rial will be in twinned martensite state. Once the deposited sheet
Fig. 1(a) shows the schematic layout of the experimental setup was removed from the holder, thermal stresses of the deposited
used for the deposition process. The deposition was carried out material tend to propagate in the direction of the pre-set polyimide
on DuPont-Kapton polyimide HN-type sheets of 50 ␮m and 75 ␮m shape. In this case it tends to form a semi-circular shape with the
thickness. The sheets were cut into 7 × 7 cm2 samples, baked and deposited material on the external surface forming the detwinned
cleaned prior to deposition. The procured polyimide had a pre-set martensite structure. The thermal stress is more at the epicenter
shape to it, which was semicircular in this case. During deposition of the semi-circle and it gradually reduces as it reaches the periph-
the sheets were clamped to substrate holder in a flat and uniform ery. On the application of heat, the bi-morph transforms from the
manner for homogenous deposition. The deposition was carried out detwinned martensite phase to the austenite phase. During actu-
in two steps where the first step was to allow the materials to melt ation, the material will incline towards the pre-strained shape or
at the eutectic temperature and form an alloy in the molten state. the clamped position during deposition, which acts as the residual
Once all the metals were present in molten state, the temperature stress free shape. This process can be repeated in cycles and thus
was increased rapidly beyond 1500 ◦ C, which led the evaporation the developed bi-morphs did not require any training.
of the materials placed in the crucible. The evaporated material
deposited on the polyimide samples placed 15 cm above the cru- 3.1. Morphological, structural and thermal analysis
cible. Due to heat convection the substrate temperature increased
to 40 ◦ C. In order to study the morphological, structural and thermal The thickness of the deposited film was found to be 300 nm as
properties, the samples were characterized with X-Ray diffraction, measured by the quartz crystal oscillator present inside the deposi-
30 A. K et al. / Sensors and Actuators A 254 (2017) 28–35

Table 1
Composition analysis results obtained from EDAX analysis.

Substrate thickness Cu Al Ni
(Atomic%) (Atomic%) (Atomic%)

50 ␮m 82.46% 13.73% 3.81%

75 ␮m 82.43% 13.61% 3.96%

material such as Titanium was not used for grain refinement. The
elemental analysis of the developed films was studied using Energy
dispersive spectroscopy, performed at five different places and the
average atomic percentage is reported in Table 1. The results show
a minor deviation from the nominal composition. The results show
the films having homogenous composition was developed through
the proposed method.
Fig. 3(b) shows the X-Ray diffraction pattern and it can be
observed that the evolution of crystalline peak corresponding to
␤ (220) (ICSD pattern, card no: 01-072-3498) martensitic struc-
ture and other ␣ and ␥ phases were present [35,36]. However, the
signal from the XRD was very coarse and the evolution of other
Fig. 2. (a) Image of the Detwinned martensite structure with a scale, (b) Image of
the austenite structure achieved after heating. martensite peaks was not evident. The crystallite size calculated
using Scherrer formula was 6.67 nm. The transformation between
the two phases depends on the structural properties and the com-
tion chamber. Adhesion of the film was excellent as observed from position of the alloy [37]. Structural properties such as single crystal
the scotch tape analysis, which showed no removal of the deposited or polycrystalline alloys, affects the shape memory effect vastly
SMA film. The shape memory alloy deposited on varying thickness as single crystal shape memory alloys are better because of the
of polyimide sheets, displayed similar morphological and structural defined transformation between one phase to another [38–40].
information. Fig. 3(a) shows the microscopic image of the as devel- Whereas, polycrystalline alloys have a difficulty in remember-
oped bi-morph. It was observed that, the morphology of the film ing their low temperature structure as the probability of cycling
was uniform without any cracks or porosity and the average grain between two different phase are high [41]. Furthermore, polycrys-
size was approximately 100 nm which is far less than convention- talline alloy shows recoverable strains up to 5% only, corresponding
ally developed alloy through casting [30–34]. Therefore additional to brittleness and order less phase transition, which reduces the

Fig. 3. (a) Microscopic image of the as developed sample, (b) XRD plot showing the ␤ (110) phase and other structural information (c) Thermogravimetry analysis showing
the decomposition temperature of bare polyimide and SMA/PI samples. (d) Temperature vs. resistance graph showing the austenite start and finish temperatures.
 A. K et al. / Sensors and Actuators A 254 (2017) 28–35 31

shape recovery significantly [42–44]. Parameters such as heat the temperature was raised slightly above 300 ◦ C, as seen in the
treatment, ageing, addition of other materials and training of the third cycle, the maximum displacement was only 12 mm and the
polycrystalline alloys at two particular phases [33,45–49] can have film did not return to its original position. The return stroke was
significant effect in the shape memory effect. limited to 6 mm due to plastic deformation of the bi-morph. There-
Fig. 3(c) shows the TGA analysis of the bi-morph as well as fore, 230 ◦ C–250 ◦ C is the appropriate actuation temperature range,
the bare polyimide sheet where, single stage decomposition was where the maximum displacement was observed.
observed. Sample amount of 5 mg were used for the analysis and Fig. 4(c) and (d) shows the hysteresis curve of the first two cycles
the heating rate was maintained at 10 ◦ C/min. The samples started of the bimorph structure. In the first cycle it can be noticed from
degrading gradually from 390 ◦ C and the initial decomposition rate the hysteresis graph at Fig. 4(c) that the displacement continues to
(IDR) of both the samples was less than 5% till 500 ◦ C. From 505 ◦ C increase for approximately 5 s even after the heating is stopped. On
the Cu-Al-Ni/Polyimide sample weight loss was rapid and the bi- the contrary, the hysteresis for second cycle as shown in Fig. 4(d),
morph was completely decomposed at 670 ◦ C. The maximum rate exhibited a minimal hysteresis. Even though there was reduction in
of decomposition temperature (MRDT) was found to be in the range major hysteresis loop, it exhibited a complex behavior as observed
of 500 ◦ C–670 ◦ C. However the bare polyimide exhibited a different from the minor decline in displacement. The reason for the reduced
decomposition rate and the sample got completely decomposed hysteresis loop might be due the attainment of maximum displace-
at 725 ◦ C. The rapid decomposition of Cu-Al-Ni/polyimide samples ment in the previous cycle. After saturation the bi-morph will be
may be attributed to the ability of the alloys to absorb heat which more sensitive to the temperature changes which could result in
might result in conduction of the polyimide samples. The decompo- low hysteresis. The hysteresis plots show that the as developed
sition temperature range assisted in relating the voltage required bimorphs can have very low hysteresis after attaining its saturation,
during electrical actuation. To further locate the phase transition at specific actuation temperatures. Further, temperatures beyond
temperature of the developed bi-morphs, a four probe van der 300 ◦ C are not suitable for actuation since there is irrecoverable
pauw method which provides temperature vs. resistance measure- plastic strain as observed from the third cycle, where there was a
ments was utilized. The samples were cut in 2 × 2 cm2 sheets and drastic decline in displacement caused majorly due to high temper-
silver conducting paste (1–3 × 10−5 W-cm) was used to make the atures. Fig. 4(e) shows the actuation of the bimorph during heating
contacts. Heating was controlled at 5 ◦ C/min and the analysis was placed in front of calibrated scale. The deflection can be clearly seen
conducted at argon atmosphere. Fig. 3(d) shows the temperature from the images.
vs. resistance measurement. The austenite start and finish temper-
atures was observed at 215 ◦ C and 240 ◦ C. 3.3. Life cycle analysis

3.2. Shape recovery ratio analysis To investigate the cyclic behavior and the fatigue life of the
developed structures, electrical actuation was employed. Three dif-
In order to investigate the shape recovery ratio and maxi- ferent voltages of 2 V, 2.5 V and 3 V were selected and two different
mum displacement from the edge of the bi-morph a test bench frequencies of 0.05 Hz and 0.5 Hz were used for the investigations.
with substrate heating was designed to heat and cool the bi- 0.05 Hz was used to find the maximum displacement at different
morph. A 7 × 2 cm2 Cu-Al-Ni/polyimide sheet was clamped to a voltages and 0.5 Hz was used as an initial value to study the suit-
substrate heater with thermal tape. It was found that the maxi- ability of the bi-morph in MEMS actuators. Fig. 5(a) shows the
mum displacement was achieved only with substrate heating as the maximum displacement graph for samples deposited on 50 ␮m
contact points reached the degradation temperature at higher volt- polyimide sheet. The maximum displacement achieved with 2 V,
ages with electrical actuation. Fig. 4(a) shows the shape recovery 2.5 V and 3 V was 2.8 mm, 4.1 mm and 4.6 mm respectively. For
ratio Dr vs temperature plot. The recovery ratio increases during 2 V and 2.5 V the bi-morph returns to its original position with-
heating and it returns back to its original value as the bi-morph out any deformation. However at 3 V, the cycle was incomplete as
transforms from high temperature austenite phase to low temper- the bi-morph showed a loss of 0.5 mm in displacement during cool-
ature martensite phase. 75 ␮m polyimide sheets exhibited a higher ing. First cycle had larger displacement however once the actuation
recovery ratio of 1.38 whereas, 50 ␮m sheet exhibited only 1.21 frequency was attained the maximum displacement was 2.5 mm,
ratio. The recovery ratio was calculated by finding the diameter of 3.4 mm and 3.8 mm respectively. Fig. 5(b) shows the maximum dis-
the curved bi-morph structure at various temperatures. The recov- placement graph for samples deposited on 75 ␮m polyimide sheets.
ery ratio gradually decreased during cooling as the sheet recovered The plots displayed a similar behavior as compared to 50 ␮m sheet
to its original position. The recovery ratio is higher than previously where the bi-morph failed to return to original position during
reported works on shape memory alloy/polyimide bi-morph. This cooling. Nevertheless the maximum displacements achieved with
demonstrated the ability of the developed samples to exhibit two different voltages were 4.1 mm, 7.2 mm and 9.2 mm.
way shape memory effect, with polyimide acting as a bias force The bi-morph was tested for its fatigue life at 0.5 Hz for 500
during cooling. cycles. Fig. 5(c) shows the life cycle of samples deposited on 50 ␮m
Fig. 4(b) shows the time vs. displacement and time vs. tem- polyimide sheet. The bi-morph showed minor fluctuations in dis-
perature plots of the samples deposited on 75 ␮m sheets. The placement however an average displacement of 0.5 mm, 0.6 mm
temperature of the plate during first cycle was 250 ◦ C and for and 0.65 mm was observed with different voltages. The 75 ␮m
the second and the third cycle the temperature was increased to thick Cu-Al-Ni/polyimide bi-morphs showed no signs of fatigue
300 ◦ C. By performing this, the thermal fatigue limit of the bi-morph and exhibited a consistent and steady displacement of 0.75 mm,
was deduced. It can be observed that a maximum displacement 1.05 and 1.4 mm.
of 19 mm was achieved from the edge of the bi-morph. The time The stiffness of 50 ␮m polyimide sheets is lower than 75 ␮m
required to reach this maximum displacement during heating was sheets, which directly affect the magnitude of pre-strain applied
37 s. The cooling cycle takes more time as natural heat convection to the sheets. After deposition, the developed films generate a
was allowed to cool the sample. The cooling time was approxi- compressive stress which tends to act against the stiffness of the
mately 75 s and the film retuned to its original position after 110 s, polyimide substrate. This was distinct, as there was increase in cur-
without any plastic deformation. As the temperature was increased vature of the bi-morph. Further the radius of curvature of 50 ␮m
to 300 ◦ C, the displacement of the bi-morph reduced to 17 mm, sheets was higher due to its low stiffness. As observed from the
and the retraction took same time as the first cooling cycle. When shape recovery ratio graphs the shape memory effect of 50 ␮m
32 A. K et al. / Sensors and Actuators A 254 (2017) 28–35

Fig. 4. (a) Shape recovery ratio of 50 ␮m and 75 ␮m SMA/polyimide bimorph, (b) cyclic heating and cooling to find the maximum displacement of the bimorph, (c) hysteresis
curve showing the time lag which was high at initial stages, (d) Hysteresis plot after attaining maximum displacement (e) pictures of the bimorph at various stages of
actuation.

bi-morph sheets, was not sufficient to recover from the compres- - XRD results a high intensity peak corresponding to ␤ (220) and
sive stress completely. Also the inability of 50 ␮m to overcome the the crystallite size was found to be 6.67 nm, which shows the
stress, with the given actuation conditions was evident from the crystallinity of the developed structures.
fluctuations observed in the life cycle analysis. Whereas in case - SEM images showed a continuous film with a grain size of approx-
of 75 ␮m sheet the stress induced in the SMA film was recov- imately 100 nm.
ered with all the actuation conditions. Stiffness and the residual - The thermal decomposition of the Cu-Al-Ni/Polyimide bi-morph
stress was optimum for the SMA film to recover its shape effort- was rapid when compared to bare polyimide sheet as confirmed
lessly. by TGA analysis.
As it can be observed from the life cycle analysis, 50 ␮m - The austenite transformation temperature was found to be
CuAlNi/polyimide bi-morphs has unstable actuation behavior with As = 215 ◦ C and Af = 240 ◦ C measured by temperature vs resistance
fluctuations. The displacement was constantly varying during plots.
actuation at varying frequencies and voltage. There was no satu- - The bi-morph structures without any post-processing and train-
ration attained even after 500 cycles. However, 75 ␮m bi-morphs ing, showed maximum displacement of 19 mm during both
displacement presented a steady and stable actuation behavior heating and cooling cycles.
throughout the 500 cycles. - The shape recovery ratio was calculated and it was found that
75 ␮m polyimide sheet had better recoverability of than 50 ␮m.
4. Conclusion - The cyclic behavior was studied using an electrical actuation and
the bi-morph was tested for 500 cycles and the bi-morph showed
From the above discussion, it can be concluded that Cu-Al- minor signs of deviation from the average displacement.
Ni/polyimide bi-morphs developed through thermal evaporation - 75 ␮m thick polyimide substrate has a stable life as compared to
showed cyclic repeatability. The results are summarized as 50 ␮m sheets and has a better applicability in devices

- The adhesion between Cu-Al-Ni and polyimide was tested using The as developed structures are suitable to be used as high tem-
scotch tape analysis and there was no removal of the deposited perature actuators such as a bi-morph in electrical circuit breaker as
SMA film. shown in Fig. 6. Conventionally a bimetallic strip is used for smaller,
 A. K et al. / Sensors and Actuators A 254 (2017) 28–35 33

Fig. 5. (a) Maximum displacement obtained through electrical actuation for 50 ␮m PI, (b) Maximum displacement obtained through electrical actuation for 75 ␮m PI (c) Life
cycles analysis of 50 ␮m showing the deviation in displacement for the measured 500 cycles (d) Life cycles analysis of 75 ␮m showing the deviation in displacement for the
measured 500 cycles.

heating process can be utilized as a mechanism for analyzing the

effect of substrate thickness for large cycles.

Acknowledgments

The authors would like to thank Mr. Mayank Modak from heat
Transfer Lab IIT Indore and Mr. Shivendra K Pandey from Phase
Change Memory Lab IIT Indore for helping us with our characteriza-
tion. We would also like the thank Molecular and Nano-Electronics
Research Group (MNRG) from IIT Indore for their valuable sup-
port during the work. The authors are grateful for the continuous
support from Sophisticated Instrumentation Centre of IIT Indore.

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 A. K et al. / Sensors and Actuators A 254 (2017) 28–35 35

Ashish Shukla obtained his Master’s degree from Delhi Tameshwer Nath did his Masters in Manufacturing Sys-
Technological University. He is currently a Ph.D. student tems Engineering at SLIET, Longowal, Punjab. He is
at Indian Institute of Technology Indore, where he is work- pursuing his Ph.D from Indian Institute of Technology
ing on underwater laser etching on flexible substrates. His Indore. His research interest includes Bond Graph Mod-
areas of specialization include material characterization eling, Control Systems, and Mechatronics.
and laser based surface texturing for Photovoltaic devices.

Dr. I.A. Palani is working as Associate Professor in the

Discipline of Mechanical Engineering, IIT Indore and also
the Head of Metallurgy Engineering and Material Science.
Karthick S had completed his Masters in Control and
He did his Post-Doctoral Fellow in Graduate school of
Instrumentation Engineering at College of Engineer-
Information Science and Electrical Engineering, Kyushu
ing – Guindy, Anna University Chennai. Previously he
University, Japan. He completed his PhD from Depart-
was working with NIT Tiruchirappalli and Kurukshetra.
ment of Mechanical Engineering from IIT Madras, India.
Presently he is working for his research at Indian Institute
He has authored in book chapters on “ZnO Nanocrys-
of Technology Indore. His areas of interest are Instrument
tals and allied Materials”. His area of interest includes
System Design, Modelling and Analysis, Process Control
laser assisted micro processing, surface engineering, opto-
and Automation, Control and Computing.
mechatronics, smart materials and nano structures for
functional device.