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Procedia Engineering 184 (2017) 334 – 343

Advances in Material & Processing Technologies Conference

Co-Powder Injection Moulding (Co-PIM) Processing of Titanium

Alloy (Ti-6Al-4V) and Hydroxyapatite (HA)
F. M. Salleha,b,*, A. B. Sulonga, N. Muhamada, I.F. Mohameda, N.N. Mas’ooda, B.E.
Ukwuezea,c
a
Department of Mechanical and Materials Engineering, Faculty of Engineering and Built Environment, Universiti Kebangsaan Malaysia, 43600,
Bangi, Selangor, Malaysia
b
Faculty of Mechanical Engineering, Universiti Teknologi MARA, UiTM, 40450 Shah Alam, Selangor, Malaysia.
c
Department of Mechanical and Production Engineering, Institute of Management and Technology, P.M.B 01079, Enugu, Nigeria

Abstract

Co-powder injection moulding (Co-PIM) is a metal/ceramic injection moulding that offers co-injection of two materials, which
effectively reduces the cost and surface engineered component’s development. However, co-injection of metal and ceramics is
still lacking due to the limitation of different material properties. The purpose of this study was to investigate a co-injection of Ti-
6Al-4V and HA experimentally. Three different solid loadings (68, 69, and 70 vol%) of Ti-6Al-4V feedstocks were co-injected
with 56 vol% of HA. The binder composition added was 60 vol% polyethylene (PE) and 40 vol % palm stearin (PS). The Co-
PIM green part of Ti-6Al-4V and HA diffused well at injection processing parameters of injection melting temperature 150°C,
mould temperature 90°C, injection pressure 10 bars, and holding time 10s, respectively. The result shows that the bonding
strength increased proportionally to the increasing volume of Ti-6Al-4V. The 70 vol% Ti-6Al-4V/56 vol% HA shows the highest
density and bonding strength of 2.72 g/cm3 and 2.27 MPa was approximately achieved. In addition, the binder systems improved
the bonding mechanism of the green part without cracks appeared at the bonding of two materials.

©©2017
2017TheTheAuthors.
Authors. Published
Published by Elsevier
by Elsevier Ltd.is an open access article under the CC BY-NC-ND license
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(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of the organizing committee of the Advances in Material & Processing Technologies
Peer review under responsibility of the organizing committee of the Advances in Materials & Processing Technologies Conference
Conference.

Keywords: Co-Powder Injection Moulding, Co-Injection, Titanium Alloy, Hydroxyapatite, Polyethylene, Palm stearin

1877-7058 © 2017 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer review under responsibility of the organizing committee of the Advances in Materials & Processing Technologies Conference
doi:10.1016/j.proeng.2017.04.103
 F.M. Salleh et al. / Procedia Engineering 184 (2017) 334 – 343 335

1. Introduction

Artificial organ and implant are widely used for biomedical applications especially for orthopedic implantation.
This artificial organ is supposed to have similar properties to the natural organ such as natural bone. Hydroxyapatite
CaI0(PO4)6(OH)2 is an inorganic component which is chemically and crystallographically identical to the natural
bone. It contains bioactive materials that allow new bones to grow from the natural bone into the implant [1].
However, Hydroxyapatite (HA) has poor mechanical properties and unsuitable for high load applications. Due to
that, it requires an additional substance to improve the mechanical properties. Titanium and its alloys are the most
favourite materials due to its strong mechanical properties and high chemical resistance. Ti-6Al-4V has a higher
Young’s modulus compared to human bones and this will lead to stress shielding[2]. Therefore, the combination of
Ti-6Al-4V and HA is able to form a biomaterial with good biological and mechanical property as well as good
corrosion resistance[3].
Several techniques in Powder Metallurgy have been used to produce the implant parts. There are several types of
powder processing techniques; powder compaction (hot isostatic and cold isostatic pressing), plasma spraying, and
powder injection moulding. Fabrication of bionic design structure ZrB2–SiC/BN uses tape casting and hot
pressed[4]. As an alternative to the orthopedics implant fixation, plasma sprayed has been utilised using HA coating
on Ti-6Al-4V. It was shown that the new bone was properly aligned onto the HA coatings, resulting in a very good
adhesion between HA and the new bone [5], [6] . For powder injection moulding (PIM), Ti-6Al-4V/HA composite
were investigated its mechanical and physical properties [3] [7]. Both authors found that the good biocompatibility
existed between those two materials even with different binder systems. The Co-PIM was introduced in the work
[8]. The fabricated zirconia-stainless steel and advanced analytical techniques were utilised to explore the interface
formation mechanism of nanocrystalline zirconia/430L stainless steel composite layers. As a far as author is
concerned none of Ti-6Al-4V/HA layer has been studied. This motivates the author to investigate the bonding
mechanism of both materials using Co-PIM processing.
Co-PIM is based on PIM method. PIM engages mixing stages of either metal or ceramic powder with binder
to produce a feedstock. During injection moulding stages, the feedstock flows into the mold cavities under pressure
to form a green part. The green part is then de-bound and sintered to form the final part [9]. In injection moulding
stage the Co-PIM used the co-injection method. This method employs two methods of injection moulding known as
sequential moulding and simultaneous moulding. The sequencing injection moulding started with the first feedstock
was injected into the mould. Then, second feedstock will overmould the first injected part. Meanwhile, simultaneous
injection moulding used two single barrels whereas the first and second feedstocks were injected simultaneously [10
-12].
The binders were significantly important in powder injection moulding. The binders have two main roles that
provide feedstock fluidity and strength in holding powder particle together until the sintering process. Several
studies investigating palm stearin (PS) binder have been carried on its capability to provide capillary route for an
ease of processing and shape retention[13], the contamination effects of PS to the part [14], and feasibility of PS
binder to produce Ti-6Al-4V/HA composite part [7]. Surveys reported the good relationship of PS and Polyethylene
(PE) as a binder system in producing PIM part; Ti-6Al-4V/HA[7], Ti-6Al-4V [15-17], 316L stainless steel[18].
However, in Co-PIM generally the bonding two components materials constitute particular technical challenges
to the researcher. The selection of polymer binders for holding and retaining the green part after injection moulding
is a critical stage. The good green part will proceed to the debinding and sintering stage. The aim of this research is
to investigate the green part mechanical and physical properties and establish the co-injection frameworks of Ti-
6Al-4V/HA layer.

2. Experimental procedure

Ti-6Al-4V and HA powders from Sigma Aldrich with pycnometer density of 4.4583 g/cm3 and 3.3008 g/cm3
were used. The average particle sizes of Ti-6Al-4V and HA were 19.6 μm and 5.31 μm respectively. The XRD
analyses for powders were performed using diffractometer with a radiation over a 2-theta range from 10-90 degrees
as shown in Fig. 1. The DSC test for binders system is according to ASTM D3418 (Standard Test Method for
Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential Scanning
336 F.M. Salleh et al. / Procedia Engineering 184 (2017) 334 – 343

Calorimetric). The tests were carried out to obtain the melting temperatures for binders to determine the mixing
temperatures as well as the solvent debinding temperature. The TGA test was conducted according to ASTM E1131
(Standard Test Method for Compositional Analysis by Thermogravimetry). A heating rate of 10 oC/min was used in
both tests. Palm stearin and polyethylene melting temperatures were 53.97 oC and 124.75oC. The decomposition
range temperatures were 296.3 to 459 oC.1 and 406.4 to 496.3 oC respectively. The data were retrospectively
reported from previous research work by Arifin et. al [19]

(a) (b)

Fig. 1. XRD result (a) HA (b) Ti-6Al-4V

Two feedstocks were prepared based on Critical Powder Volume Percentage (CPVP). The powder CPVP was
measured using the oil absorption technique based on ASTM: D-281-12. The CPVP for both Ti-6Al-4V and HA
was 72 vol% and 59 vol% respectively. The feedstocks were prepared based on a range of 2-5% from critical
powder loading reported by German and Bose[20]. The Ti-6Al-4V and HA feedstock each 100 wt% was prepared.
The composition of binder system with 60 wt% polyethylene and 40 wt% palm stearin was used. The powders were
mixed with the binder for 2 hours using a bra-bender mixer at 150oC with constant speed of 25 rpm. Conversely, the
rheological test was conducted using a Shimadzu CFT- 500D at various temperatures of 130 oC,140 oC,150 oC, and
160 oC to analyse the flow behaviour of Ti-6Al-4V feedstocks. Meanwhile, the rheological of HA feedstock was
tested using RH Rosand 2000 capillary rheometer at temperature ranges of 150 oC,160 oC, 170 oC, and 180 oC with
the capillary die of 1mm diameter and length of 10mm (L/D=10).
The sequence co-injection mechanism was performed using an injection molding machine (DSM Xplore
Injection Molding). The injection process parameters were run at melt temperature, mold temperature, injection
pressure, and holding pressure set at 150 oC, 90 oC, and 10 bars and 10 s, respectively. The density of the green parts
was measured by using the Archimedes method with distilled water as a medium (Mettler Toledo MS204S). The
Scanning electron microscopy (SEM) was used to study the surface morphology. The mechanical properties of Ti-
6Al-4V and HA green parts bonding were measured using INSTRON 5567 with 1kN load, an Instron universal test
machine based on MPIF standard 41.

3. Result and discussion

3.1. Feedstock Preparation

The preparation of feedstock was performed through mixing powders and binders using a bra-bender mixer
machine. The mixing temperature was kept above the melting point to assist binder melt completely and to prevent
binder decomposed. The mixing process started with melting PE before adding the Ti-6Al-4V powder and PS
progressively. The same step was followed to prepare HA feedstock. Three different types of powder loading of 70
vol%, 69vol%, and 68 vol% of Ti-6Al-4V feedstock and 56 vol% of HA feedstock with weight percentage are
tabulated in Table 1. The HA powder loading was in the ceramic range of 50-55 vol% as reported by German and
Bose[20]. The previous finding reported that the powder loading for spray dried HA powder is 40 vol% [21], 20-40
vol%, for non-calcined powder and 61.2-68.6 vol% calcined powder [22]. The homogeneity of feedstock is
 F.M. Salleh et al. / Procedia Engineering 184 (2017) 334 – 343 337

confirmed when the torque graph shows a steady torque level during the mixing process. Fig.2 indicates the graph of
mixing torque for those feedstocks. It shows that, torque was achieved at a higher level at first 60 minutes before the
feedstock went through with steady torque. This findings further support the previous method to evaluate the
feedstock homogeneity [23].

Table 1. Ti-6Al-4V and HA feedstock with binder composition

Powder Powders Binders

Feedstock
Loading (Vol%) (wt%) (wt%)
TI68PL 68 91.3 8.7
TI69PL 69 91.7 8.3
TI70PL 70 92.0 8.0
HA56PL 56 82.31 17.69

8
7
6
5 69vol % 70 vol%
Torque (Nm)

4
3
2
1 68 vol %
0
24.7 65.6 90.6 115.6 133.1
Time (min)
(a)

144
132
120
108
Torque [Nm]

96
84
72
60
48
36
24
12
0
0 48 96
Time (min)
(b)

Fig. 2. Mixing Torque (a) 68vol%, 69 vol%, 70 vol% Ti-6Al-4V (b) 56 vol% HA

Fig. 3 indicates the morphology of feedstocks consisting of PS and PE. It shows the binder having homogeneous
dispersion around the powder particles. The first backbone polymer PE was used to hold the green part and generate
wetting for the feedstock to ease moulding and shaping. The second backbone PS is used to act as a soft polymer
that can provide the moisture to the feedstock. The PS helps to generate capillary route to the feedstock for the next
debinding process. Fig.3(a), 3(b), and 3(c) clearly shows the structure of PE and PS polymer surrounding the Ti-
338 F.M. Salleh et al. / Procedia Engineering 184 (2017) 334 – 343

6Al-4V particle. However, Fig 3(d) polymers structure cannot be seen clearly due to HA flake shapes. The HA
particles tend to penetrate themselves with the help of PE and PS binders .

(a) (b)

10μm
m 10μm
m

(c) (d)

10μm
μm 10μm
μm

Fig. 3. SEM Morphology of feedstocks (a) 68 vol% Ti-6Al-4V (b) 69 vol% Ti-6Al-4V (c) 70 vol% Ti-6Al-4V (d) 56 vol% HA

3.2. Rheological behavior of feedstock

The rheological characteristic is desirable in an injection process when powder-binder mixture is injected into a
die cavity. In PIM, the shear rate generally varies from 10 2 to 105 s-1. The viscosity lower than 1000 Pa.s is required
to ensure the feedstock flows to the mold cavity at elevated temperature [24]. Moreover, the feedstock properties
need to be investigated its flow behaviour and flow activation energy with elevated temperature as stated in the
experimental procedure. The behaviour of feedstock is calculated according to the following power law Eq. (1).
η = Kγn-1 (1)
where η and K is the flow behaviour indexes for viscosity and constant. The feedstock with pseudoplastic behaviour
has n value less than 1, whereas the feedstock with n = 1 is called Newtonian. Fig.4 shows the correlation between
viscosity and shear rate graph for Ti-6Al-4V and HA feedstock derived from the Eq. (1). The viscosity decreasing
at higher shear rate due to shear thinning existed, where as it called pseudoplastic behaviour. Fig 4 (a), (b), (c)
indicates that Ti-6Al-4V feedstock viscosity and shear rate are in the range of 84.2 to 603.3 Pa.s and 124.2-2039 s-1,
respectively. The power law is an exponent n ranging from 0.56 to 0.856 at temperature range of 130 oC-150 oC.
Although HA feedstock viscosity is 10 to 1200, Pa.s slightly higher than standard value 1000 Pa. s. The 50 – 5000 s-
1
was still in the shear rate range n value is range of 0.18- 0.22. For both Ti-6Al-4V and HA feedstocks shows n is
below than 1 represents pseudoplastic behaviour. The lower the value of n means that there is more viscosity
dependence to the shear rate [25].
 F.M. Salleh et al. / Procedia Engineering 184 (2017) 334 – 343 339

400
200
130 130
140
150 140
150 160 300 150
160

Viscosity (Pa.s)
Viscosity (Pa.s)

100 200

50 100

0 0
0 500 1000 1500 2000 0 500 1000 1500 2000
shear rate (1/s)
shear rate (1/s)
(a) (b)

1300
700 1200 150
130 160
1100
600 140
1000 170
150
500 160 900 180
Viscosity (Pa.s)
Viscosity (Pa.s)

800
400 700
600
300
500
200 400
300
100 200
100
0 0
0 500 1000 1500 2000 0 500 1000 1500 2000 2500 3000 3500 4000 4500
shear rate (1/s) shear rate (1/s)
(c) (d)

Fig. 4. Correlation between viscosity and shear rate of feedstocks (a) 68 vol% Ti-6Al-4V (b) 69 vol% Ti-6Al-4V (c) 70 vol% Ti-6Al-4V (d) 50
vol% HA

The flow activation energy describes the influence of temperature on the feedstock viscosity. Based on Arrhenius
equation, the activation energy, E kJ/mol can be determined for each feedstock powder loading [26]. For Ti-6Al-4V
feedstocks, 68 vol%, 69 vol%, and 70 vol% of powder loading produced result E value 10 kJ/mol, 16.92 k/Jmol and
32.58 k/J mol, respectively. The result indicates that the lower powder loading the lowest E value can be
determined. The E values represent the sensitivity of feedstock where lower value is preferred in PIM since it
reduces the stress concentration that results in preventing any cracks or distortion of green part to occur [26]. The
activation energy of 56 vol% of HA powder loading is 5.36 k/J mol.
340 F.M. Salleh et al. / Procedia Engineering 184 (2017) 334 – 343

3.3. Co-Powder Injection Moulding

The co-injection in sequence mechanism process was performed using injection molding machine (DSM Xplore
Injection Molding) as shown in Fig. 5. Such process begins by injecting Ti-6Al-4V feedstock into the mould. The
green part of Ti-6Al-4V was removed and cut to half before replaced into the mould cavity. Then, the HA is injected
to overmould Ti-6Al-4V so that they will be bonded together. The injection process parameters were run at melt
temperature, mold temperature, and injection pressure and the holding time was set at 150 oC, 90 oC, 10 bars, and 10
s respectively. This method was successful for both feedstocks bonded as a co-injected part of Ti-6Al-4V /HA
material, as the binder system helps in strengthening the green part.

(i) (ii) (iii)

Fig. 5. (a) Co-injection of Ti-6Al-4V/HA (i) Ti-6Al-4V is injected into the mould (ii) HA overmould half of Ti-6Al-4V part (ii) co-injected part.

Fig. 5. (b) DSM Xplore Injection Molding Fig. 5. (c) Co-injected Ti/HA green part

3.4. Morphology of co-Injected of green part

Fig. 6. (a), (b) and (c) shows the morphology of the Ti-6Al-4V /HA green part consisting of PE and PS binder
looked denser and the wetting of the bonding interface appeared more significant. It can be observed that no gap or
crack happened at the interface. Good behaviour of bonding for all powder loading of Ti-6Al-4V feedstock was
observed, which means Co-PIM green parts were produced. Such finding provides a new knowledge in Co-PIM.
 F.M. Salleh et al. / Procedia Engineering 184 (2017) 334 – 343 341

(a) (b)

50µm 50µm

(c)

50µm

Fig. 6. SEM micrographs for Co-injected green part of Ti-6Al-4V /HA (a) 70Vol % Ti/56 vol% HA, (b) 69 vol % Ti/56 vol% HA (c) 68 vol %
Ti/56 vol% HA

Table 2 shows the Ti-6Al-4V /HA green part density with increasing powder loading of Ti-6Al-4V feedstock and
HA powder loading is remained constant. It shows that as the powder loading increases the density for Ti-6Al-4V is
also increased. The same trend was observed for co-injected Ti-6Al-4V/HA green part. The higher powder loading
will reduce the space between the particles and affect the part more dense after the sintering process. Hence, the
high powder loading is the most preferable due to high amount of powder content.

Table 2. Density for Ti-6Al-4V/ HA co-injected part

Theoretical Ti-6Al-
HA Theoretical Ti-6Al-4V
density 4V/ HA
No.item density density HA No item density No.item
Ti-6Al-4V density
(g/cm3) (g/cm3) (g/cm3)
(g/cm3) (g/cm3)
2.11 68PL 3.27 3.32 6856PL 2.7
56PL 2.11 2.24 69PL 3.28 3.36 6956PL 2.71
2.11 70PL 3.32 3.39 7056PL 2.72

3.5. Three-point bending test of green part

The flexural test was conducted to evaluate the bending strength of the green part. For Ti-6Al-4V /HA green part,
the bonding strength was important to ensure no breakage before the next debinding process. Fig. 7 displays clearly
the 7056PL which has higher bonding strength with 2.279 MPa. This is because of the stiffness is dependent on its
density. The high volume of powder loading for both Ti-6Al-4V and HA feedstock provides resistance deformation.
It can be observed with decreasing powder loading of Ti-6Al-4V proportionally decreased the bonding strength
parts. The addition of binder, especially 60 vol% of PE polymer, provides the strength for the different materials to
be attached together.
342 F.M. Salleh et al. / Procedia Engineering 184 (2017) 334 – 343

16

12.015 12.015 12.015

12 HA
Flexural stress (MPa)

4.089 4.360 4.452 Ti-6Al-4V

4
2.279 Ti-6Al-4V/HA
1.604 1.696

6856PL 6956PL 7056PL

0
1 2 3

Fig. 7. Flexural stress of HA, Ti-6Al-4V and Ti-6Al-4V /HA green part

4. Conclusion

The Ti-6Al-4V /HA co-injected green part was successfully developed through sequential injection method. The
co-injected green part was diffused well with binder support of 60 vol% PE and 40 vol% PS. The 70 vol% /56 vol%
HA presents highest density and bonding strength of 2.72 g/cm3 and 2.279 MPa, correspondingly. The feedstock of
69 vol% and 68 vol% Ti-6Al-4V with fixed HA powder loading shows bonding strength decreased slightly at
1.696MPa and 1.604MPa, respectively. The co-injected part 70 vol% Ti-6Al-4V /56 vol% HA is selected for the
next debinding and sintering processing stage.

Acknowledgements

The authors would like to appreciate Universiti Kebangsaan Malaysia (National University of Malaysia) for
financial support under Grant No. ICONIC-2013-003.

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