International Journal of Lightweight Materials and Manufacture 1 (2018) 215e218

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International Journal of Lightweight Materials and Manufacture

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Original Article

Effect of NiTi content and test temperature on mechanical behaviors of

NiTiePU composites
Xingke Zhao*, Tao Chen, Shufan Wang
School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, PR China

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

Article history: For purpose of developing damping materials with increased damping capacity over a wide band, NiTi
Received 21 June 2018 ePU composites were fabricated by vacuum molding polyether polyurethane melt with NiTi alloy
Received in revised form chips additive. The composites were tested using three-point bending at various testing temperatures.
14 September 2018
Appreciable improvements were observed in bending modulus and load-deflection hysteresis loops of
Accepted 17 September 2018
Available online 27 September 2018
PU matrix. The bending modulus and hysteresis loop area of a composite with 70% NiTi volume content
reach a maximum, which are 5.4 times and 5.6 times higher than those of PU matrix, respectively. The
mechanism of bending modulus enhancement of NiTi additive was discussed.
Keywords:
Nitinol
© 2018 The Authors. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd.
Polyurethane This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
Composites nc-nd/4.0/).
Bending modulus
Hysteresis loop

1. Introduction there are many reports on NiTi-reinforced composites [6e8], but, to

Polyurethane (PU) elastomers have a very high damping ca-
pacity owning to their energy dissipation caused by viscoelastic
deformation. However, the Young's modulus and strength of PU
elastomers make it difficult to find applications in variety of in-
dustries, such as automobile and aviation industries. Besides, PU
elastomers can appear high damping capacities only for a high
frequency vibration and in a narrow range of temperature. Many
studies have been conducted on improving the damping capacity
and mechanical properties via segments modification as well as
fillings composite [1e3]. NiTi shape memory alloy shows is an
excellent damping capacity to high frequency vibration since a
large number of movable interfaces of austenite-martensite
boundaries and inter-martensite variant boundaries [4]. In addi-
tion, NiTi alloy has many other advantages, such as large recover-
able deformation, anti-fatigue, wear-resisting, good mechanical
properties. Considering the advantages and disadvantages of these
two damping materials, NiTiePU composite might have high
strength, Young's modulus and high damping capacity in a wide
temperature range and wide vibration frequency [5]. Although
* Corresponding author.
E-mail address: zhaoxingke@yahoo.com (X. Zhao).
Peer review under responsibility of Editorial Board of International Journal of
Lightweight Materials and Manufacture.
the best of our knowledge, mechanical behavior of NiTiePU com-
posites prepared by vacuum molding PU melt with NiTi alloy chips
additive is firstly studied in this present paper.
2. Experimental procedures
NiTi alloy used in this study was 30 mm in diameter hot-rolled
rod (XI'AN SaiTe Metal Materials Development Co., Ltd, China) with
a chemical composition of Ni-49.4Ti (at.%). The NiTi bar was
machined into chips, as shown in Fig. 1a. The NiTi alloy chips was
then degreased and washed followed by annealed at 500
C for
30 min in a vacuum furnace. The phase transformation temperature
of the as-treated NiTi chips were determined using a TA 2920 dif-
ferential scanning calorimetric (DSC) set with a heating -cooling
rate of 3 K min1. The characteristic phase transformation tem-
peratures are indicted in Fig. 1b. Both the Ms (the start temperature
of martensite phase transformation) and Af (the finish temperature
of martensite phase transformation) are near room temperature.
Polyurethane (PU) used in this study was Polyether poly-
urethane bar (Shenyang Xinyang Polyurethane Science and Tech-
nology Co. Ltd, China). The PU particles were weighted, and then
melted in a stainless steel crucible at 200
C. The NiTi chips were
added into the PU melt, and stirred for 10 min with an electric
mixer. The content of NiTi chips in mixed melt was selected as 0%,
10%, 40%, 70%, 85%, 87.5%, 90% or 92.5% in volume fraction. The

https://doi.org/10.1016/j.ijlmm.2018.09.003
2588-8404/© 2018 The Authors. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
216 X. Zhao et al. / International Journal of Lightweight Materials and Manufacture 1 (2018) 215e218
Fig. 1. NiTi chips (a) and DSC curves (b).
mixed melt were filled into a stainless steel mold, cooling to room
temperature in the mold which were placed in a vacuum chamber.
The size of NiTiePU composite samples is 2.5 mm  7 mm 
24 mm.
The morphology of NiTiePU composite samples was observed
using an optical microscope (4XC-II). Three-point bending test was
carried out using an universal material testing machine (HDW-10,
Ji'nan Heng Xu Test Machine Technology Co., Ltd., China) for the
characterizing the stress-strain hysteresis properties of NiTiePU
composites. The bending specimen was loaded under a rate of
0.1 mm-s to a maximum deflection value of 3 mm and then
unloaded back to zero stress at the same rate. The load-deflection
(stressestrain) curve was recorded automatically during loading
and unloading cycle, as illustrated in Fig. 2. The bending test was
conducted at 0
C, 25
C and 50
C, separately. Considering the two
facts, one is that the NiTi chips are at a single martensite phase and
a dual-phase of martensite-austenite when at a temperature below
26
C and above 26
C (according to Fig. 1b), and the other is that
most engineering applications of damping devices are near room
temperature. Damping property of NiTiePU composites is deter-
mined by calculating the area of load-deflection hysteresis loop.
3. Results and discussions
3.1. Macroscopic morphology
Pure PU specimen is light yellow transparent at room temper-
ature, as shown in Fig. 3. With the amount of NiTi chips increasing
in the PU matrix, the color gets darker and thicker. Pure PU spec-
imen is so dense that no voids can be found on surface or inside. It
Fig. 2. Schematic diagram of three-point bending (a) and hysteresis loop (b).
indicates that the gas involved during PU melt stirring process can
be removed when PU melt solidifies in vacuum. The roughness of
NiTiePU composite increases with the amount of NiTi chips
increasing due to NiTi chips sticking out the surface. When the
amount of NiTi chips is much higher than that of PU, voids formed
on surface or even inside of NiTiePU composite, because PU is not
enough to fill the spaces between irregular NiTi chips. Fig. 4 shows a
surface void between two edges of NiTi chips in a 92%NiTiePU
composite. As the voids formation in the NiTiePU composite results
from the less PU amount, the porosity of the composite increases
with NiTi chips additive increasing.
3.2. Load e deflection curves
Fig. 5 shows the load-displacement curve obtained from the
25
C bending test of NiTiePU composite specimen. All the
specimens can recover to their initial shape after a loading-
unloading cycle. However, there is obviously delay between
unloading process and shape recovery process, resulting in an
obvious bending load-deflection hysteresis loop. It is worth
noting that the bending modulus of composite specimens does
not always increase with increasing NiTi additive, but the
maximum value of bending modulus appears in the 70%NiTiePU
composite specimen.
The bending load-deflection curves obtained at temperatures of
0
C or 50
C are similar to that at 25
C. At all the three bending
temperatures, the maximum bending modulus appears in the 70%
NiTiePU composite specimen. One can find from Fig. 6 that the
bending modulus of the composite decreases with the increase of
the bending temperature. For the same bending deflection (3 mm),
 X. Zhao et al. / International Journal of Lightweight Materials and Manufacture 1 (2018) 215e218 217

Fig. 3. Macroscopic morphology of NiTiePU composite with various NiTi chips content.

Fig. 4. Voids formed on surface of a 90%NiTiePU specimen.

Fig. 6. Load e deflection curves of 70%NiTiePU Composites bending at various

temperatures.

Fig. 5. Load e deflection curves of NiTiePU composites bended at 25
C. Fig. 7. Bending modulus of NiTiePU composites as function of NiTi content.

the larger the bending modulus, the larger the bending load rea-
ches and the larger area of the hysteresis loop forms.
Fig. 7 shows the effect of NiTi chips content and bending tem-
perature on the bending modulus of the NiTiePU composite. At a
given bending temperature, the bending modulus increases with
increasing NiTi content, and reaches its maximum when NiTi
content is 70%. Then the bending modulus value drops rapidly
when increasing NiTi content furtherly. For a given NiTi chips
content, the bending modulus of NiTiePU composite decreases
with increasing test temperature. The bending modulus of 70%
NiTiePU is 5.4 times higher than that of PU matrix bending at 0
C.
218 X. Zhao et al. / International Journal of Lightweight Materials and Manufacture 1 (2018) 215e218
Fig. 8. Area of hysteresis loop as function of NiTi content.
3.3. Areas of hysteresis loops
The area of hysteresis loops for various composites at different
temperatures are shown in Fig. 8. The effects of NiTi chips content
and bending temperature on the area of hysteresis loops are just
similar to that on bending modulus of the NiTiePU composite. With
increasing NiTi chips content, the area of hysteresis loop first in-
creases and then decreases. When the NiTi content is 70%, the
hysteresis loop area reaches its maximum value. Similarly, the
hysteresis loop area of 70%NiTiePU is 5.6 times higher than that of
PU matrix when bending at 0
C.
The reason that peak values of both bending modulus and
hysteresis loop area are in the 70%NiTiePU composite specimen
can be explained with two factors of NiTi additive reinforcement
and voids weakness to the composite. Bending modulus of NiTiePU
composites can be described simply as follows.
E ¼ xEm þ ð1  xÞ EP þ Ei ðxÞ
where, x is NiTi volume percentage in the composite; Em and Ep are
bending modulus of NiTi and PU, respectively; Ei represents the
contribution of the interfacial bonding of NiTiePU to the bending
modulus of the composite. Ei(x) is related to NiTi reinforcement and
void weakness as mentioned above.
With x increasing, the increase in the first and third terms in
Formula 1 is greater than the reduction in second term, since Em is
generally higher than Ep at a given temperature. However, when x
exceeds 70%, voids form at the boundary of NiTi chips and PU,
resulting to the decrease of Ei(x). With increasing x further, the
increase in the first item is smaller than the reduction in the other
two terms, leading to the decrease of E in Formula 1.
It should be note that Em relies on phase constitution of NiTi
chips. From Fig. 1b one know that NiTi chip is in a single martensite
phase when temperature is below 26
C, and in a dual-phase of
martensite and austenite when temperature is in range of
26e54
C. As well known, NiTi alloys show a lower modulus in their
dual-phase state than in a single martensite state. Therefore, for a
given NiTi chips content, the bending modulus of NiTiePU com-
posite sample is higher when tested at 0
C than tested at 25
C or
50
C. In addition, the NiTi alloy machine processing chips is
irregular, the thickness and the curvature are very different, so Em is
not constant, even temperature is fixed.
4. Conclusions
NiTiePU composites samples have been fabricated by vacuum
molding polyether polyurethane melt with NiTi chips additive.
Voids formed on surface or even inside of NiTiePU composite as
NiTi chips additive exceeds 70%. Both bending modulus and the
area of load-deflection hysteresis loops increases firstly and then
decreases with NiTi volume content, and reaches their maximum in
the 70%NiTiePU composite specimen, which are 5.4 times and 5.6
times higher than those of PU matrix, respectively. For a given NiTi
chips content, the bending modulus and the area of load-deflection
hysteresis loops of NiTiePU composite decreases with increasing
test temperature from 0
C to 50
C.
Acknowledgements
The work was supported by the Fundamental Research Funds
for the Central Universities [FRF-IC-15-005]; and the International
Research Staff Exchange Scheme of Marie Curie Action in Seventh
Framework Programme of the European Commission [PIRSES GA-
2013-612585].
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