Intermetallics 32 (2013) 344e351

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Intermetallics
journal homepage: www.elsevier.com/locate/intermet

Inuence of annealing on NiTi shape memory alloy subjected to severe plastic

deformation
Shuyong Jiang a, *, Yanqiu Zhang a, Lihong Zhao a, Yufeng Zheng b
a
b

Industrial Training Centre, Harbin Engineering University, Harbin 150001, China

Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001, China

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 13 February 2012
Received in revised form
30 April 2012
Accepted 19 July 2012
Available online 10 October 2012

The amorphous phase with the retained nanocrystalline phase, the deformation bands and the amorphous bands coexist due to inhomogeneous plastic deformation in nickeletitanium shape memory alloy
(NiTi SMA) subjected to severe plastic deformation (SPD) based on local canning compression. Transmission electron microscopy, X-ray diffraction and differential scanning calorimetry are used to investigate microstructural evolution and phase transformation of NiTi sample subjected to SPD in the case of
annealing for 2 h at 300
C, 450
C and 600
C, respectively. Annealing at 300
C and 450
C leads to
nanocrystallization of amorphous NiTi sample, while annealing at 600
C results in the coarse-grained
NiTi sample, where the (001) martensite compound twins are found. The precipitation phases such as
Ni4Ti3 and Ni3Ti are suppressed in NiTi sample formed as a result of crystallization of the amorphous
structure and thus occur more easily in the deformation bands in the case of annealing. Martensitic
phase transformation is inuenced by the grain size and is suppressed with the decrease in the nanocrystalline grain size.
2012 Elsevier Ltd. All rights reserved.

Keywords:
A. Nanostructured intermetallics
B. Martensitic transformations
B. Shape-memory effects
C. Heat treatment
C. Plastic forming, cold

1. Introduction
Nickeletitanium shape memory alloy (NiTi SMA) is widely
used in engineering elds due to its shape-memory effect as well
as superelasticity [1]. Cold working plays an important role in
engineering application of NiTi SMA and has a signicant inuence on shape-memory effect as well as superelasticity of NiTi
SMA. In general, cold plastic deformation leads to a high density
of dislocations in NiTi SMA, which makes a contribution to
superelasticity of NiTi SMA [2e4]. However, severe plastic
deformation (SPD) based on cold working is able to lead to
nanocrystallization or amorphization of NiTi SMA. So far, plenty
of work with respect to SPD of NiTi SMA in the case of cold
working has been done over the last decade by means of highpressure torsion (HPT) [5,6], cold rolling [7,8], cold drawing
[9,10] and surface mechanical attrition treatment (SMAT) [11,12].
SPD of NiTi SMA followed by subsequently appropriate heat
treatment contributes to improving the mechanical properties
and the functional properties of NiTi SMA, such as high ultimate
strength and high elongation at the elevated temperatures [13]
and perfect superelasticity [14,15], which is attributed to

* Corresponding author. Tel.: 86 139 36266338; fax: 86 451 82519952.

E-mail address: jiangshy@sina.com (S. Jiang).
0966-9795/$ e see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.intermet.2012.07.025

nanocrystallization of amorphous NiTi SMA prepared by SPD in

the case of annealing. Many researchers investigated crystallization mechanism of amorphous NiTi SMA subjected to SPD and
phase transformation behaviour of NiTi SMA after crystallization.
Waitz et al. [16,17] induced nanocrystallization of an amorphous
NiTi SMA based on HPT in the case of annealing and found that
martensitic phase transformation is suppressed with decreasing
the nanocrystalline grain size and phase transformation behaviour is closely related to the nanocrystalline grain size. Peterlechner et al. [18] studied relaxation and crystallization kinetics
of amorphous NiTi SMA made by repeated cold rolling and
revealed that nucleation and growth of the crystalline phase is
based on mixed nucleation or nucleation with a decreasing rate
as well as three-dimensional growth. Srivastava et al. [19]
investigated the inuence of the different annealing temperatures on crystallization of amorphous bands of cold-rolled
NiTi SMA and demonstrated that annealing for 30 min at or
above 350
C leads to crystallization of the amorphous regions
and the grain size increases with the increase in the annealing
temperature.
In the present study, local canning compression was used in
order to lead to SPD of NiTi SMA, and subsequently the inuence of
annealing on microstructural evolution, precipitation and phase
transformation of NiTi samples subjected to SPD was investigated
systematically.

S. Jiang et al. / Intermetallics 32 (2013) 344e351

2. Materials and methods

As-received NiTi alloy with a nominal composition of Ni50.9Ti49.1
(at.%) was prepared by means of vacuum induction melting
method, and then was rolled at 800
C and nally was drawn to
NiTi bar with the diameter of 12 mm. The transformation temperatures of NiTi bar are as follows: Ms 27.2
C, Mf 41.7
C,
As 17.3
C, Af 4.1
C. Therefore, microstructure of as-received
NiTi bar possesses a typical B2 austenite structure at room
temperature. NiTi samples with the diameter of 4 mm and the
height of 6 mm were cut from the NiTi bar by means of electrodischarge machining (EDM) and then were locally inserted into
the low carbon steel cans with the inner diameter of 4 mm, the wall
thickness of 3 mm and the height of 3 mm. The locally canned NiTi
samples were placed between the top anvil and the bottom one of
INSTRON-5500R universal testing machine and then were
compressed at the reduction in height by 75% at the strain rate of
0.05 s1 at room temperature. The compressed NiTi samples were
annealed for 2 h at 300
C, 450
C and 600
C, respectively, and
subsequently were cooled to room temperature at the atmosphere.
Microstructural evolution of NiTi samples subjected to SPD and
subsequent NiTi samples subjected to annealing was investigated
by means of transmission electron microscope (TEM). Foils for TEM
observation were mechanically ground to 70 mm and then thinned
by twin-jet polishing in an electrolyte consisting of 6% HClO4, 34%
C4H10O and 60% CH3OH by volume fraction. TEM observations were
conducted on a FEI TECNAI G2 F30 microscope with a side-entry
and double-tilt specimen stage with angular range of 40
at an
accelerating voltage of 300 kV.

345

In order to further understand the phase structures of NiTi

samples subjected to annealing, X-ray diffraction (XRD) was carried
out using a Philips XPert Pro diffractometer with CuKa radiation at
ambient temperature. The samples were scanned over 2q ranging
from 10
to 100
by continuous scanning with tube voltage of 40 kV
and tube current of 40 mA.
Differential scanning calorimeter (DSC) was used in order to
obtain the transformation temperatures of NiTi samples subjected
to annealing in the temperature range from 100
C to 100
C at
the heating and cooling rates of 10
C/min.
3. Results
3.1. NiTi sample subjected to SPD under local canning compression
Fig. 1 demonstrates the schematic diagram of deformation mode
of NiTi sample under local canning compression and the corresponding TEM photographs taken from the different deformation
zones of NiTi sample subjected to SPD. Fig. 1(a) shows the schematic diagram of deformation mode of NiTi sample subjected to
SPD based on local canning compression. It can be seen from
Fig. 1(a) that NiTi sample is caused to be in a three-dimensional
compressive stress state during plastic deformation. In order to
better understand deformation mechanism of NiTi sample under
local canning compression, the continuous deformation process
can be divided into two stages, namely intermediate deformation
degree by 50% and nal deformation degree by 75%. When NiTi
sample is subjected to reduction in height by 50%, it is completely
compressed into the steel can, which undergoes radial and

Fig. 1. Schematic diagram of deformation mode of NiTi sample under local canning compression and the corresponding TEM photographs taken from the different deformation
zones. (a) Schematic diagram of deformation mode showing NiTi sample subjected to SPD; (b) dark-eld image showing nanocrystalline phase embedded in the amorphous matrix;
(c) bright-eld image showing the presence of amorphous bands; and (d) bright-eld image showing the presence of deformation bands.

346

S. Jiang et al. / Intermetallics 32 (2013) 344e351

tangential elongation strain without axial compression strain. Both

NiTi sample and the steel can are subjected to radial and tangential
elongation strain as well as axial compression strain in the case of
reduction in height by 75%. Furthermore, the plastic deformation
zones of NiTi sample under local canning compression consist of
the principal deformation zone, the intermediate deformation zone
and the minimum deformation zone. It can be found that inhomogeneous plastic deformation leads to the different microstructural morphologies in NiTi sample subjected to SPD. TEM brighteld image of NiTi sample in the principal deformation zone is
indicative of the presence of an almost complete amorphous phase,
in which the retained nanocrystalline phase is embedded in the
amorphous matrix, as shown in Fig. 1(b). However, the amorphous
bands and the deformation bands occur in the plastic deformation
zones other than the principal deformation zone, as shown in
Fig. 1(c) and (d), respectively.
3.2. Nanocrystallization of amorphous NiTi sample subjected to
annealing

crystallized after annealing at 600
C for 2 h and is characterized by

the coarse grains rather than the nonacrystalline grains. In addition,
there exist plenty of annealing twins in the coarse-grained NiTi
sample. The corresponding selected area electron diffraction
patterns (SAEDPs) reveal that the annealing twins belong to (001)
martensite compound twins.
3.4. Microstructural evolution of amorphous bands after annealing
There exist a lot of amorphous bands in NiTi sample subjected to
SPD. Fig. 5 illustrates microstructural evolution of the amorphous
bands after annealing for 2 h at 300
C and 450
C, respectively. It
can be seen from Fig. 5 that a lot of nanocrystalline grains arise in
the amorphous bands of NiTi sample subjected to SPD. In terms of
annealing at 300
C, the dislocation defects remain between the
amorphous bands since thermal driving force is insufcient to
eliminate them. However, the amorphous bands in NiTi sample
after annealing at 600
C for 2 h is unable to be found.
3.5. Microstructural evolution of deformation bands after annealing

Figs. 2 and 3 demonstrate TEM photographs of NiTi samples

subjected to SPD after annealing for 2 h at 300
C and 450
C,
respectively. NiTi samples subjected to SPD before annealing
belong to an almost complete amorphous phase, in which a small
amount of nanocrystalline phase is embedded in the amorphous
matrix. It can be seen from Figs. 2 and 3 that annealing at 300
C
and 450
C for 2 h leads to nanocrystallization of amorphous NiTi
samples. Furthermore, the nanocrystalline grain size increases
with the increase in the annealing temperature. The size distribution of the nanocrystalline grains was measured by means of
extra TEM bright and dark images, in which the diameter of the
nanocrystalline grain in the selected area can be obtained by
combining DigitalMicrograph software with equal perimeter
method. The mean grain size in the diameter can be calculated
according to the selected 200 grains. In the case of annealing at
300
C, the mean grain size is about 12 nm in the diameter, but in
the case of annealing at 450
C, the mean grain size is about
50 nm in the diameter.
3.3. Twinning of amorphous NiTi samples subjected to annealing
Fig. 4 indicates microstructural morphologies of NiTi sample
subjected to SPD after annealing at 600
C for 2 h. It can be found
from Fig. 4 that NiTi sample subjected to SPD is completely

There exist a lot of deformation bands in NiTi sample subjected

to SPD due to inhomogeneous plastic deformation under local
canning compression. The deformation bands are attributed to
a consequence of dislocation slip. Fig. 6 indicates that the microstructures of the deformation bands in NiTi sample subjected to
SPD after annealing at 300
C and 450
C, respectively. It can be
seen from Fig. 6 that annealing at the two temperatures is unable to
lead to complete elimination of the deformation bands and a lot of
ne precipitation phases occur in the deformation bands after
annealing. Furthermore, as compared to annealing at 450
C, the
deformation bands of NiTi sample in the case of annealing at 300
C
are more apparent since thermal driving force is more insufcient.
However, the deformation bands in NiTi sample after annealing at
600
C for 2 h have been completely eliminated by means of
thermal driving force.
3.6. XRD curves of annealed NiTi samples
Fig. 7 indicates XRD curves of NiTi samples subjected to SPD
after annealing at 300
C, 450 and 600
C, respectively. NiTi
sample annealed at 300
C is mainly composed of B2 austenite
phase with a small amount of Ni4Ti3 precipitation phase. In the case
of annealing at 450
C, NiTi sample consists of B2 austenite phase,

Fig. 2. TEM photographs of NiTi sample subjected to SPD after annealing at 300
C. (a) Bright-eld image; and (b) dark-eld image.

S. Jiang et al. / Intermetallics 32 (2013) 344e351

347

Fig. 3. TEM photographs of NiTi sample subjected to SPD after annealing at 450
C. (a) Bright-eld image; and (b) dark-eld image.

B190 martensite phase, Ni4Ti3 precipitate and Ni3Ti precipitate. In

terms of annealing at 600
C, NiTi sample is made up of B2
austenite phase, B190 martensite phase and Ni3Ti precipitate, but
B190 martensite phase is dominant.

3.7. DSC curves of annealed NiTi samples

Fig. 8 indicates the DSC curves of NiTi samples subjected to SPD
after annealing at the different temperatures. The selected NiTi

Fig. 4. TEM photographs of NiTi sample subjected to SPD after annealing at 600
C. (a) Bright-eld image with ne twins; (b) SAEDP of (a); (c) bright-eld image with coarse twins;
and (d) SAEDP of (c).

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S. Jiang et al. / Intermetallics 32 (2013) 344e351

Fig. 5. TEM photographs of amorphous bands in NiTi samples subjected to SPD after annealing at different temperatures: (a) 300
C; and (b) 450
C.

samples for DSC test are located in the principal deformation zone
and thus are obtained by means of crystallization of the amorphous
NiTi phase. It can be found from Fig. 8 that NiTi sample annealed at
300
C shows no phase transformation, while NiTi samples
annealed at 450
C and 600
C exhibit martensitic phase transformation. Furthermore, as compared to as-received NiTi sample,
martensitic phase transformation temperatures are enhanced for
NiTi samples subjected to SPD as well as subsequent annealing.
4. Discussion
Inhomogeneous plastic deformation is unavoidable during SPD of
NiTi alloy under local canning compression at room temperature. An
almost complete amorphous matrix with a small amount of nanocrystalline phase occurs in the principal deformation zone of NiTi
sample. In the plastic deformation zones other than the principal
deformation zone, there exist a lot of deformation bands in which
there are plenty of crystal defects, such as dislocations, stacking
faults, and twins. At the low annealing temperatures of 300
C and
450
C, some crystal defects can be eliminated by means of static
recovery, but the deformation bands are unable to be removed
completely due to insufcient thermal driving force. In the case of
annealing at 600
C, the occurrence of static recrysallization leads to

complete elimination of the deformation bands. However, the

amorphous NiTi sample caused by SPD belongs to the metastable
phase and possesses the low thermal stability [16]. For example, the
fully amorphous NiTi sample after being subjected to high-pressure
torsion (HPT) exhibits partial nanocrystallization along with the
extremely small grains of 10e20 nm even at room temperature,
while the complete nanocrystallization with homogeneous nanocrystalline structure of 20e30 nm is performed in the case of
annealing at 200
C for 2 h [13]. In the present study, the complete
crystallization of the amorphous NiTi sample is obtained by
annealing for 2 h at 300
C, 450
C and 600
C, respectively, while
the grain size increases with the increase in the annealing temperature. In particular, the complete nanocrystallization is obtained in
the case of annealing at 300
C and 450
C, respectively. Physical
mechanism of crystallization with respect to the amorphous NiTi
sample obtained by SPD can be outlined as nucleation and growth of
the grains in the amorphous matrix, in which the retained nanocrystalline debris can rstly act as the heterogeneous nucleation sites
[16]. The nucleation rate and the growth rate during crystallization
play the critical roles in determining the nal grain size. In general,
the fast nucleation rate and the slow growth rate contribute to
obtaining the ne grains. In the present work, the annealing
temperature is considered as the only variable. Therefore, the grain

Fig. 6. TEM photographs of deformation bands in NiTi samples subjected to SPD after annealing at different temperatures: (a) 300
C; and (b) 450
C.

S. Jiang et al. / Intermetallics 32 (2013) 344e351

349

Fig. 7. XRD curves of NiTi samples subjected to SPD after annealing at different temperatures: (a) 300
C; (b) 450
C; and (c) 600
C.

size after crystallization depends on the growth rate of the grains,

while the elevated annealing temperature leads to increasing the
growth rate and thus results in the occurrence of the coarser grains.
As a result, in the case of annealing at 600
C, the faster growth rate
leads to rapid growth of the grains in a certain time, so the coarsegrained NiTi sample occurs.

Furthermore, annealing has an inuence on not only microstructural evolution, but also precipitation process of NiTi sample
subjected to SPD. It can be seen from XRD curves in Fig. 7 that
annealing at 300
C leads to only Ni4Ti3 precipitate and annealing at
600
C leads to only Ni3Ti precipitate, while Ni4Ti3 precipitate and
Ni3Ti precipitate coexist in the case of annealing at 450
C. It can be

Fig. 8. DSC curves of NiTi samples subjected to SPD after annealing at different temperatures: (a) 300
C; (b) 450
C; and (c) 600
C.

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S. Jiang et al. / Intermetallics 32 (2013) 344e351

found that SPD results in the occurrence of Ni3Ti precipitate at the

lower temperature and leads to the decrease of the highest
temperature at which Ni4Ti3 precipitate occurs. In general, there are
three precipitation phases including Ni4Ti3, Ni3Ti2 and Ni3Ti in Nirich NiTi SMA after annealing, which depends on annealing
temperature and annealing time. Ni4Ti3 phase occurs at the lower
annealing temperature and the shorter annealing time, and Ni3Ti
phase arises at the higher annealing temperature and the longer
annealing time, while Ni3Ti2 phase appears at intermediate
annealing temperature and time [1]. Therefore, both Ni4Ti3 and
Ni3Ti2 are the metastable phases, while Ni3Ti is the equilibrium
phase. In the present work, no Ni3Ti2 phase is found at the three
annealing temperatures. In addition, TEM observations reveal that
no precipitation phases are found in NiTi specimens derived from
crystallization of amorphous phase. Accordingly, the precipitation
phases occur in the deformation bands of NiTi sample after
annealing. The grain size seems to have a considerable effect on
nucleation and growth of Ni4Ti3 precipitate. For instance, Ni4Ti3
precipitate shall be suppressed in the nanocrystalline NiTi sample
obtained by crystallization of the amorphous phase after HPT [20].
Therefore, in the present study, annealing at 300
C and 450
C
leads to nanocrystallization of amorphous NiTi sample and consequently the precipitation phases shall be suppressed since the
nanocrystalline grains impede the formation of the selfaccommodation. However, no precipitation phases are found in
the coarse-grained NiTi sample formed as a result of crystallization
of the amorphous structure by means of annealing at 600
C, which
shall be further investigated in the future work.
It can be seen from the previous experimental results that the
grain size has a considerable inuence on martensitic phase
transformation of NiTi sample. Annealing at 300
C leads to the
nanocrystalline NiTi sample with the smallest mean grain size of
about 12 nm, where martensitic phase transformation is
completely suppressed. Annealing at 450
C results in further
increase of the grain size of the nanocrystalline NiTi sample, where
the mean grain size is about 50 nm, while the largest grain size is
about 90 nm. Therefore, in the nanocrystalline NiTi sample obtained in the case of annealing at 450
C, martensitic phase transformation takes place in the larger nanocrystalline grains, but is still
suppressed in the smaller nanocrystalline grains. However,
annealing at 600
C leads to the coarse-grained NiTi sample of
which the grain size is greater than 200 nm. Martensitic phase
transformation occurs more easily in the coarser grains. Accordingly, it can be concluded that martensitic phase transformation is
suppressed with the decrease in the nanocrystalline grain size.
Similar conclusions were reported in the nanocrystalline NiTi
sample derived from crystallization of the amorphous structure in
the case of HPT and subsequent annealing [16]. Suppression of
martensitic phase transformation in the nanocrystalline NiTi
sample is possible to be attributed to the presence of elastic strains,
lattice defects or crystal renement [7,16]. In the present study, the
elastic strains and the lattice defects shall be almost eliminated in
the nanocrystalline NiTi sample resulting from crystallization of the
amorphous phase in the case of annealing, so grain renement as
well as the corresponding constraint by the grain boundaries plays
an important role in suppressing martensitic phase transformation
based on self-accommodation of the martensitic variants. As
compared to the nanocrystalline NiTi sample, martensite is able to
nucleate at the dislocation tangles and near the grain boundaries in
the coarse-grained NiTi sample, which contributes to the occurrence of martensitic phase transformation.
Furthermore, the (001) compound twins are observed during
transformation of B2 austenite to B190 martensite in the coarsegrained NiTi sample formed as a consequence of annealing at
600
C. It is well known that f111g type I twin, h011i type II twin

and (001) compound twin are frequently found in martensitic

phase transformation of NiTi alloy in the case of heat treatment.
f111g type I twin and h011i type II twin comply with the
phenomenological crystallographic theory and thus belong to
a lattice invariant shear [21e23]. However, (001) compound twin
does not give a solution to the phenomenological crystallographic
theory and cannot be a lattice invariant shear, so it is recognized as
a deformation twin [24e26]. In the present study, the other two
twin modes except the (001) compound twin are not found. Only
(001) compound twins are observed in the nanocrystalline NiTi
sample formed as a result of crystallization of the amorphous
structure by HPT and subsequent annealing [16,17]. It is proposed
that in NiTi sample obtained by crystallization of the amorphous
phase, the (001) compound twin occurs more frequently instead of
f111g type I twin and h011i type II twin. The lattice distortion along
with the dislocation defects frequently occurs in NiTi sample with
the coarse grains derived from crystallization of the amorphous
phase and thus contributes to the occurrence of the (001)
martensite compound twins. In particular, the formation of the
twins should be more susceptible to taking place at the grain
boundaries.
5. Conclusions
(1) SPD of NiTi sample based on local canning compression leads to
the complicated microstructural morphologies, including
deformation bands, amorphous bands and amorphous phase in
which the retained nanocrystalline phase is embedded in the
amorphous matrix.
(2) Annealing at 300
C and 450
C leads to nanocrystallization of
amorphous NiTi sample, but is unable to result in complete
elimination of deformation bands and amorphous bands.
Annealing at 600
C results in complete crystallization of NiTi
sample subjected to SPD, where deformation bands and
amorphous bands are not able to be detected. The (001)
compound twins are found during transformation of B2
austenite to B190 martensite in the coarse-grained NiTi sample
formed as a consequence of annealing at 600
C.
(3) The precipitation phases are suppressed in NiTi sample formed
as a result of crystallization of amorphous structure in the case
of annealing at 300
C, 450
C and 600
C, respectively. The
precipitation phases occur more easily in the deformation
bands of NiTi sample after annealing. SPD results in the
occurrence of Ni3Ti precipitate at the lower temperature and
leads to the decrease of the highest temperature at which
Ni4Ti3 precipitate occurs.
(4) The grain size has a considerable inuence on martensitic
phase transformation of NiTi sample. Grain renement plays an
important role in suppressing martensitic phase transformation. Martensitic phase transformation is suppressed
with the decrease in the nanocrystalline grain size.
Acknowledgements
The work was nancially supported by National Natural Science
Foundation of China (No. 51071056) and the Fundamental Research
Funds for the Central Universities of China (No. HEUCFR1132 and
No. HEUCF121712).
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