Size effects of Superelasticity in Nanocrystalline NiTi
Shape Memory Alloy
Fei Wang1, Ping Huang2,*, Wenqiang Chen2, and Kewei Xu2
Abstract-NiTi shape memoy alloy thin film has been received
considerable attention because of their application as actuators
in micro- and nano-electro-mechanical systems. In this study, the
analysis of NiTi shape memory thin film by combining
transmission electron microscopy and nanoindentation
techniques were carried out elucidating the influence of the
grain size and the indentation depth on superelasticity. Partial
recovery was observed from the load-depth curves formed by a
Berkovich diamond indenter and the depth recovery ratio and
the energy recovery ratio at various indentation depth and grain
sizes were evaluated. The mechanism behind these observations
are explained and extended discussed.
BACKGROUND
With a growing requirement in developing micro- and
nano-electro-mechanical systems (MEMS and NEMS),
fabrication and characterization of such small scale materials
are being posed great challenge for both science and
technology [1-2]. Especially, nickel-titanium (NiTi) shape
memory alloys which was proposed to be an ideal candidate
of nanoscale actuators have been exploited extensively in
various MEMS and NEMS systems [3]. Its shape memory
effect, known for the ability to recover its initial shape after
deformation via solid-state phase change, has been well
characterized in coarse grain size and bulk form. It has been
reported that the shape memory properties of NiTi alloy
depend on its microstructure, and further miniaturized
actuator devices require the use of very thin film. Therefore, it
is very important to understand the effects of both grain
structure and deformation scale on mechanical properties.
However, fundamental knowledge of those size effects on
mechanical properties in NiTi alloy is still lacking and some
inconsistent findings remains [4]. In present study, we focus
on the grain size and depth dependence of pseudoelasticity in
nanocrystalline NiTi shape alloy thin film.
CURRENT RESULTS
The NiTi thin films were deposited by means of direct
current magnetron sputtering from an equiatomic NiTi and an
elemental Ti target at different temperature on the substrate.
1
MOE Key Laboratory for Strength and Vibration, School of Aerospace,
Xian Jiaotong University, Xi’an, 710049, People’s Republic of China.
2
State-key Laboratory for Mechanical Behavior of Material, Xi’an Jiaotong
University, Xi’an, 710049ୈPeople’s Republic of China.
*Contacting Author: Email address: huangping@mail.xjtu.edu.cn,
Phone:0086-29-82663869, Fax: 0086-29-82663453
978-1-4244-3544-9/10/$25.00 ©2010 IEEE
The plan-view microstructure of the NiTi thin films with
different depositing temperature are shown in the
transmission electron microscopy images of Fig.1. At
depositing temperature of 320, the NiTi alloy is not fully
crystallized and only few areas exhibit crystalline structure as
shown in Fig. 1a. When depositing temperature increases
slightly to 370, the NiTi thin film is fully crystallized and the
grain size is about 70nm. With temperature increasing, the
grain size of NiTi thin film enlarged significantly in to micron
scale as shown in Fig. 1b to Fig. 1d. The XRD analysis shown
in Fig. 2 is consistent with the TEM observation and shows
the changes of orientation at various depositing state.
The nanoindentation tests were conducted using the MTS
Nanoindenter XP® system (MTS, Inc) under continuous
stiffness measurement (CSM) mode. Different indentation
depths ranging from 50 to 150nm were applied (Fig. 3). Then,
indentation induced superelastic effect was characterized by
the depth recovery ratio obtained from indentation load-depth
curves and energy recovery ratio. The depth recovery ratio
may be defined as:
hmax  hr
Kh (1)
hmax
The energy recovery ratio is definded as the ratio of reversible
work to total work:
hmax
We
³
hr
F ˜ dh
(2)
Kw hmax
Wt
³
0
F ˜ dh
Fig. 4 shows the depth recovery and energy recovery of the
NiTi thin films. Two regimes were identified as the recovery
ratio is independent on grain size when indentation depth is
larger than 100nm, whereas the NiTi thin film with smaller
grain size exhibits more significant superelastic effect when
indentation depth less than 100nm. Those observations
provide new insides concerning the size effects on the
mechanical properties of NiTi alloy as application of actuator
in MEMS or NEMS systems.
[1] K. Bhattacharya and R. D. James, “The material is the machine,”
Science, vol.
[2] J. M. San Juan, M. L. No, C. A. Schuh, “Superelasticity and shape
memory in micro-and nanometer-scale pillars,” Adv.Mater. vol.20,
2008, pp. 272-278.
[3] Y. Fu, H. Du, W. Huang, S. Zhang and M. Hu, “TiNi-based thin films
in MEMS applications: a review,” Sensors. Actuators. A. vol.112, 2004,
pp.395.
[4] C. P. Frick, B. G. Clark, S. Orso, P. Sonnweber-Ribic and E. Arzt,
“Orientation-independent pseudoelasticity in small-scale NiTi
compression pillars,” Scripta. Mater. vol.59, 2008. pp. 7-10.
 (a) (b)

(c) (d) Fig. 3. Typical indentation load versus indentation depth from one test
performed at each initial indentation depth, the inset shows the XRD
results of the sample

Fig. 1. Plan-view TEM bright-field micrographs of NiTi deposited on

substrate with temperature of (a) 320ć, (b) 370ć, (c) 420ć and (d) 470ć.

Fig. 4. (a) Depth recovery ratio and (a) energy recovery ratio plotted as a
Fig. 2. XRD profiles of the NiTi thin film at different deposited state function of indentation depth for the NiTi thin films deposited at substrate
temperature range of 340§ to 470§.