ASME International Mechanical Engineering Congress and Exposition

November 13-19, 2015, Houston, Texas, USA

IMECE2015-51932

Microstructure and Mechanical Properties of Ni-Ti-Cu Shape Memory Alloys

Biomaterials .

M-sc.Dania Abbas
College of Engineering
AL-Mustansiriya university
Baghdad, Iraq
dandoon1992@yahoo.com
Asst prof. Kadhim K.Resan
College of Engineering
AL-Mustansiriya university
Baghdad, Iraq
kadkinani@gmail.com
Asst prof. Ayad Takhakh
College of Engineering
AL-Nahrain university
Baghdad, Iraq
ayadtakak@yahoo.com

ABSTRACT INTRODUCTION
In this study a Ni-Ti-Cu shape memory alloy was prepared by Shape Memory Alloys (SMAs) are metallic alloys that undergo a
powder metallurgy (PM) technique, various compacting pressure solid-to-solid phase transformation which can exhibit large
of (600, 700 and 800) MPa and sintering temperature of (850˚C, recoverable strains. [1] the shape memory alloys phenomenon
900˚C and 950˚C) were used, Shape Effect (strain recovery), was first observed in the 1930s, by Arne Olander while working
porosity , microhardness ,X-ray diffraction ,energy dispersion x- with an alloy of gold and cadmium.[2]
ray (EDX), scanning electron microscope (SEM) , and
SMA had phase changes while still a solid. these phase changes
differential scanning calorimeter )DSC) tests are conducted to
known as martensite and austenite, martensitic transformation is
estimate the effect of different compacting pressure and sintering
a diffusionless phase transformation in solids, in which atoms
temperature on the Ni-Ti-Cu shape memory alloy .The result
move cooperatively, and often by shear like mechanism .Usually
showed improvement in hardness and decreasing in porosity with
the austenite parent phase ( a high temperature phase) is cubic,
high compacting pressure and low sintering temperature with
and the martensite ( a lower temperature phase) has a lower
formation of the two main phases austenite and martensite.
symmetry[3].
key words: shape memory alloys , powder metallurgy , SEM test,
The most common shape memory alloy is the (nitinol) Shape
EDX test, DSC test , X- ray test.
memory alloys based on Ni and Ti, The discovery took place at
NOMENCLATURE NOL (the Naval Ordnance Laboratory) and hence the acronym
NiTi-NOL or Nitinol.[4]
As Austenite start temperature
Two separate mechanical effects Both the superelasticity and
Af Austenite finish temperature
shape-memory effects are induced in Nitinol,[5] The shape
DSC Differential scanning calorimeter memory effects refers to the phenomenon that shape memory
alloys return back to their predetermined shapes upon heating.
EDS Energy desperation X-ray The superelasticity refers to the phenomenon that SMAs can
PM Powder metallurgy undergo a large amount of inelastic deformations and recover
their shapes after unloading.[6]
SEM Scanning electron microscope
Nitinol shape memory alloys have provided new insights into
SMA Shape memory alloy biomedical area for orthopedic application such as load-bearings,
SMAs Shape memory alloys plates for bone fracture repair, spinal correctors, vertebral spacers
and bone distraction devices, cardiovascular application such as
XRD X-ray diffraction
heart valves, stents, vena cave filters. dental applications in the
correction of malocclusions .eyeglasses frame and can be used
for making advanced surgical instruments.
The biomedical success of these materials is due to their unusual
properties, which makes them superior to conventional materials.
[7].
among other applications, the possibility of using Nitinol as a
source of energy , prototypes of Nitinol engines, safety products ,
military and aerospace applications and many others.[2]
The aim of this work was to produce a Ni-Ti-Cu shape memory
alloys by powder metallurgy (PM) method and studying the
effect of different compacting pressure and sintering temperature
on it.

Figure 2. A press machine

EXPEREMENTAL WORK
Powder metallurgy was used for the preparation of the Ni-Ti-Cu
shape memory alloys ,the first step in this work was the
preparation of the powder which consist of 50% titanium 99.9% Vaccum gage
purity (-325 mesh) with 47% nickel 99.93 % purity (-325mesh)
and 3% copper 99.97% purity (-325 mesh) respectively was used
to prepare the samples. These powders were weighed Vaccum motors
accordingly and placed into cylindrical containers then mixed in
a horizontal barrel mixer as shown in “Fig. 1." , the speed of
rotating drum was set to 75 rpm and the time of mixing was 2 hrs
according to reference.[8]
after the mixing process the powder were compacted in a single
action tool steel mold to form a green cylindrical sample (11 Vaccum tube furnace
dia. Х 16.5mm length) and (11 dia. Х 5 mm length) .the
compacting operation was conducted in a press machine “Fig.
2." . at 600,700 and 800 MPa with a displacement rate of 1
mm/min and a holding time of 4 minutes, after compacting Figure 3.electrical tube furnace.
process samples had sufficient green strength for handling .
The green samples then sintered at 850,900 and 950 ºC for 7 hrs Alloy 50% Ti 47% Ni 3% Cu
in an electrical furnace supplied with a quartz tube and vacuum composition
equipment as shown in “Fig. 3." Compacting 600 700 800
Table (1) indicate the alloy composition with the compacting pressure (MPa)
pressure and the sintering temperature that where used.
Sintering 850 900 950
temperature
(˚C)

Table 1. SMAs chemical composition with compacting

pressure and sintering temperature.
The porosity was measured depending on the actual density and
the theoretical density of the samples [9]. “Eq. (1).”

Porosity % = [1-( )] x100 (1)

The actual density of sample is obtained from it's weight divided

by the volume of cylinder with 11mm diameter, while the
theoretical density equal 6.7 g/cm³ and obtained from “Eq. (2).”
Figure 1. Horizontal barrel mixer.
 (2)
= theoretical density of sample (g/cm3). , n= no. of elemental
powders.
Wt= weight percent (%)
1, 2,3,....n = density of elemental powder (g/ cm3).
Microhardness test has been conducted on the samples to
investigate the effect of the temperature and pressure on the
obtained value, more than three values of hardness for each
sample have been taken to get the mean value represents
hardness.
RESULT AND DISCUSION:
1. Porosity percentage decrease with increasing compacting
pressure since the adhesion and interdiffusion between the
particles is better which results in more elimination of pores.
Applying sintering temperature on the green sample table (2)
reduce the porosity. With further increasing of sintering
temperature the porosity increased slightly table (3) ,The reason
for this is due to that increasing of the sintering temperature
cause differences in shape and distribution of pores and the
average diameter of the pores increased ,In result of that, most of
the small pores were joined into large one forming their irregular
shapes. [11]

the microstructure and the alloying element distribution along the No. Pressure (MPa) Porosity (%)
structure was obtained using Scanning electron microscope 1 600 29.78
(SEM) and Energy dispersive X-ray spectroscopies (EDS) using 2 700 28.94
VEGA3/Tescan test device shown in. “Fig. 4." 3 800 28.77
The phases that formed by sintering process were detected using Table 2. Porosity measurement test result of green
the XRD for all the samples. samples.

DSC test was used to detect the phase transformation start and N Pressure Temperature Density Porosity
finish temperature using Linseis/STA PT-1000 device. o. (MPa) (˚C) (g/cm³) (%)
1 600 850 5.9453 11.26
2 600 900 5.8914 12.06
3 600 950 5.77 13.74
4 700 850 5.97 10.89
5 700 900 5.958 11.06
6 700 950 5.94 11.32
7 800 850 6.1532 8.16
8 800 900 6.122 8.62
9 800 950 6.0529 9.65
Table 3. Porosity measurement test result of sintered
Figure 4. SEM and EDS test device. samples.
shape memory effect test was applied on the ( 11mm dia. Х 16.5 2.Microhardness test result demonstrate an improvement in
mm length) sample by compacting the sample to 0.06% of its hardness with increasing of compacting pressure since high
normal length at a displacement rate of 1mm/min and then
heating to 110˚c for 5 min and left to cool in air then calculating pressure eliminate the pore and with decreasing of sintering
the shape effect (the return length) by applying “Eq. (3).” temperature , high sintering temperature increase the porosity.
“Fig. 5."
Shape memory effect = (2) [10]

Where :

L0: normal sample length

L1:sample length after 0.06% length compacted

L2 : sample length after heating 110°C for 5 min.

Figure 5. microhardness test result

3- SEM & EDS test :SEM test shows the microstructure of the
samples with the pore size change, it indicate that the porosity
decrease with increasing of compacting pressure and with lower
sintering temperature. “Fig. 6."
1-a 1-b
EDS shows the element distribution in all cases with their
percentage, the good distributed with concentration nearly
similar to the specified amount of mixture in the structures
indicate the successful mixing method and procedure. “Fig.
7."

1-a 1-b

1-c 2-a

1-c 2-a

2-c
2-b

2-b 2-c

3-a 3-b

3-a 3-b

3-c

3-c

Figure 6. SEM test result at (1-600MPa 2-700MPa 3- Figure 7. EDS test result at (1-600 MPa 2-700MPa 3- 800
800MPa) compacting pressure with (a- 850˚ C, b-900˚C, MPa) compacting pressure with (a- 850˚ C,b-900˚C, c-
c- 950˚C) sintering temperature. 950˚C) sintering temperature.
4. Shape memory effect test was done to determine the effect of
2-a
the temperature and pressure on the shape recovery of the
sintered sample, the result in table (4) below showed that the best
shape recovery was on the 850˚C sintering temperature and 800
MPa compacting pressure that's mean the shape recovery
improved with increasing compacting pressure and decreasing
sintering temperature since the porosity is less.
2-b
No. Pressure (MPa) Temperatur (˚C) Shape effect (%)

1 600 850 79.2

2 600 900 67
3 600 950 64 2-c

4 700 850 80
5 700 900 71.4
6 700 950 67
7 800 850 88.5
3-a
8 800 900 83.3
9 800 950 82

Table 4. Shape effect test result.

3-b
5.XRD was conducted to all sintered sample , the result showed
that NiTi alloys with different phase composition can be
achieved by controlling the sintering conditions time and
temperature . The samples consist of two main phases (austenite
and martensite ) in addition there is Ti2Ni andNi3Ti. The
formation of Ti2Ni and Ni3Ti might be attribute to the slow
cooling of the samples in furnace, there is also a small amount of 3-c
pure Ni and Ti that can be disappeared with raising sintering
temperature. “Fig. 8."

1-a

Figure 8. XRD test result at (1-600 MPa 2-700MPa 3- 800

MPa) compacting pressure with (a- 850˚ C,b-900˚C, c-
950˚C) sintering temperature.
1-b

6. DSC cooling/heating curves were registered at temperature

range between (-50˚C and +200˚C). All sintered alloys reveal the
presence of the reversible martensitic transformation .Thus, the
main condition for appearing of shape memory effect is satisfied.
“Fig. 9."
1-c
 in a shape-memory Nitinol alloy under biaxial loading,
Department of Materials Science and Engineering, University of
California, Berkeley,2003.

6- G. Songa, N. Maa, H.-N. Lib, Applications of shape memory

alloys in civil structures, 17 April 2006.

7- Marjan Bahraminasab and Barkawi Bin Sahari (2013). NiTi

Shape Memory Alloys, Promising Materials in Orthopedic
Applications, Shape Memory Alloys - Processing,
Characterization and Applications, Dr. Francisco Manuel Braz
Figure 9. DSC test result. Fernandes (Ed.), 2013

CONCLUSION 8-Hogg R. , " Mixing and Segregation in Powders , Evaluation ,

1. Hardness and porosity improved with increasing of
compacting pressure and decreasing of sintering temperature
due to elimination of pores.
2. SEM & EDS shows the good distribution of element and
decreasing porosity with increasing compacting pressure.
3. XRD test shows the formation of two main phases (austenite
and martensite) in Ni-Ti-Cu shape memory alloys.
4. shape effect test and DSC test results shows the presence of
shape recovery in the alloys.
ACKNOWLEDGEMENTS
Mechanisms and Processes ", Hosokawa Powder Technology
Foundation / KONA Powder and Particle Journal No.27-2009
9- J. T. Al-haidary & Shadi Al- Khatiab Academy of Sience, Vol.
42, February"Manufacturing and characterization of dental shape
memory alloy" materials Scienc and Engineering A 419, pp. (45-
49) (2006).
10- Jianfeng Wan, Xing Huang, Shipu Chen, T. Y. Hsu (Xu
Zuyao) , Effect of Nitrogen Addition on Shape Memory
Characteristics of Fe-Mn-Si-Cr Alloy, School of Materials
Science and Engineering, Shanghai Jiao Tong University Vol43,
No,5. Pp 920-925

The authors would like to acknowledge: (Al-Mustansiriya

University – material engineering dep. Labs), Baghdad –Iraq for 11- Tomasz Goryczka, Ni25Ti50Cu25 Shape Memory Alloy
the provision of facilities. Produced by Nonconventional Techniques, Shape Memory
Alloys: Processing, Characterization and Applications, Dr.
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