Micro-Compression Study of Ni-Fe(Co)-Ga Magnetic

Shape Memory Alloy for MEMS Sensors

Kengo Igawa1,2,3, Tso-Fu Mark Chang1,2,3, Chun-Yi Chen1,2,3, Akira Umise2,4, Takashi Nagoshi 5, Masaki Tahara1,2,
Tomonari Inamura1,2, Hideki Hosoda1,2, Volodymyr A. Chernenko1,6,7, Masato Sone1,2,3
1
Laboratory for Materials and Structures, Tokyo Institute of Technology, Yokohama 226-8503, Japan
2
Laboratory for Future Interdisciplinary Research of Science and Technology,
Tokyo Institute of Technology, Yokohama 226-8503, Japan
3
CREST, Japan Science and Technology Agency, Yokohama 226-8503, Japan
4
Institute of Biomaterials and Bioengineering, Tokyo Medical and Dental University, Tokyo 101-0062, Japan
5
National Institute of Advanced Industrial Science and Technology, Ibaraki 305-8564 Japan
6
BCMaterials & University of Basque Country, UPV/EHU, Bilbao 48080, Spain
7
Ikerbasque, Basque Foundation for Science, Bilbao 48013, Spain
E-mail: sone.m.aa@m.titech.ac.jp

Abstract—Magnetic shape memory alloys (MSMAs) are
expected to be implemented into micro actuators and sensors
because they have a large magnetic field induced strain combined
and high response frequency. On the other hand, when dimensions
of metallic materials are reduced from a bulk size to the
micrometer scale, the mechanical response would vary along with
the dimension change. Therefore, it is important to evaluate the
mechanical properties of microscale specimens of shape memory
alloys to be implemented in miniaturized devices. In the present
work, the superelastic properties of the single crystal of
Ni50Fe19Co4Ga27 (at.%) MSMA have been studied by a micro-
compression testing. The specimens were micropillars, fabricated
by a focus ion beam technique. The compression stress-strain
hysteretic dependences show typical superelastic behavior in a
wide temperature range alongside a tendency to disappearance of
hysteresis near the critical point at about 373K. The temperature
shifts the martensitic transformation start stress with a rate of ~1.1
MPa/K, which is similar in value to the bulk alloy. Thus, the
studied alloy could retain the superelastic properties, including in
a postcritical region, down to microscale.
Keywords—Ni-Fe(Co)-Ga Shape memory alloy; Superelasticity;
Micro-compression test
I. INTRODUCTION
Shape memory alloys (SMAs) exhibit a shape memory effect
(SME), when they recover, during heating across the reverse
martensitic transformation (MT), a large deformation induced in
martensite; and superlasticity effect (SE), when they are heavily
deformed and unloaded in austenite owing to reversible stress-
induced MT. SMAs exhibit SE in the temperature range between
the austenite transformation finish temperature ( ) and a
maximum temperature (Md) where the conventional plastic
deformation of martensite occurs. SME and SE make SMAs
promising materials for the applications as actuators and/or
sensors in the micro-electro-mechanical-systems (MEMS) [1,
2].
The thermal actuation due to the SME is too slow, so the
conventional nonmagnetic SMAs are not suitable for the
applications requiring a high frequency response. To solve this
problem, magnetic shape memory alloys (MSMAs) have been
developed [3]. MSMAs can generate a large magnetic field
induced strain with a relatively high frequency. Hence, these
materials are very attractive for applications in the rapid micro-
actuators and sensors.
Heusler type Ni50Fe19Co4Ga27 (at.%) alloy is one of the
MSMAs which exhibits a reduced hysteresis in the superelastic
regime [4]. MSMAs showing small hysteresis possess the high
stability to fatigue [5]. The A for the Ni50Fe19Co4Ga27 alloy is
about 270 K [4]. Therefore, this MSMA is appropriate to study
a superelastic behavior in the compression mode at the room
temperature and above it.
When SMAs are examined on the microscale, the
mechanical response and its temperature dependence can be
significantly different than those in the bulk alloy [6,7]. It is also
typical for SMAs that MT temperatures change as a function of
the specimen size. For instance, in the Cu-Al-Ni microwire the
MT temperatures increase when diameter of the wire decreases
[7].
In this study, superelastic properties of the Ni50Fe19Co4Ga27
micropillars have been disclosed by the micro-compression tests
at various temperatures and “stress – temperature” phase
diagram is obtained.
II. EXPERIMENTAL METHODS
A. Fabrication of micro-pillars
Crystallographic grains situated at the edge of a thin plate,
cut from the Ni50Fe19Co4Ga27 polycrystalline alloy prepared in
this work, were used to fabricate the micropillars. Non-tapered
pillar fabrication was conducted by a focused ion beam (FIB)
(FB2001, Hitachi) with ion irradiation parallel to the pillar axis.
The pillar fabrication steps are illustrated in Fig. 1. At first, two
squared areas were milled away from the plate leaving a
rectangular pillar at its edge. Then, all corners of the pillar were
further milled away by FIB at 45 deg. with the plate. Each face
of the pillar was then polished with a low current beam to
remove damaged surface and make it smooth. Final dimensions
of the pillars were 10 × 10 × 20μm . The crystallographic
orientation of each pillar was determined using scanning
electron microscope (SEM, S-4300SE, Hitachi) equipped with
the electron backscattered diffraction (EBSD) detector (e-Flash,
Bruker AXS).

978-1-5090-1012-7/17/$31.00 ©2017 IEEE

B. Micro-compression test
The micro-compression tests were conducted with an in-
house made test machine [8]. The general view of machine and
its components are shown in Fig. 2. Specimen holder attached to
the X-Y-Z stage was carefully manipulated to align the pillar
with a flat-ended indenter. The compression was controlled by a
Fig.1 Schematic showing flow of the pillar fabrication steps.
Fig.2 General view of machine designed for the mechanical testing of
micro-sized specimens and its schematic
Fig.3 The view of the temperature stage variable test.
piezoelectric actuator at a rate of 0.01 μm/s. The displacement
and the force applied were recorded by an AC/DC converter.
The in-situ optical images were obtained with a CCD camera.
The temperature control during mechanical tests was realized by
placing the sample holder between two heaters, as shown in Fig.
3. The thermocouple was in a contact with sample holder. Each
“loading/unloading” cycle was performed at fixed temperatures
which was step-wise increased by 15~20 K. The temperature
was 298 K in the first cycle, and 393 K in the last cycle.
III. RESULTS AND DISCUSSION
Images of the selected micro-pillar before and after full set
of the micro-compression tests are shown in Fig. 4. The as-
fabricated pillar was not tapered and had a smooth surface. The
crystal orientation along the compression axis was identified by
EBSD to be [436]. By comparing the pillar before and after the
test, shape and size of the pillar turned out not changed. In other
words, the pillar exhibited a perfect superelasticity effect.
Fig.4 SEM images of the micropillar before and after compressions
under different constant temperatures.
Fig.5 Stress-strain curves during compressive loading and unloading
of micropillar at different temperatures. Arrow indicate the MT start
stress at each temperature.
The engineering stress-strain curves at different
temperatures are shown in Fig. 5. The initial part of the curve at
room temperature (298K) is linear reflecting an elastic
deformation of austenite. When the stress reaches about 110
MPa, the stress-induced MT starts and during further loading the
preferentially oriented martensite variants are formed giving rise
to an accumulation of the significant deformation (about 3%).
After a plateau-like part of the curve corresponding to MT is
ended, the second linear part appears due to the elastic behavior
of martensitic phase. During unloading, the strain recovery
occurs due to the reverse MT with a stress hysteresis originated
from the MT first-order character. The hysteretic stress-strain
loop, like the one obtained at room temperature, is a signature of
the conventional superelastic effect. Fig. 5 shows evolution of
the superelastic curves with the temperature elevation. The
results confirm that the superelastic behavior occurs in the
micropillars at all the test temperatures, also meaning that the
temperature of this alloy is not achieved, i.e., it is higher than
393K. The turning points on the stress-strain curves in Fig. 5
marked by arrows correspond to the MT start stress, σs. Two
main important features of the temperature evolution of
superelastic loops in Fig. 5 can be outlined: (i) increasing of
critical stress; and (ii) tendency to the disappearance of stress
hysteresis.
 Concerning evolution (i), despite large scatter of results,
the plot depicted in Fig. 6 can be roughly approximated by a
straight line described by Clausius-Clapeyron equation:
/ =− / (1)
where , Δ and is test temperature, transformation entropy
and transformation strain, respectively. Stress and directions
have the same sign and correspond to the same crystal
orientation. Since Δ is always negative, the derivative in Eq.(1)
is always positive. The slope of line shown in Fig. 6 is equal to
1.1 MPa/K. This value is similar to 0.95 MPa/K obtained for the
bulk single crystal Ni49Fe18Ga27Co6 studied in the tensile mode
and in different crystal direction [9]. Thus, Ni-Fe(Co)-Ga
micropillars retain superelastic properties observed in the bulk.
200
160
Stress/MPa
120
80
40
0 to check minor over-heating,” Sens. Actuators, A, vol. 238, pp. 337–343,
260 280 300 320 340 360 380 400 420
Temperature/K
Fig.6 Temperature dependence of transformation start stress. The dependence
is ended in the point marked by an open circle, presumably considered as the
critical point.
Evolution (ii), seemingly, results, in the almost zero-
hysteretic curve at T=373K, which means that this temperature
value and the corresponding σs≈160MPa could be accepted as
provisional coordinates of a critical point at the “σs versus T“
phase diagram (see Ref.4 for more detail). More studies are
needed to confirm the postcritical behavior of the strain above
critical point.
IV. CONCLUSIONS
Superelastic properties of the Ni50Fe19Co4Ga27 magnetic
shape memory micropillars for applications in the micro-
actuators and sensors at various temperatures were evaluated in
this study. The following main conclusions can be drawn:
• No change in shape and size of the micro-pillar was observed
after the compression tests at all temperatures.
• The stress-strain curves confirmed the superelastic behavior
at all temperatures.
• No plastic deformation was observed at 393 K, which
indicates that M temperature of the pillar is higher than 393
K.
• The temperature dependence of the MT start stress, although
dispersed, presumingly, due to impossibility to measure
directly the pillar temperature, was approximated by straight
line according to Clausius-Capeyron relationship with a
slope of ⁄ = 1.1 MPa/K which is similar to that in
the bulk alloy. It is speculated that (T) phase diagram is
terminated at a critical point. In a postcritical region, above
373 K, the micropillar should exhibit still large nonlinear
anhysteretic strain behavior.
• The results imply that the pillars of Ni50Fe19Co4Ga27 MSMA
can retain the superelastic behavior in a wide range of
temperatures similar to the bulk, which is advantageous for
applications in the microscale actuators and sensors.
ACKNOWLEDGMENT
This work has been supported by the Grant-in-Aid for
Scientific Research (S) (JSPS KAKENHI Grant Number
26220907), Wakate B (JSPS KAKENHI Grant Number
26870194) and CREST Project (#14531864) operated by the
Japan Science and Technology Agency (JST), as well as by the
project MAT2014-56116-C4-3-4-R by Spanish Ministry of
Economy and Competitiveness.
REFERENCES
[1] C. Tang, T.X. Wang, W.M. Huang, L. Sun, and X.Y. Gao, “Temperature
sensors based on the temperature memory effect in shape memory alloys
2016.
[2] W.L. Benard, H. Kahn, A.H. Heuer, and M.A. Huff, “Thin-film shape-
memory alloy actuated micropumps,” J. Microelectromech. S. , vol. 7, pp.
245–251, 1998.
[3] J.M. Stephan, E. Pagounis, M. Laufenberg, O. Paul, and P. Ruther, “A
novel concept for strain sensing based on the ferromagnetic shape
memory alloy NiMnGa,” IEEE Sens. J., vol. 11, pp. 2683–2689, 2011.
[4] V.A.Chernenko, V.A. L’vov, S.Kabra, I.R.Aseguinolaza, M.Kohl, H.
Hosoda, and J.M. Barandiaran “Large Anhysteretic Deformation of Shape
Memory Alloys at Postcritical Temperatures and Stresses,” Phys. Status
Solidi B, 1700273, 2017.
[5] Y. Chumlyakov, E. Panchenko, I. Kireeva, I. Karaman, H. Sehitoglu, and
H.J. Maier, “Orientation dependence and tension/compression asymmetry
of shape memory effect and superelasticity in ferromagnetic Co40Ni33Al27,
Co49Ni21Ga30 and Ni54Fe19Ga27 single crystals,” Mater. Sci. Eng., A, vol.
481-482, pp. 95–100, 2008.
[6] L. Riccardi, G. Rizzello, D. Naso, B. Holz, S. Seelecke, H. Janocha, and
B. Turchiano, “Modeling and control of innovative smart materials and
actuators: A tutorial,” 2014 IEEE Conference on Control Applications,
pp. 965–977, 2014.
[7] Y. Chen and C.A. Schuh, “Size effects in shape memory alloy
microwires,” Acta Mater., vol. 59, pp. 537–553, 2011.
[8] A. Shibata, T. Nagoshi, M. Sone, S. Morito, and Y. Higo, “Evaluation of
the block boundary and sub-block boundary strengths of ferrous lath
martensite using a micro-bending test,” Mater. Sci. Eng., A, vol. 527, pp.
7538–7544, 2010.
[9] K. Oikawa, R. Saito, K. Anzai, H. Ishikawa, Y. Sutou, T. Omori, A.
Yoshikawa,V.A. Chernenko, S. Besseghini, A. Gambardella, R. Kainuma
and K. Ishida. “Elastic and Superelastic Properties of NiFeCoGa Fibers
Grown by Micro-Pulling-Down Method”. Mater.Trans. vol. 50, pp.934 -
937,2009.