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Effect of TiN and TiCN additions on spark plasma

sintered Ti–6Al–4V

Oluwasegun E. Falodun, Babatunde A. Obadele, Samuel R. Oke, Oladeji O.

Ige & Peter A. Olubambi

To cite this article: Oluwasegun E. Falodun, Babatunde A. Obadele, Samuel R. Oke,

Oladeji O. Ige & Peter A. Olubambi (2020) Effect of TiN and TiCN additions on spark
plasma sintered Ti–6Al–4V, Particulate Science and Technology, 38:2, 156-165, DOI:
10.1080/02726351.2018.1515798

To link to this article: https://doi.org/10.1080/02726351.2018.1515798

Published online: 10 Oct 2018.

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PARTICULATE SCIENCE AND TECHNOLOGY
2020, VOL. 38, NO. 2, 156–165
https://doi.org/10.1080/02726351.2018.1515798

Effect of TiN and TiCN additions on spark plasma sintered Ti–6Al–4V

Oluwasegun E. Falodun, Babatunde A. Obadele, Samuel R. Oke, Oladeji O. Ige, and Peter A. Olubambi
Centre for Nanoengineering and Tribocorrosion, University of Johannesburg, Johannesburg, South Africa

ABSTRACT KEYWORDS
In this study, the microstructural and densification behavior of titanium nitride (TiN) and titanium Nanoparticle; TiCN;
carbonitride (TiCN) reinforced Ti-6Al-4V were investigated under an applied pressure of 50 MPa, microstructure; TiN;
sintering temperatures of 1000–1100
C, heating rate of 100
C/min and dwell time of 10–20 min shrinkage rate
through spark plasma sintering technique. Results show that the microstructural transformation of
the titanium matrix composite comprises of a mixture of lamellar colonies with b grain boundaries
and nanoparticles with an average grain size range of 4.5–6.0 lm. Furthermore, an addition of
nanoceramics TiN/TiCN resulted in microstructural transformation, uniform particle distribution
within the metal matrix and along the grain boundary. However, the sintered relative density of
the composites decreased with the percentage increase in TiCN, while fully dense composites
were obtained at a sintering temperature of 1100
C. Microhardness values of the sintered compo-
sites reach a greater level in comparison to Ti-6Al-4V alloy while fracture morphology of the
sintered composites with addition of nanoceramics (TiN/TiCN) displayed a transgranular transform-
ation within the matrix accompanied with fine dimple features.

1. Introduction transferred to the samples (Nygren and Shen 2003). A

Spark plasma sintering (SPS) is both a recognized and
emerging sintering method, which has recently become
widespread in use and has attracted considerable attention
for powder metallurgy due to certain characteristics of its
heating mechanism, such as lower sintering and cooling
times, rapid temperature increase and a fixed heating state
for sintered materials. This has been useful in the consolida-
tion of metal matrix composites with improved mechanical
properties in comparison to the sintering techniques of con-
ventional methods (Kim et al. 2009; Song, Wang, and Shi
2013; Obadele, Ige, and Olubambi 2017). Spark plasma sin-
tering (SPS) originates from an electrical current pulsed
through a graphite die. The powder is intensely heated by
the usage of Joule heating of powder and graphite die, which
generates spark discharge between the conductive particles
(Tokita 1993; Kumar et al. 2005; Shearwood et al. 2005;
Zhou, Mei, and Zhu 2005). Rapid heating is achieved, which
sequentially reduces the entire sintering time to one minute,
and thus using the spark plasma sintering technique is con-
sidered advantageous in fabricating nanocrystalline and
ultrafine-grained materials (Fu and Shearwood 2004; Kim
et al. 2005; Zhang et al. 2008).
One promising approach is the application of automatic
pressure, which helps in the elimination of pores from the
compacted material and further improving diffusion.
Transfer of heat from graphite die to the sintered materials
is effectual in these practices. Graphite dies serve as heating
components and the required drive for compaction is well
pulsed DC current works in initiating and further creating
improvement in sintering kinetics, improving densities, dis-
tinguishing microstructures, cleansing the interface between
the grains, and removing impurities from the surface using
the spark plasma technique, which has given rise to general
improvement in the materials’ behavior (Groza, Garcia, and
Schneider 2001; Shen and Nygren 2005; Anselmi-Tamburini
et al. 2006). The release of sparks and/or plasma at the early
stage of heating progression causes the removal of any accu-
mulated liquid or gases (CO2 and H2O) present on the pow-
der surfaces. In supplementary stages, removal of reactive
surfaces is expected to improve the grain boundary diffusion
which, composed with the anticipated spark releases and/or
plasma methods will increase transfer of material and fur-
ther speed up densification and grain growth (Yamazaki
et al. 1996).
Titanium and Titanium alloys are very attractive materi-
als, which provide extensive choice of applications including
aerospace, biomedical, and other industrial applications.
However, despite the superior definite strength to weight
ratio, corrosion resistance and biocompatibility, the lack of
strength and hardness limit their usage for high-temperature
applications (Eylon and Seagle 2000; Sobiecki, Wierzcho
n,
and Rudnicki 2001; Gurrappa 2003). Titanium matrix com-
posites (TMCs) have been reinforced with various types of
materials and have proved a promising substitute to improve
strength and Young’s modulus of titanium alloys
(Ranganath 1997; Lagos et al. 2016; Falodun et al. 2017a).

CONTACT Oluwasegun E. Falodun segzy201@gmail.com Centre for Nanoengineering and Tribocorrosion, Department of Metallurgy, University of
Johannesburg, Johannesburg 2028, South Africa.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/upst.
ß 2018 Taylor & Francis Group, LLC

Metal matrix composites (MMCs) are associated with sever-
ity and strengthened with ceramic material provided by a
metal matrix (Gofrey, Goodwin, and Ward-Close 2000).
Abkowitz et al. (2004) and Choi et al. (2008) stated that
adding ceramic particles to titanium alloy matrix can
enhance its mechanical properties and also improve high-
temperature capability (Abkowitz et al. 2004; Choi et al.
2008). However, recent advancement in MMCs have led to
their consideration for various uses in aerospace, as well as
the marine and automobile industries where the prerequisite
for high-temperature applications area combination of
strength, stiffness, reduction in density, and resistance to
wear (Gofrey, Goodwin, and Ward-Close 2000). Also, sev-
eral studies have investigated the influence of ceramic addi-
tives (as a reinforcement phase) such as Al2O3, TiN, TiB2,
SiC, TiC, and B4C in the microstructural evolution and
mechanical properties of TMCs (Morsi et al. 2008; Zhang
et al. 2010; Shen et al. 2011). Development of new materials
with recent nano synthesis technology has been practically
applicable with better properties and further improving the
mechanical properties of traditional materials (Zheng et al.
2005). In order to avoid the failure of MMCs, strengthening
with fine ceramic particles is desired (Li et al. 2015).
Figure 1. XRD diffractogram of as–received powders: (a) Ti–6Al–4V alloy, (b) nano-TiN, (c) nano-TiCN and (d) Ti–6Al–4V þ 4% TiN þ1% TiCN.
PARTICULATE SCIENCE AND TECHNOLOGY 157
Strengthening a metal matrix with ceramic particles serves
as a pinning effect, which acts to impede movement of dis-
locations within the grains and interface between the grains
(Mazahery and Shabani 2013). The process of increasing the
matrix/reinforcement boundary plays an important role in
determining the strength of the MMCs (Chu et al. 2013).
Final properties achieved in this boundary determine the
strength of the composite for the reason that load bearing
from the matrix is transferred to the reinforcement (Piggott
1989; Chen and Alpas 1996).
Dispersion of nitrogen into titanium and titanium alloys
has been studied and found to efficiently protect them
against wear. Nitrogen has a great solubility in a-Ti, so it
strengthens the surface layer effectively (Zhecheva et al.
2005). Falodun et al. 2017b have successfully synthesized
Ti–6Al–4V with the nanoparticle of TiN composite, using
spark plasma sintering methods. However, there is no pub-
lished literature of the spark plasma sintering technique in
the synthesis of Ti–6Al–4V with nano-TiN/TiCN ceramic.
The objectives of this paper are (i) to explore the synthe-
sis of titanium based metal matrix composite with minor
addition of nanoparticle TiN/TiCN reinforcement using the
spark plasma sintering technique, and (ii) to explore the
158 O. E. FALODUN ET AL.
Figure 2. (a,b) SEM microstructure of Ti–6Al–4V powder mixed with 4 vol.% TiN and 1 vol.% TiCN use during SPS process (c) TEM microstructure of
Ti–6Al–4V þ 4 vol.% TiN þ1 vol.% TiCN powders.
Figure 3. Shrinkage rate against time plots of Ti–6Al–4V þ 4 %TiN þ1 %TiCN
to determine the sintering behavior of the sintered composite.
densification, phase constituents, microstructural evolution,
microhardness, and fracture morphology of the titanium
matrix composite. The sintering parameters such as heating
rate, temperature, and dwelling time have a crucial effect on
density and mechanical properties of the material.
2. Experimental procedure
2.1. Materials and powder preparation
Titanium nitride (TiN) and Titanium carbonitride
(TiC0.7N0.3) powders (purity and APS of 97%, 20 nm; 97%,
80 nm supplied by Nanostructured and Amorphous Matls
Figure 4. Relative density with different percentages of reinforcement samples.
Inc., USA) were used as reinforcement materials and
Titanium powder (Purity 99.9% APS 25 mm) from TLS
Technik company as starting matrix material. XRD patterns
of the supplied raw materials of Ti–6Al–4V, TiN and TiCN
powders are shown in Figures 1 and 2. The powders were
mechanically mixed using turbula T2F mixer for 8 h in a
dry medium state to prepare the composite materials.
2.2. Fabrication of Ti–6Al–4V/TiN/TiCN and
thermo-mechanical processing
The composite materials were produced by a powder metal-
lurgy (PM) process, namely spark plasma sintering. The
 PARTICULATE SCIENCE AND TECHNOLOGY 159

Table 1. Relative density, Vickers hardness and obtained average grain sizes of the samples.
Sintering conditions
Sintering Materials Temp (
C) Time (min) Relative Density(%) Average grain size(lm) Hardness(HV0.1)
Ti-6Al-4V þ 4TiN þ0.5% TiCN 1000 10 97.05 5.5 569
20 99.26 5.0 580
Ti-6Al-4V þ 4TiNþ 0.5% TiCN 1100 10 98.99 4.5 560
20 99.01 5.5 591
Ti-6Al-4V þ 4TiN þ1% TiCN 1000 10 99.12 6.0 616
20 99.08 6.0 625
Ti-6Al-4V þ 4TiN þ1% TiCN 1100 10 99.05 5.0 644
20 98.96 5.5 640

Figure 5. Optical microstructure of composites with 4 vol% TiN and 0.5–1 vol% TiCN sintered at: 0.5 vol.% TiCN (a) 1000/10, (b) 1000/20, (c) 1100/10, (d) 1100/20;
and 1 vol.% TiCN (e) 1000/10, (f) 1000/20, (g) 1100/10, (h) 1100/20.

powder mixtures were loaded into a cylindrical graphite die
and then consolidated using spark plasma sintering
(HHPD–25 FCT model, Germany). Sintering was carried
out in vacuum conditions at 1000–1100
C under a constant
pressure of 50 MPa. The temperature in the furnace was
monitored with a top mounted pyrometer at 3 mm which
focused on the inside face of the hollow punch from the
powder. The heating rate was set at 100
C/min and after
holding at the sintering temperature the samples were
cooled down in the SPS chamber to room temperature. A
diameter of 30 mm and a 5 mm thickness were produced
from the sintered compact.
2.3. Material characterization
The density of sintered composite samples was determined
by the Archimedes’ principle using distilled water as the
immersion medium. The relative density of the sintered
samples was estimated in accordance with the theoretical
density, calculated based on the rule of mixtures. The
160 O. E. FALODUN ET AL.
densities of the raw materials used were as follows;
Ti–6Al–4V (4.43 g/cm3), TiN (5.22 g/cm3), and TiCN
(5.02 g/cm3). For microstructural examination, the sintered
samples were cut using a precision cutter and their cross
section was mounted, grinded, polished, and etched using
Kroll’s reagent in order to explore the microstructures in
greater detail. Microstructural observations were performed
using Zeiss optical microscope and a scanning electronic
microscope (JEOL JSM-7600F model) with attachment of
Figure 6. XRD patterns of sintered titanium matrix composite at 1000
and 1100
C.
Figure 7. Microstructures of titanium matrix composites with 0.5 vol.% TiCN sintered at: 1000
C (a) 10 min, (b) 20 min and 1100
C (c) 10 min, (d) 20 min.
energy dispersive x-ray spectroscopy (EDS). x-ray diffraction
(XRD) was done before and after the SPS process in order
to identify the constituent phases present in the sintered
composites. A Philips diffractometer (PANalytical Empyrian
PW1710) with monochromatic Cu Ka radiation at 40 kV
and 40 mA was used for measurements. The microhardness
values of the samples were characterized by a Vickers tester
(FALCON 500 series) with a diamond indenter under an
applied load of 100 gf and dwelling time of 15 sec. on the
polished surfaces.
3. Results and discussion
3.1. Analysis of materials and mixing operation
The detectable crystalline phases in the powders are shown
based on the x-ray diffraction pattern presented in Figure
1(a–c). Typical XRD patterns of the powder mixture with
different amounts of TiN/TiCN nanoparticles are shown in
Figure 1(d) with normalized peak intensity. It can be seen
that the powder presents identical patterns and neither
transformations nor new compounds appear after mixing
of the powder. The diffraction peak of a phase
slightly decreased.
Varying reinforcement ratios of 4 vol.% TiN,
0.5–1.0 vol.% TiCN were added to Ti–6Al–4V powder to
produce TMC. Figure 2(a–b) presents microstructure of

Ti–6Al–4V/TiN/TiCN powders and Figure 2(c) shows the
TEM morphology of the mixed powders. This shows that
the nanoparticles diffuse into the titanium grains.
3.2. Analysis of shrinkage rate behavior of the
sintered composite
The shrinkage behavior details during SPS of nanocompo-
sites for the duration were assessed; Figure 3 shows the
shrinkage rate during SPS against sintering time of the sin-
tered TMCs. The shrinkage rate can be helpful in connect-
ing the start and total amount of shrinkage during the
sintering processes. These further demonstrate that densifi-
cation occurrences of nanocomposites during sintering can
be observed through the shrinkage rate of the matrix com-
posites. Shrinkage rate behavior exhibits similar trends irre-
spective of the sintering conditions and the difference in
reinforcement; this behavior is characterized by three dis-
tinct peaks labeled (1, 2, and 3).
The rearrangement of powder particles shown in the ini-
tial peak is attributed to the relative motion of the powders,
gas removal, and creation of spark between titanium alloy
and reinforcement particles due to the application of pres-
sure and drive taking place from the lower and upper
punches (Oke et al. 2018). Angerer et al. 2004 reported that
smaller particle sizes of powders require an initiation energy
before the reaction can occur, which then increases their
Figure 8. Microstructures of titanium matrix composites with 1 vol.% TiCN sintered at: 1000
C (a) 10 min, (b) 20 min and 1100
C (c) 10 min, (d) 20 min.
PARTICULATE SCIENCE AND TECHNOLOGY 161
rate to deform under an applied pressure and the presence
of heat due to their higher amount of surface enclosed
within a boundary. The higher resistivity of the reinforcing
ceramic particles and their harder nature compared to their
metal matrix particles could cause problems of gas removal
during sintering (Ghasali et al. 2017). Furthermore, the
second peak is connected to the localized distortion at an
interaction point between them, while the third peak repre-
sents a greater deforming zone for the TMC (Diouf and
Molinari 2012). An increase in the density gradation is a
function of the strength of the peaks and degree of the
deforming particles.
Figure 4 presents the effects of TiCN at different sinter-
ing temperatures and dwelling times on the relative density
of the TMC. It is a clear indication that addition of TiCN
has a significant effect during the sintering process.
Addition of 0.5–1.0 vol.% TiCN slightly decreases the rela-
tive density of the composites, although the relative den-
sities have a similar values range. This occurrence might
be related with the initiated grain development and the
arrangement of structures with pores situated in the inter-
ior. The relative density of the sintered composites at
1000–1100
C for 10 and 20 min, respectively resulted in
sintered densities ranging from 98.99 to 99.12% upon add-
ition of TiCN as shown in Table 1. The reduction in the
porosity level could be as a result of an increase in the
sintering time, which increases the material’s density.
162 O. E. FALODUN ET AL.
3.3. Microstructural evolution and XRD analysis of
sintered Ti–6Al–4V/TiN/TiCN composites
The optical microstructure of sintered materials with
increasing SPS temperature and dwelling time is shown in
Figure 5(a–h). The microstructure of all the sintered samples
revealed light-colored parts and some dark-colored parts.
The addition of a ceramic phase impeded the diffusion of
atoms and therefore caused a decrease in the sintering rate
of the materials during sintering (Goujon and Goeuriot
Figure 9. Microhardness values of the sintered composites.
Figure 10. SEM fracture surfaces of titanium matrix composites with 0.5 vol.% TiCN sintered at: 1000
C (a) 10 min, (b) 20 min and 1100
C (c) 10 min, (d) 20 min.
2001). The distribution of grains was homogeneous and had
a dense structure in TMCs. Nevertheless, grain sizes of the
sintered composites were all within the range of 4.5–6.0 lm
in accordance with ASTM E 112 standard as shown in
Table 1. Figure 5(h) shows evidence that it has considerably
lower porosity when compared to the remaining sintered
composites. Nanoparticle TiN/TiCN addition resulted in the
microstructural transformation from lamellar phase to
bimodal phase as a result of temperature and time which
produces b-grain size.
The XRD analysis of sintered Ti-6Al-4V/TiN/TiCN sam-
ples at the sintering temperature of 1000, 1100
C and dwell-
ing time of 10 and 20 min are shown in Figure 6. The
characteristics XRD confirm the presence of a and b peaks
phases, which are formed after SPS processing and no other
undesirable phases were found. However, reduction in the
titanium characteristic reflection is observed with increasing
TiN/TiCN nanoparticles. A decrease in the intensity peak
can be attributed to the x-ray absorption effect.
Figure 7 shows the SEM microstructures of the sintered
composites at different temperature and dwelling times,
from all the reinforcing phases of 4 vol.% TiN and
0.5–1.0 vol. % TiCN powder mixtures. The grains grow sig-
nificantly under the increase in both temperature and hold-
ing time. It is well-known that the crystal lattice of a phase
structure has a lower atomic packing factor than that of b

phase structure. Hence, the presence of a less compacted
phase assists the diffusion which consequently promotes the
grain growth. It was observed that increasing the tempera-
ture resulted in a and b phase layers to grow together.
Higher sintering temperatures may lead to advanced grain
boundary migration and grain progression with the relative
increase of the densities (Miklaszewski, Garbiec, and
Niespodziana 2018). Figure 7(a–d) shows the SEM micro-
structure of the sintered composites prepared from 0.5 vol.
% TiCN - 4 vol. % TiN and sintered at 1000/1100
C
revealed the TiCN distribution surrounded in the titanium
matrix. Microstructure revealed the absence of any micro
pores, except for Figure 7(c), which revealed micropores in
the surrounding area of coarse Ti–6Al–4V particles with a
weak bonding of TiCN particles and within titanium matrix
surrounding. Fine TiN particles were uniformly distributed
in the titanium matrix. SEM microstructure (Figure 8(a–d))
of the sintered material prepared from the powder mixtures
with 1 vol. % TiCN, 4 vol. % TiN sintered at 1000/1100
C.
The structure has generated a duplex microstructure made
of a mixture of lamellar colonies and b grain boundaries
containing some nanoparticles. The increase in densification
with increased temperature correlates with grain movement,
which gradually leads to closure of pores as anticipated.
Therefore, increase in sintering temperature resulted in grain
size development, while increase in the consolidated com-
posite remained rather limited.
Figure 11. SEM fracture surfaces of titanium matrix composites with 1 vol.% TiCN sintered at: 1000
C (a) 10 min, (b) 20 min and 1100
C (c) 10 min, (d) 20 min.
PARTICULATE SCIENCE AND TECHNOLOGY 163
3.4. Microhardness
Figure 9 shows the microhardness results, in respect to both
sintering temperature and dwelling time. The sintered sam-
ple at 1000
C/10 min has the lowest hardness value of 389
HV. The hardness measurement result revealed that the
addition of 0.5–1.0 vol. % TiCN increases the hardness of
the TMCs from 569 to 644 HV0.1. The increase in hardness
can be described by the high hardness attributes of the
added additives. Relative density and grain size of a material
have an effect on the hardness of sintered materials
(Muhammad et al. 2011) and a larger load can be carried
for the dense specimens compared to specimens with a high
porosity. It is outstanding that decrease in hardness could
be due to grain size increase in accordance to Hall–Petch
relationship (Yuan et al. 2011). Therefore, grain size and
densification behavior play a significant role in the hardness
of sintered samples. As shown in the Figure 9, hardness sig-
nificantly increased with increased content of nanoparticles
for both the composites. The higher constraint of localized
matrix distortion due to the increased content of nanopar-
ticles would contribute to the increase in hardness of the
composite (Ugandhar, Gupta, and Sinha 2006). Also increase
in hardness was improved upon the addition of nanocompo-
sites due to the stronger diffusional connections and struc-
tural integrity achieved after the SPS process and
microstructural characteristic features.
164 O. E. FALODUN ET AL.
3.5. Fractography
Figures 10 and 11 show the SEM fractographs of sintered
titanium samples at different temperatures and holding
times. Fracture morphology of the sintered samples shows a
well-developed cooperation between the particles, and the
possibility exists that fracture surfaces significantly change
with increasing the sintering temperature. The presence of
dimples and shabby areas can be attributed to their high
plasticity and could be a result of good cohesion between
reinforcements and the TMCs (Falodun et al. 2018). Figures
10 and 11 show the presence of a trans-granular pattern
with fine dimple features upon the addition of 4 vol.% TiN
and 0.5–1.0 vol.% TiCN. A notable effect on the fracture
behavior of the sintered composites was revealed by the
amount of TiN/TiCN reinforcement added to the matrix. In
other fracture surfaces (Figure 11(c–d)), the sintered samples
at 1100
C show a well-built joint between the particles and
thus change significantly with increase in temperature and
dwelling times. Also, a ductile fracture mode was revealed
with quasi-cleavage areas on the fracture surfaces.
4. Conclusion
Spark plasma sintering (SPS) method was successfully used
in the production of a titanium matrix with addition of
nano TiN/TiCN reinforcement particles at different temper-
atures of 1000 and 1100
C for 10–20 min under 50 MPa in
a vacuum. The influence of sintering temperature on densi-
fication, phase constituents, microstructure, fracture morph-
ology, and microhardness on TMCs was investigated.
The sintered sample reached 99% theoretical density
when sintered at 1100
C and increase in dwelling time from
10 to 20 min led to higher density. Titanium alloys with
TiN/TiCN nanoparticles were sintered by the SPS method to
find a suitable sintering temperature and the majority of the
samples were highly dense. TiN/TiCN nanoparticles were
uniformly dispersed along the titanium matrix boundary
and little agglomeration was seen in the matrix. However,
microhardness values of the samples were almost in close
range irrespective of the sintering temperature and time.
The hardness values, upon addition of 0.5–1.0 vol. % TiCN,
increased from 569 to 644 HV0.1. A duplex microstructure
made of a mixture of lamellar colonies and b grain bounda-
ries containing some nanoparticles was revealed, while the
fracture morphology of the sintered TMCs with TiN/TiCN
showed transgranular transformation within the matrix with
fine dimples features. Also, a ductile fracture mode with
quasi-cleavage was revealed and the fractography behavior
further changed from a multiple arrangement to a predom-
inantly transgranular one.
Acknowledgments
The authors would like to thank Global Excellence and Stature (GES),
University of Johannesburg, South Africa for funding Oluwasegun
Falodun. Also, Dr Obadele would like to specially acknowledge Claude
Leon Foundation for fellowship grant.
References
Abkowitz, S., S. M. Abkowitz, H. Fisher, and P. J. Schwartz. 2004.
CermeTiV R discontinuously reinforced Ti-matrix composites:
Manufacturing, properties, and applications. JOM 56 (5):37–41.
Angerer, P., L. Yu, K. A. Khor, and G. Krumpel. 2004. Spark-plasma-
sintering (SPS) of nanostructured and submicron titanium oxide
powders. Materials Science and Engineering: A 381 (1-2):16–9.
Anselmi-Tamburini, U., Y. Kodera, M. Gasch, C. Unuvar, Z. A. Munir,
M. Ohyanagi, and S. Johnson. 2006. Synthesis and characterization
of dense ultra-high temperature thermal protection materials pro-
duced by field activation through spark plasma sintering (SPS): I.
Hafnium diboride. Journal of Materials Science 41 (10):3097–104.
Chen, H., and A. Alpas. 1996. Wear of aluminium matrix composites
reinforced with nickel-coated carbon fibres. Wear 192 (1-2):186–98.
Choi, B.-J., S.-Y. Sung, M.-G. Kim, and Y.-J. Kim. 2008. Evaluation the
properties of titanium matrix composites by melting route synthesis.
Journal of Materials Science and Technology-Shenyang 24 (1):105.
Chu, K., C.-C Jia, L.-K Jiang, and W.-S Li. 2013. Improvement of inter-
face and mechanical properties in carbon nanotube reinforced
Cu–Cr matrix composites. Materials & Design 45:407–11.
Diouf, S., and A. Molinari. 2012. Densification mechanisms in spark
plasma sintering: Effect of particle size and pressure. Powder
Technology 221:220–7.
Eylon, D., and S. Seagle. 2000. Titanium’99: Science and technology. St.
Petersburg, 866–875.
Falodun, O., B. Obadele, S. Oke, M. Maja, and P. Olubambi. 2017a.
Synthesis of Ti-6Al-4V alloy with nano-TiN microstructure via
spark plasma sintering technique. In IOP conference series: Materials
science and engineering, 012029. Bristol, UK: IOP Publishing.
Falodun, O. E., B. A. Obadele, S. R. Oke, O. O. Ige, P. A. Olubambi,
M. L. Lethabane, and S. W. Bhero. 2017b. Influence of spark plasma
sintering on microstructure and wear behaviour of Ti-6Al-4V/TiN
composites. Transactions of Nonferrous Metals Society of China T 28
(1):47–54.
Falodun, O. E., B. A. Obadele, S. R. Oke, M. E. Maja, and P. A.
Olubambi. 2018. Effect of sintering parameters on densification and
microstructural evolution of nano-sized titanium nitride reinforced
titanium alloys. Journal of Alloys and Compounds 736 (Supplement
C):202–10.
Fu, Y., and C. Shearwood. 2004. Characterization of nanocrystalline
TiNi powder. Scripta Materialia 50 (3):319–23.
Ghasali, E., K. Shirvanimoghaddam, A. H. Pakseresht, M. Alizadeh,
and T. Ebadzadeh. 2017. Evaluation of microstructure and mechan-
ical properties of Al-TaC composites prepared by spark plasma sin-
tering process. Journal of Alloys and Compounds 705:283–9.
Gofrey, T., P. S. Goodwin, and C. M. Ward-Close. 2000. Titanium par-
ticulate metal matrix composites–reinforcement, production meth-
ods, and mechanical properties. Advanced Engineering Materials 2
(3):85–91.
Goujon, C., and P. Goeuriot. 2001. Solid state sintering and high tem-
perature compression properties of Al-alloy5000/AlN nanocompo-
sites. Materials Science and Engineering: A 315 (1-2):180–8.
Groza, J., M. Garcia, and J. Schneider. 2001. Surface effects in field-
assisted sintering. Journal of Materials Research 16 (1):286–92.
Gurrappa, I. 2003. Characterization of titanium alloy Ti-6Al-4V for
chemical, marine and industrial applications. Materials
Characterization 51 (2-3):131–9.
Kim, C. K., H. S. Lee, S. Y. Shin, J. C. Lee, D. H. Kim, and S. Lee.
2005. Microstructure and mechanical properties of Cu-based bulk
amorphous alloy billets fabricated by spark plasma sintering.
Materials Science and Engineering: A 406 (1-2):293–9.
Kim, J., I. Povstugar, P. Choi, E. Yelsukov, and Y. Kwon. 2009.
Synthesis of Al–Y–Ni–Co composites by mechanical alloying and
consecutive spark-plasma sintering. Journal of Alloys and
Compounds 486 (1):511–4.
Kumar, R., K. Prakash, P. Cheang, and K. Khor. 2005. Microstructure
and mechanical properties of spark plasma sintered zirconia-
hydroxyapatite nano-composite powders. Acta Materialia 53 (8):
2327–35.

Lagos, M. A., I. Agote, G. Atxaga, O. Adarraga, and L. Pambaguian.
2016. Fabrication and characterisation of titanium matrix compo-
sites obtained using a combination of self propagating high tempera-
ture synthesis and spark plasma sintering. Materials Science and
Engineering: A 655 (Supplement C):44–9.
Li, M., H. Zhai, Z. Huang, X. Liu, Y. Zhou, S. Li, and C. Li. 2015.
Tensile behavior and strengthening mechanism in ultrafine TiC 0.5
particle reinforced Cu–Al matrix composites. Journal of Alloys and
Compounds 628:186–94.
Mazahery, A., and M. O. Shabani. 2013. Plasticity and microstructure
of A356 matrix nano composites. Journal of King Saud University-
Engineering Sciences 25 (1):41–8.
Miklaszewski, A., D. Garbiec, and K. Niespodziana. 2018. Sintering
behavior and microstructure evolution in cp-titanium processed by
spark plasma sintering. Advanced Powder Technology 29 (1):50–7.
Morsi, K., V. Patel, S. Naraghi, and J. Garay. 2008. Processing of tita-
nium–titanium boride dual matrix composites. Journal of Materials
Processing Technology 196 (1-3):236–42.
Muhammad, W. N. A. W., Z. Sajuri, Y. Mutoh, and Y. Miyashita.
2011. Microstructure and mechanical properties of magnesium com-
posites prepared by spark plasma sintering technology. Journal of
Alloys and Compounds 509 (20):6021–9.
Nygren, M., and Z. Shen. 2003. On the preparation of bio-, nano- and
structural ceramics and composites by spark plasma sintering. Solid
State Sciences 5 (1):125–31.
Obadele, B. A., O. O. Ige, and P. A. Olubambi. 2017. Fabrication and
characterization of titanium-nickel-zirconia matrix composites pre-
pared by spark plasma sintering. Journal of Alloys and Compounds
710:825–30.
Oke, S. R., O. O. Ige, O. E. Falodun, B. A. Obadele, M. B. Shongwe,
and P. A. Olubambi. 2018. Optimization of process parameters for
spark plasma sintering of nano structured SAF 2205 composite.
Journal of Materials Research and Technology 7 (2):126–34.
Piggott, M. 1989. The interface in carbon fibre composites. Carbon 27
(5):657–62.
Ranganath, S. 1997. A review on particulate-reinforced titanium matrix
composites. Journal of Materials Science 32 (1):1–16.
Shearwood, C., Y. Q. Fu, L. Yu, and K. A. Khor. 2005. Spark plasma
sintering of TiNi nano-powder. Scripta Materialia 52 (6):455–60.
Shen, X., Z. Zhang, S. Wei, F. Wang, and S. Lee. 2011. Microstructures
and mechanical properties of the in situ TiB–Ti metal–matrix
PARTICULATE SCIENCE AND TECHNOLOGY 165
composites synthesized by spark plasma sintering process. Journal of
Alloys and Compounds 509 (29):7692–6.
Shen, Z., and M. Nygren. 2005. Microstructural prototyping of ceram-
ics by kinetic engineering: applications of spark plasma sintering.
The Chemical Record 5 (3):173–84.
Sobiecki, J. R., T. Wierzcho
n, and J. Rudnicki. 2001. The influence of
glow discharge nitriding, oxynitriding and carbonitriding on surface
modification of Ti–1Al–1Mn titanium alloy. Vacuum 64 (1):41–6.
Song, S.-X., Z. Wang, and G.-P. Shi. 2013. Heating mechanism of spark
plasma sintering. Ceramics International 39 (2):1393–6.
Tokita, M. 1993. Trends in advanced SPS spark plasma sintering sys-
tems and technology. Journal of the Society of Powder Technology,
Japan 30 (11):790–804.
Ugandhar, S., M. Gupta, and S. Sinha. 2006. Enhancing strength and
ductility of Mg/SiC composites using recrystallization heat
treatment. Composite Structures 72 (2):266–72.
Yamazaki, K., S. Risbud, H. Aoyama, and K. Shoda. 1996. PAS (plasma
activated sintering): transient sintering process control for rapid
consolidation of powders. Journal of Materials Processing Technology
56 (1-4):955–65.
Yuan, W., S. Panigrahi, J.-Q. Su, and R. Mishra. 2011. Influence of
grain size and texture on hall–petch relationship for a magnesium
alloy. Scripta Materialia 65 (11):994–7.
Zhang, Z-h, X.-B. Shen, S. Wen, J. Luo, S-K Lee, and F-C Wang. 2010.
In situ reaction synthesis of Ti–TiB composites containing high
volume fraction of TiB by spark plasma sintering process. Journal of
Alloys and Compounds 503 (1):145–50.
Zhang, Z.-H., F.-C. Wang, L. Wang, and S.-K. Li. 2008. Ultrafine-
grained copper prepared by spark plasma sintering process.
Materials Science and Engineering: A 476 (1-2):201–5.
Zhecheva, A., W. Sha, S. Malinov, and A. Long. 2005. Enhancing the
microstructure and properties of titanium alloys through nitriding
and other surface engineering methods. Surface and Coatings
Technology 200 (7):2192–207.
Zheng, Y., W. Xiong, W. Liu, W. Lei, and Q. Yuan. 2005. Effect of
nano addition on the microstructures and mechanical properties of
Ti (C, N)-based cermets. Ceramics International 31 (1):165–70.
Zhou, W., B. Mei, and J. Zhu. 2005. Fabrication of high-purity ternary
carbide Ti 3 SiC 2 by spark plasma sintering technique. Materials
Letters 59 (12):1547–51.