Defence Technology 14 (2018) 408e411

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Defence Technology
journal homepage: www.elsevier.com/locate/dt

Characterization of ceramic reinforced titanium matrix composites

fabricated by spark plasma sintering for anti-ballistic applications
S.W. Maseko a, *, A.P.I. Popoola a, O.S.I. Fayomi a, b
a
Department of Chemical, Metallurgical, and Materials Engineering, Tshwane University of Technology, Pretoria, South Africa
b
Department of Mechanical Engineering, Covenant University, Ota, Nigeria

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

Article history: Titanium has found extensive use in various engineering applications due to its attractive physical,
Received 16 March 2018 mechanical, and chemical characteristics. However, titanium has relatively low hardness for use as an
Received in revised form armour material. ZrB2 was incorporated to the Ti matrix to form a Ti-based binary composites. In this
26 April 2018
study, powder metallurgy techniques were employed to disperse the ceramic particulates throughout
Accepted 28 April 2018
Available online 30 April 2018
the matrix material then consolidated through spark plasma sintering. The composites were densified at
1300  C, pressure of 50 MPa, and holding time of 5 min. The microstructure and phase analysis of the
sintered composites was carried out using SEM and XRD, while the hardness was determined using
Keywords:
SPS
Vickers' microhardness tester. The SEM and XRD results confirmed the presence of the TiB whiskers
TiB whiskers which renowned with the improving the hardness of titanium. The hardness of the composite with 10 wt
Hardness % ZrB2 showed the highest hardness compared to that obtained for the 5 and 15 wt% ZrB2 composites
Titanium matrix composites which was 495 and 571Hv respectively.
Reinforcement © 2018 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/).

1. Introduction stiffness of the titanium matrix ([11]:43, [12]:243, [14]:152).

The development of advanced materials that out-perform
existing materials is an area which is in the fore front of the 4th
industrial revolution. Materials such as titanium are one of the
most sought-after materials; as it is used in a wide variety of heavy
and light engineering applications. The need for lightweight high-
performance materials sees materials such as aluminium and ti-
tanium as the ideal solution for armour. However, the use of
aluminium as armour material is limited by its lower strength
when compared to titanium ([7]:12964). Boyer ([2]:22) states that
titanium owns exceptional ballistic resistance behaviour and pro-
vides a 15e35% reduction in weight compared to aluminium.
Although titanium has good ballistic resistance properties, efforts
have been made by researchers to enhance its use as armour ma-
terial ([6]:1, [10]:387). Ceramics remain a highly viable option to
enhance anti-ballistic properties of titanium. Titanium forms stable
TiB whiskers when reinforced with boron-based reinforcements.
Studies have proven that TiB whiskers enhance the hardness
* Corresponding author. Department of Chemical, Metallurgical, and Materials
Engineering, Tshwane University of Technology, P.M.B X680, Pretoria, South Africa.
E-mail address: maseko.sfiso@yahoo.com (S.W. Maseko).
Peer review under responsibility of China Ordnance Society.
However, processing of ceramics remains a serious challenge in the
materials engineering; this is due to the high melting temperatures
and grain coarsening associated with these materials. Spark plasma
(SPS) is a state-of-the-art sintering technology, with the capability
to fabricate fully dense specimens at significantly low temperatures
([13]:320). The unique process parameters associated with this
sintering technology are known to provide exception grain size
retention when compared to conventional processing techniques
([5]:4). However, there is little knowledge in open literature using
reinforcement for a titanium matrix composite. This study aims to
fabricate a titanium-based composite with enhanced anti-ballistic
characteristics through the incorporation of ceramic particulates.
2. Experimental procedure
2.1. Feedstock material
In this study, fine titanium powder supplied by Merck Millipore
(with less than 150 mm particle size, 98% purity) was used as the
matrix material. TiB2 powder supplied by Merck Millipore was used
as the reinforcement material. Figs. 1 and 2 are the SEM and XRD
images of the feedstock commercially pure titanium (CpTi) and
ZrB2.

https://doi.org/10.1016/j.dt.2018.04.013
2214-9147/© 2018 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/).
 S.W. Maseko et al. / Defence Technology 14 (2018) 408e411 409

Fig. 1. SEM micrographs of the feedstock powders: (a) CpTi and(b) ZrB2.

Fig. 2. XRD spectra of the feedstock powders: (a) CpTi and (b) ZrB2.

2.2. Powder mixing characterization using conventional metallography procedures

prior to analysis.
The powder materials were mixed using the PM 400 high en-
ergy ball mill at 300 rpm for 8 h with 3 agate balls to enhance the 2.4. Characterization of sintered samples
mixing kinetics. Three composites were prepared, with reinforce-
ment composition of 5,10,15 wt% ZrB2. Table 1 below, contains a The microstructure and phase evolution of the sintered samples
detailed description of the admixed composites. were investigated using an optical microscope (OPM), scanning
electron microscope (SEM), and x-ray diffractometer (XRD). The
2.3. Powder consolidation microhardness of the samples was determined using the Vickers'
microhardness tester with an applied load of 100 kg. The indenta-
The admixed samples were then densified using the SPS furnace tion was carried out at 10 randomly chosen areas on the surface of
(HPD5, FCT Systeme GmbH). The admixed powders were densified the sample.
at a temperature of 1300  C, at an applied load of 50 MPa, 5 min
dwell time, and heating rate of 100  C/min under a vacuum atmo- 3. Results and discussion
sphere. The sintered products were then prepared for analysis and
3.1. Microstructure and phase characterization
Table 1
Composition of mixed powders.
The OM micrographs depict the formation of needle-like TiB
whiskers for all composites (see Fig. 3(a)-(c)). There is more promi-
Sample Composition
nent formation of TiB whiskers in 85Ti-15 wt%ZrB2 (see Fig. 3(c))
Sample 1 95Ti-5 wt% ZrB2 when compared to the composites with lower reinforcement com-
Sample 2 90Ti-10 wt% ZrB2 positions. Fig. 3(a) shows a few un-diffused ceramic phases which
Sample 3 85Ti-15 wt% ZrB2
can be seen by the black spots. The microstructure of the composites
410 S.W. Maseko et al. / Defence Technology 14 (2018) 408e411

Fig. 3. Micrographs of Ti-ZrB2 binary composites. (a) 95 Ti with 5 wt% ZrB2. (b) 90 Ti with 10 wt% ZrB2. (c) 85 Ti with 15 wt% ZrB2.

showed a decrease in grain size with an increase in composition. This
phenomenon was also evident in the studies conducted by Chaud-
hury et al. ([3]:759) and Kumar, Rao, and Selvaraj ([8]:59). This
phenomenon is attributed to the evolution of TiB2 to TiB which leads
to grain refinement.
Fig. 3(a) and (c) and Fig. 4(a) and (c) shows two distinctive
regions: one is the dominant light and grey, which confirm the
presence of titanium, while the darker boride-rich phase is
randomly distributed in the form of needle-like microstructures
and irregular shaped microstructure. The images also show the
presence of white-like phase, which is less distinctive compared
to the other two prominent phases, the white-coloured phase
occurs along the grain boundaries, this phase is also observed in
the XRD results as (Zr1-x, Tix)O2 phase. The conditions for the
formation of srilankite (Zr1-x, TixO2), and its role in phase equi-
librium studies, are still uncertain. Previous studies have been
carried out with the aim of fabricating (Zr1-x, Tix)O2 species from
through the mechanical alloying of TiO2 and ZrO2 ([4]:153,
[9]:181). The formation of this phase in this study is attributed to
the interstitial oxygen present in the feedstock powders as an
impurity. An even dispersion of the reinforcement particulates
(phases) throughout the matrix can be observed from the images.
This is attributed to the efficient mixing and blending kinetics
associated with the planetary ball mill. The SEM images for all
three composites show that the presence of the ceramic phase is
not only by needle-like structures, TiB is also present in other
irregular shapes. The images also depict grain refinement with an
increase in reinforcement for three composites. This phenomenon
was also observed on the OM micrographs.
The metallographically prepared samples were analysed for
phases. The XRD spectra of the composites is depicted in Fig. 5. The
spectra show that a-Ti is the most prominent phase for all three
composites, this was also observed in the XRD spectra of the un-
sintered CpTi powder. The results also depict the detection of the
cubic b-Ti phase for all three composites: the b phase was detected
at 2q angles of approximately 40 and 54 for sample 4; 40,54, and
70 for sample 5; 70 for sample 3. The formation of the b phase is
due to the evolution of the a phase during the sintering process
([1]:844). The evolution of the a phase is due to the thermo-
mechanical processes of applied pressure and the joule heating
effect associated with SPS ([13]:320). The observation also confirms
the transformation of all the boron species (ZrB2) into TiB in the

Fig. 4. SEM Micrographs of Ti-ZrB2 binary composites: (a) 95Ti with 5 wt% ZrB2. (b) 90Ti with 10 wt% ZrB2. (c) 85Ti with 15 wt% ZrB2.
 S.W. Maseko et al. / Defence Technology 14 (2018) 408e411
Fig. 5. XRD Spectra of Sintered Ti-ZrB2 binary composites.
Fig. 6. Vickers microhardness of the composites.
resultant composites matrix. The patterns also showed that there is
no presence of Ti3B4, which was a possible intermediate phase in
the matrix.
3.2. Microhardness
The microhardness of the composites was presented in Fig. 6. As
expected, the hardness of the composite with the least reinforce-
ment composition was relatively lower compared to the other two
composites; from the SEM images it was observed that sample 1
had the fewest TiB whiskers formed. Sample 2 showed a highest
hardness of 595Hv, which is higher than 571Hv obtained for the
sample 3. This is attributed to the relatively lower densification
expected at high reinforcement compositions. Relative density was
listed as one the physical properties that have significant effect on
hardness in the work carried out by Huang and Chen ([7]:12951).
The OM results of sample 3 (see Fig. 3) showed high contents of the
white-like (Zr1-x, Tix)O2 phase, the low hardness might be due to its
high content compared to sample 1 and 2. However no studies
were found in literature to support this postulation.
411
4. Conclusions
SPS is an effective technique that can be used to fabricate Ti-ZrB2
binary composites at relatively low sintering temperatures. The
methodology used in this study was effective in inducing disper-
sion strengthening effect on the composites; as all the composites
showed an improvement in hardness due to the dispersion of the
ceramic particulates throughout the matrix material. TiB was
readily fabricated through in-situ reaction of Ti and B species, this
resulted in the formation of good interfacial bonding between the
Ti matrix and the TiB reinforcement phase. The good interfacial
bonds between the titanium matrix and the boride based re-
inforcements will lead to the enhancement of the anti-ballistic
properties of titanium.
Acknowledgement
This material is based upon work supported financially by the
National Research Foundation. The authors also acknowledge the
support from the the Tshwane University of Technology, Pretoria,
South Africa which helped to accomplish this work.
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