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Experimental observations on mechanical response of three-phase NiTi shape memory alloy

under uniaxial tension

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2016 Mater. Res. Express 3 105701
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Mater. Res. Express 3 (2016) 105701

doi:10.1088/2053-1591/3/10/105701

PAPER

RECEIVED

16 September 2016
REVISED

Experimental observations on mechanical response of three-phase

NiTi shape memory alloy under uniaxial tension

2 October 2016
ACCEPTED FOR PUBLICATION

Yao Xiao, Pan Zeng and Liping Lei

5 October 2016

Department of Mechanical Engineering, Tsinghua University, Beijing 100084, Peoples Republic of China

PUBLISHED

E-mail: zengp@mail.tsinghua.edu.cn

19 October 2016

Keywords: shape memory alloy, strain localization, reorientation, digital image correlation

Abstract
In this paper, the mechanical behavior of three-phase NiTi shape memory alloy (SMA) is examined in
a wide temperature range using in situ digital image correlation. By varying the temperature and the
cooling/heating history, we get the specimens with initial austenite (A), initial R-phase (R), initial
martensite (M), initial mixture of A and R, initial mixture of R and M and initial mixture of A and M. It
is observed in the experiments that NiTi SMA exhibits localized AM transformation and RM
transformation while homogenous R-reorientation and martensitic reorientation. Moreover, the
inuence of the initial mixed states, i.e. mixture of A and M, mixture of R and M and mixture of A and
R, on the mechanical response of NiTi SMA is discussed. Interestingly, we nd that the specimens with
initial mixture of R and M demonstrate homogenous deformation manner and the emergence of R in
M facilitates the transformation of NiTi SMA greatly. The three-phase phase diagram is also
established. The thermal dependences of the critical transformation stresses associated with various
transformation processes are calculated for further theoretical investigation and simulation.

1. Introduction
NiTi shape memory alloy (SMA) has been widely deployed in engineering applications due to the unique
features such as superelasticity and shape memory effect, arising from the solidsolid reversible phase
transformation between austenite (A) and martensite (M) directly or via intermediate R-phase (R) [1, 2]. Due to
the practical use in the engineering community, the fatigue performance of SMA has garnered signicant
attention [39] and it is found that the well-known localized AM transformation in NiTi SMA [1017]
contributes a lot to its fatigue and fracture [18, 19]. In recent years, increasing attention is also paid to the Rphase related transformation. Although the transformation strain of R-phase related transformation (about 1%)
is much less than that of AM transformation (about 7%), R-phase related transformation exhibited small
temperature hysteresis and stable dynamic behavior without varying much with cycling, thus demonstrating
excellent functional fatigue properties [20]. Owing to this arresting feature, R-phase related transformation is
viewed as an attractive alternative for the design of actuator with narrow hysteresis and small strain [20, 21]. In
order to detect and distinguish R-phase related transformation, Sittner et al [2224] utilized in situ neutron
diffraction and ultrasonic measurements to study the mechanical response of NiTi SMA with R-phase under
different thermomechanical loadings. Ng and Sun [25] investigated the deformation behavior of polycrystalline
NiTi tubes with initial A, R, M and the mixture of A and R. Homogeneous deformation mode and localized
deformation mode were identied in martensitic reorientation and AM transformation, respectively.
Helbert et al [26] investigated the impacts of the temperature, the strain rate and the mechanical cycling on the
deformation behavior of NiTi SMA in the presence of R-phase. The homogeneous AR transformation was
observed by strain measurement and infrared imaging.
Although lots of literatures listed and not listed here focused on the global mechanical response of AM
transformation and that of R-phase related transformation, we know relatively little about the local mechanical
response of three-phase NiTi SMA. In this paper, we tested three-phase NiTi SMA in a wide range of
2016 IOP Publishing Ltd

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Figure 1. DSC thermogram of NiTi SMA.

temperature through in situ digital image correlation (DIC). The local deformation behavior of NiTi SMA with
various initial phases, i.e. A, R, M and their mixtures, are systematically studied. The three-phase phase diagram
is also presented in order that it can be utilized for further theoretical investigation and simulation.

2. Experimental methods
2.1. Material characterization
As-received polycrystalline NiTi sheets (55.12 wt% Ni, Memry Corp.) with thickness of 1.0 mm were used in the
current study. As discussed in the previous study [27], electrical discharge machining is especially useful for
machining SMA into arbitrary shape without inuencing the material characteristics of the bulk specimen. So all
the specimens in the study were electro-discharge machined into dog-bone shape along the rolling direction.
The gauge section of the sample was 40 mm in length and 6 mm in width. Differential scanning calorimeter
(DSC) test was conducted to measure the phase transformation temperatures of the material. The cooling/
heating rate was 10 C min1. The results are shown in gure 1. The austenite start temperature, the austenite
nish temperature, the R-phase start temperature, the R-phase nish temperature, the martensite start
temperature, the martensite nish temperature are denoted as As, Af, Rs, Rf, Ms and Mf, respectively.
2.2. Experimental procedures
All the experiments were performed by Shimadzu AG-X universal testing machine in the environmental
chamber. Since the thermally stable phase of the specimens at room temperature (RT, 25 C) is R or M, the
specimen was rstly heated to the temperature much higher than Af, i.e. 150 C, to recover the possible
deformation at stress-free state. Secondly, in order to obtain the specic initial state, the specimen was mounted
into the testing machine, held under a slight tensile force at about 20 N (3.3 MPa), and cooled down from 150 C
to the testing temperature or the specimen was quenched in liquid nitrogen, and then mounted into the testing
machine, held under a slight tensile force at about 20 N (3.3 MPa), and heated up to the testing temperature.
Finally, the temperature was kept constant and the specimen was loaded/unloaded under displacement control.
The cross-head movement was controlled at a relatively low velocity of 0.4 mm min1 (nominal strain rate of
1.67104 s1) to avoid signicant self-heating/self-cooling [10, 16]. For some of the cases, the shape memory
effect was checked by heating the specimen right after the complete unloading. Upon heating, the specimen was
slightly stretched by constant force about 20 N (3.3 MPa). The heating rate of the environmental chamber was
about 10 C min1.
For the DIC portion of the experiments, the digital images were taken by a CCD camera (Daheng Image,
DH-SV1410FM, with the resolution of 13921040). Before thermomechanical loading, a ne speckle pattern
was sprayed on the surface of the specimen. Two LED lights were put in front of the specimen to guarantee the
adequate illumination intensity. The image of the specimen right prior to straining was chosen as the reference
image. The digital images were post-processed by commercial software NCM-2D. With a subset size of 31 and a
step size of 5, its theoretical resolution is 1/200 pixel and the testing accuracy is up to 0.5 m, which can meet the
requirements of the experiments.
In order to facilitate the subsequent discussion, the identication number of the sample is dened as follows:
for the sample cooled from 150 C to the testing temperature T (in unit Celsius), it is classied as Type C and
denoted as CT; for the liquid-nitrogen-quenched sample heated up to the testing temperature T (in unit Celsius),
2

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Table 1. Testing cases and the initial states of the specimens.

Specimen ID (Type C)
C110
C90
C75
C65
C55
C45
C35
C25
C15
C5
C-5
C-15
C-25

Specimen ID (Type H)

Initial state
A
A
A
A
Mixture of A and R
R
R
Mixture of R and M
Mixture of R and M
Mixture of R and M
Mixture of R and M
M
M

H75
H65
H55
H45
H35
H25
H15
H5
H-5
H-15
H-25

Initial state
A
Mixture of A and M
Mixture of A and M
M
M
M
M
M
M
M
M

it is classied as Type H and dominated as HT. Taking the DSC results into consideration, the testing cases and
the corresponding initial states of the specimens are listed in table 1.

3. Results and discussion

The evolution of the longitudinal strain distribution along the central axis of the specimen is illustrated as the
contour plot in gures 24. In order to show more clearly the thermomechanical response of the specimen, the
evolutions of stress, temperature and global strain are also presented in gures 24. Figures 57 depict the global
mechanical responses of the specimens. The global strain is obtained by averaging the strain eld within the
gauge section.
3.1. Mechanical response of NiTi SMA with initial A and initial A&M mixture
The initial states of Specimens C110, C90, C75, C65 and H75 are A. The initial states of Specimens H55 and H65
are mixture of A and M. The specimens were rst submitted to elastic deformation. Followed by a stress drop
after the nucleation stress peak, localized AM transformation took place, as presented in gure 2. After the
gauge section underwent complete martensitic transformation, subsequent deformation is the elastic
deformation of M. It can be seen in gures 2 and 5 that the transformation strain across AM front, the initial
elastic modulus and the nucleation stress drop of Specimen H55 are much less than those of the other specimens
in this regime. Taking the uniform deformation of Specimen H45 (gure 3(g)) into account, one can easily
conclude that Specimen H55 demonstrates a transient state from homogenous martensitic reorientation to
localized AM transformation. Moreover, the results of H55 and H65 reveal that the emergence of A in M has
signicant inuence on the deformation behavior of NiTi SMA. Even at the testing temperature slightly higher
than As, NiTi SMA exhibits localized deformation feature.
During unloading, three types of deformation modes were observed:
(1) For Specimens C90 and C110, they rst underwent homogeneous deformation. When the stress dropped to
a certain level, MA transformation occurred. Contrary to the commonly observed localized MA
transformation (see references [310] or the results at 90 C), the specimen underwent homogenous MA
transformation at 110 C. Similar phenomenon was also observed in the previous study if the testing
temperature is much higher than Af [28]. After complete unloading, residual strain can be distinguished in
gures 2(d) and (e), which can be attributed to material plasticity [28] and the blocked martensite [29].
(2) For Specimens C65, H55 and H65, upon unloading, they deformed in a homogenous manner and
considerable residual strain was left. Since M was thermally stable in these specimens, the irreversible strain
mainly originated from the presence of stable detwinned martensite. By heating the specimen, most of the
residual strain could be recovered by the shape memory effect, as shown in gures 2(b), (f) and (g).
(3) For Specimens H75 and C75, since the testing temperature was only slightly higher than Af, MA
transformation will proceed at a low stress. So, although theoretically the thermal stable states of Specimens
H75 and C75 are A, the reverse transformation can hardly be completed (H75, gure 2(h)) or even initiated
(C75, gure 2(c)). The retained martensite could be fully transformed back to austenite by heating the
specimen mildly.
3

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Figure 2. The evolution of the longitudinal strain distribution along the central line of the specimen (contour plot), the evolution of
stress (overlaid, black line), the evolution of global strain (overlaid, gray line) and the evolution of the testing temperature (overlaid,
green line). (a)(e) Specimens C55, C65, C75, C90 and C110; (f)(h) Specimens H55, H65 and H75.

3.2. Mechanical response of NiTi SMA with initial R and initial A&R mixture
The initial states of Specimen C45 and C35 are R and the initial state of Specimen C55 is mixture of A and R.
From gure 6, the appearance of double knee (two-stage yielding phenomenon) [30] can be distinguished in
the global stress-strain response of Specimens C35 and C45. As commented by Churchill et al [30], the rst
yielding stage corresponds to R-reorientation. The continuing elongation resulted in the linear response of
reoriented R and then the second yielding stage, indicating RM transformation. As shown in gures 2(a),
3(a) and (b), during the rst yielding stage, the deformation was uniform and the occurrence of the localized
deformation coincided with the second yielding stage. Therefore, it is safe for us to conclude that the specimen
was submitted to homogeneous R-reorientation and localized RM transformation, which is an important
supplement to the previous experimental observations [23, 3034]. The RM transformation bands
4

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Figure 3. The evolution of the longitudinal strain distribution along the central line of the specimen (contour plot), the evolution of
stress (overlaid, black line), the evolution of global strain (overlaid, gray line) and the evolution of the testing temperature (overlaid,
green line). (a)(f) Specimens C45, C35, C25, C15, C5 and C-5; (g)(l) Specimens H45, H35, H25, H15, H5 and H-5.

Mater. Res. Express 3 (2016) 105701

Y Xiao et al

Figure 4. The evolution of the longitudinal strain distribution along the central line of the specimen (contour plot), the evolution of
stress (overlaid, black line), the evolution of global strain (overlaid, gray line) and the evolution of the testing temperature (overlaid,
green line). (a) Specimen C-15, (b) Specimen C-25, (c) Specimen H-15, (d) Specimen H-25.

Figure 5. The global mechanical responses of the specimens with initial A and initial mixture of A and M.

Figure 6. The global mechanical responses of the specimens with initial R and initial mixture of A and R.

Mater. Res. Express 3 (2016) 105701

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Figure 7. The global mechanical responses of the specimens with (a) initial M (temperature lower than Mf), (b) initial M (Type H) and
(c) initial mixture of R and M (Type C).

propagated with the stress maintained almost constant until the band covered all the gauge section of the
specimen. Subsequently, the stressstrain curve rose sharply, which was the macroscopic indicator of the end of
RM transformation in the gauge section [3032]. The unloading response was linear. After complete
unloading, retained martensite led to the accumulation of the residual strain, which could potentially be
recovered upon heating.
3.3. Mechanical response of NiTi SMA with initial M phase and initial R&M mixture
The initial states of Specimens C-15, C-25 and H-25 to H45 are M. As can be seen in gures 3(c)(l) and gure 4,
the specimen was rst subjected to elastic deformation and then the stressstrain curve gradually bent, which
was commonly attributed to the martensitic reorientation [25, 31]. During martensitic reorientation, the
initially twinned martensite variants transform into a single variant which has the highest stability under the
applied stress, leading to a large inelastic strain [35]. Since excessive loading will lead to further detwinning and
eventually massive dislocation [34, 35], the specimens were unloaded when the nominal strain reached 6%.
Subsequent unloading response was linear and the residual strain ranged from 4% to 5%. The irreversible strain
can be attributed to the presence of stable detwinned martensite. The shape memory ability was checked in
Specimens H5 to H45. It was found that most of the residual strain can be recovered by heating the specimen up
to Af. As illustrated in gures 7(a) and (b), for specimens with initial M, despite of some nuances, their global
mechanical responses coincide with each other, regardless of the cooling/heating history and the variation of
testing temperature.
The emergence of R in M has little effect on the deformation mode of NiTi SMA. All of the specimens exhibit
homogenous deformation mode, as shown in gures 3(c)(f). Nevertheless, the appearance of R in M has
signicant inuence on global mechanical response of NiTi SMA. As shown in gure 7(c), when the testing
temperature decreases from 25 C to 5 C, the global mechanical responses of Specimens C25 to C-5
transform from double knee pattern (two-stage yielding phenomenon) to single knee pattern (one-stage
yielding phenomenon). This conversion implies that as the testing temperature decreases from Ms to Mf,
although R-related transformation and martensitic reorientation coexists in the deformation of NiTi SMA, Rreorientation will be gradually suppressed and eventually disappear.
7

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Figure 8. The three-phase phase diagram of NiTi SMA. The critical transformation stresses are obtained from Type C (blue) and Type
H (red) specimens with initial A (solid square), initial R (solid circle), initial M (solid triangle), initial mixture of A and R (open square),
initial mixture of R and M (open circle) and initial mixture of A and M (open triangle). The critical stress of R-orientation
transformation is marked as solid star. The data are t linearly (green dash line) with following slopes: 7.31 MPa/C (AM, RM,
A&MM and A&RM transformations), 0.36 MPa/C (martensitic reorientation), 0.94 MPa/C (R&MM transformation) and 0.32 MPa/C (R-reorientation).

Figure 9. An instance of the determination of critical transformation stress. The stress value of Point A represents the critical stress of
R-reorientation, and the stress value of Point B represents the critical stress of martensitic reorientation.

3.4. Three-phase phase diagram

The three-phase phase diagram revealing the thermal dependence associated with different transformation
processes is shown in gure 8. The y axis of the phase diagram refers to the critical transformation stress of the
specimen. Due to the limitation of the data, only the temperature dependence of forward transformation is
presented. For the specimens with localized transformation behavior, the critical transformation stress is chosen
as the nucleation stress. For the specimens deforming homogenously, the critical stress is determined by the
intersection of the lines t through distinct linear sections from the stress-strain plot. Specially, for Specimens
C15 to C55, two critical stresses will be obtained. As discussed above, the lower critical stress indicates the
beginning of R-reorientation, and the higher critical stress implies the beginning of the martensitic
reorientation. The case of C35 is shown in gure 9 as an instance.
The thermal dependence associated with different transformation processes can be obtained from the phase
diagram. Taking the ClausiusClapeyron equation [3639] into consideration, the thermal dependence of the
transformation is t linearly. Since the slopes of RM transformation and AM transformation are very
similar [26, 30], the critical stresses of AM, RM, A&RM and A&MM transformations are t into
a single line. Its slope is 7.31 MPa/C, which is in good agreement with the data published in the existing
literatures [26, 30, 31, 40, 41]. The slopes of R&MM transformation, R-reorientation and martensitic
reorientation are 0.94 MPa/C, 0.32 MPa/C and 0.36 MPa/C, respectively. The results further verify the
earlier observations that the critical stresses for R-reorientation and martensitic reorientation are relatively
independent of the temperature [30, 42].
Given the phase diagram and the aforementioned experimental observations, we are able to have a
comprehensive understanding on the mechanical response of three-phase NiTi SMA. If the temperature is
higher than Af or lower than Mf, the global mechanical responses of the specimens at a given testing temperature,
8

Mater. Res. Express 3 (2016) 105701

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e.g. specimens tested at 75 C, 15 C and 25 C, coincide with each other regardless of the cooling/heating
history. If the temperature locates between Mf and Ms, the emergence of R in M facilitates the transformation
greatly (see 5 C 25 C in phase diagram), while has little effects on the deformation modes. If the
temperature locates between Ms and Af, the critical transformation stresses at a given temperature are
approximately identical (see 35 C 65 C in phase diagram). However, the stress-strain responses may vary
greatly with each other in terms of the length of the stress plateau, the number of the yielding stage (single knee
pattern versus double knee pattern) and the deformation mode (localized deformation versus homogenous
deformation).

4. Conclusions
In this paper, the mechanical behavior of three-phase NiTi is examined in a wide temperature range utilizing
in situ DIC. By varying the temperature and the cooling/heating history, we get the specimens with initial A,
initial R, initial M, initial mixture of A and R, initial mixture of R and M and initial mixture of A and M. From the
experimental results obtained in the present study, the following conclusions can be drawn:
(1) NiTi SMA exhibits localized AM and RM transformations while homogenous R-reorientation and
martensitic reorientation. The emergence of R-reorientation can be identied by the appearance of double
knee (two-stage yielding phenomenon) from the global mechanical response of NiTi SMA.
(2) At the temperature between Mf and Ms, NiTi SMA with initial mixture of R and M demonstrates
homogenous deformation manner. At the temperature between As and Af, NiTi SMA with initial mixture of
A and M exhibits localized deformation mode.
(3) From the phase diagram, we nd that the slopes of the critical stresses of AM, RM, A&RM and
A&MM transformations are 7.31 MPa/C. The slope of R&MM transformation is 0.94 MPa/C.
The thermal dependences of R-reorientation and martensitic reorientation are 0.32 MPa/C and
0.36 MPa/C, respectively, which means these two procedures are temperature insensitive.
(4) The emergence of R in M facilitates the transformation of NiTi SMA greatly, while has little effect on the
deformation modes. Nevertheless, the emergence of A in M has signicant inuence on the deformation
behavior of NiTi SMA. Even at the testing temperature slightly higher than As, NiTi SMA exhibits localized
deformation feature.

Acknowledgments
The authors gratefully acknowledge the nancial support from National Natural Science Foundation of China
(No.51275270).

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