Microstructural and Mechanical Characteristics of

in-situ Titanium Metal Matrix Composites

K. Srinivasa Vadayar1, S. Devaki Rani2 & V.V. Bhanu Prasad3

1&2

Dept. of Met. Engineering, JNTUH, College of Engineering, Kukatpally, Hyderabad-85.

3
Scientist G, CCG, DMRL, Kanchanbagh, Hyderabad-58
E-mail : ksvadayar@rediffmail.com,

Abstract Discontinuously reinforced titanium matrix

composites (DRTMCs) are emerging as an alternate to
titanium and its alloys for ambient and elevated
temperature applications. The present investigation deals
with P/M processing of DRTMCs and their
characterization. Ti & B4C (1200#, d50 3m ) powders in
three different proportions were blended, compacted and
pressureless sintered resulting in Ti matrix composites
with 10, 20 &30 vol.% of TiB-TiC reinforcements.
Completion of reaction between Ti and B4C resulting in Ti,
TiB and TiC was confirmed through XRD and
microstructural study by SEM. Density, flexural strength,
hardness and elastic modulus were measured. TMCs
exhibited better mechanical properties in comparison to
unreinforced titanium.

and Ti-B4C powders, respectively. Their study reported

formation of TiB needles in former case while TiB
particles in the latter case. Ma et al. [5] prepared Ti-TiB
composites with low volume fractions (<15%) of
reinforcements by reaction hot pressing the Ti-B, TiTiB2, Ti-B4C and Ti-BN. The hot pressing route
followed by the above researchers is expensive and has
size & shape limitations. The present investigation is
aimed at evaluation of pressureless sintering process to
synthesize Ti-TiB-TiC composites out of Ti-B4C cold
pressed compacts and to study the effect of vol.% of the
reinforcement on the microstructural features as well as
on the mechanical properties.
II. EXPERIMENTAL PROCEDURE
Ti-TiB-TiC composites have been synthesized by
pressureless reaction sintering of Ti-B4C green
compacts making use of the following reaction.

Key words : Elastic Modulus, Flexural strength, Titanium

matrix composites, SEM.

I.

INTRODUCTION

5 Ti + B4C 4 TiB + TiC H298 = -754.36 kJ/mol (1)

Discontinuously reinforced titanium matrix

composites (DRTMCs) are of considerable interest for
structural, thermal and armour applications due to the
potential for making composites with high specific
modulus and strength at relatively low costs. Ranganath
et al. [1] produced Ti-TiB-TiC composites by
combustion assisted synthesis of Ti-B4C (CAS) using
arc melting technique. This process could not be
followed for synthesizing composites having higher
volume fractions of reinforcements due to non
uniformity in microstructures. Panda et al. and Sahay et
al. [2,3] studied a series of TMCs, with varying volume
fractions (30% to 90%) of TiB needles, made by hot
pressing the Ti-TiB2 powders. It was reported that
morphology of TiB needle changes depending upon the
reinforcement volume fraction in the composite. Bhat et
al. [4] produced in-situ TMCs containing high volume
fractions of TiB, TiB-TiC, by hot pressing the Ti-TiB2

Excess titanium over and above the stoichiometric

titanium content determined by Eq (1) was used to get
necessary amount of matrix titanium. Powders of
titanium and three different vol.% of B 4C (1.8, 3.6 and
5.4 ) have been used to synthesize 10, 20 and 30 vol.%
(TiB + TiC) reinforcements, respectively in titanium
matrix. Titanium powder made by hydride- dehydrade
route having average particle size of 13m was blended
with B4C powder having average particle size of 3m
in a roller mill using a poly propylene bottle for 24 hrs.
The blended powder was cold compacted into 70 mm x
35 mm x 6 mm compacts at a pressure of 60 MPa for 30
seconds. The green compacts so obtained were
subjected to pressureless sintering under 2x10 -3 m.bar
vacuum at a temperature of 1450C for a period of 1 hr.
Sintering resulted in integral compacts having ~98.5%
theoretical density which are free from cracks and
warpage. Shrinkage of 16-18% has been observed in the
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dimensions of the cold compact as a result of sintering.

Phillips PW 3020 diffractometer with Cu K radiation
was used to conduct X-ray diffraction studies on
pressureless sintered compacts of titanium and
composites using for confirmation of phases before and
after sintering process. LEO 440i Scanning Electron
Microscope (SEM) has been used to study the
morphology and distribution of the reinforcements in the
un-etched as well as etched composite samples. Flexural
strength of the composite and un-reinforced titanium
specimens in three point bending mode has been
determined. Vickers hardness of the composite and unreinforced titanium specimens using 5 kg load has been
measured. The elastic moduli of the composites and
unreinforced titanium specimens of 4 mm x 4 mm x 50
mm was studied by using dynamic methods based on
impulse excitation of vibrations (Buzz Mac. Intl. USA).

titanium powder and 2.4 m TiB2 powder (size ratio of

11.6:1) used by Sahay et al [3] has resulted in localized
increase in concentration of boron. In addition longer
duration required for completion of the reaction between
titanium and coarser B4C resulted in smaller mean free
path for the growth of primary needles, promoted the
growth of secondary TiB needles.

III. RESULTS & DISCUSSION

3.1 XRD & Microstructure
X-ray diffractogram of the pressureless sintered
composite and titanium samples is illustrated in Fig. 1.
Presence of Ti, TiB, TiC peaks and absence of B 4C peak
in Fig. 1 confirms completion of the reaction between
Ti-B4C during sintering. Highly exothermic reaction
(H298 = -754.36 kJ/mol) between the reactants helps in
completion of the reaction [6]. Fig. 2(a) shows the
SEM image of sintered titanium. Fig. 2(b) (10 vol.%
TiB+TiC) shows the presence of primary and secondary
needles of TiB distributed uniformly. The population
density of the TiB needles increased as seen in Fig. 2(c)
(20 vol.% TiB+TiC) with some amount of refinement in
the structure. Fig. 2(d) (30 vol.% TiB+TiC) illustrates
the presence of needle shaped randomly oriented TiB
whiskers in the titanium matrix and colonies of densely
packed short TiB whiskers. The short TiB whisker
colonies appear to be interconnected and uniformly
distributed in the matrix. The
needle shaped
morphology of TiB whiskers observed in the
microstructure has been explained in terms of crystal
structure and boron diffusion mechanism for TiB [2].
Sahay et al. [3] categorized such TiB needles with
different sizes as primary and secondary needles and
proposed a mechanism for formation of TiB in different
aspect ratios and diameters in terms of preferential
growth rate of TiB along [010] direction due to higher
density of strong B-B bonds and one way diffusion of B
along this direction. Sahay et al. proposed a critical
volume fraction of TiB2 (29 vol.%) above which thin
secondary needle shaped TiB starts growing. However,
secondary TiB needles were noticed even at 10 vol.% of
(TiB + TiC) reinforcements in the present study. Use of
finer (13 m) titanium powder and coarser (3 m) B 4C
powder in the present study in contrast to 28 m

Figure 1 : X-Ray diffraction patterns for both pressureless

sintered titanium and composite samples having different
vol.% of (TiB + TiC).

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content the flexural strength of the composites are

increasing. It is worth noting that the flexural strength of
the composite with 30 vol.% reinforcement is almost
double the strength of the unreinforced titanium.
Marginally lower flexural strength obtained for Ti-30
vol.% (TiB+TiC) composite (614 MPa) when compared
to
the flexural strength of hot pressed Ti-70%
(TiB+TiC) composite (629 MPa) reported elsewhere
[4], indicates that pressureless sintering process is
potential alternative method to VHP method for
synthesizing Titanium Matrix Composites. Similar trend
can also be observed in case of hardness of the
composites. Presence of TiB in the form of long single
crystalline whiskers or needles with clean interface is
responsible for the improved flexural strength and
hardness according to the theories of whisker induced
stiffening and strengthening [7].

TABLE 1: Mechanical properties of pressureless

sintered Ti (TiB+TiC) composites
Material

Titanium

Flexural
Strength
(MPa)
234

Vickers
Hardness
(VHN)
415

Ti-10% (TiB+TiC )

447

526

Ti-20% (TiB+TiC )

578

572

Ti-30% (TiB+TiC )

614

690

Elastic modulus measured for the composites by

pulse excitation technique are reported in Table 2.
Average elastic modulus of 131 GPa exhibited by the
sintered samples of unreinforced titanium in the present
study, is in between the elastic modulus values of 100
145 GPa reported for the transverse and longitudinal
directions of hexagonal close packed unit cell of high
purity titanium [8].

There is a gradual increase in the elastic modulus

values from 155 GPa to 188 GPa for composites with
increasing reinforcement content from 10 to 30
volume%. Elastic modulus values obtained in the
present study have been compared with those obtained
using different models as shown in the Fig. 3. While
calculating the elastic modulus values using various
models, elastic modulus of TiB has been assumed to be
482 GPa [9]. It has been observed that present values are
in between the values obtained by upper bound isostrain model and lower bound iso-stress model. The
observed values are matching with the values calculated
by Tsai-Halpin equation by assuming the aspect ratio of
(l/d) = 1. Whereas with the observed average aspect
ratio value of (l/d) = 10, the calculated elastic modulus
values are deviating from the observed values. This
indicates that even though most of the reinforcement

Figure 2 : SEM micrographs of the deep etched (a) Sintered

Titanium (b) Ti-10 vol. % (TiB + TiC) composite (c) Ti -20
vol.% (TiB + TiC) composite (d) Ti-30 vol.% (TiB + TiC)
composite

3.2 Mechanical Properties

Table 1 shows the mechanical properties of the
composites and unreinforced titanium samples
processed under similar conditions. Sintered sample of
unreinforced titanium exhibited average flexural
strength of 234 MPa. With increase in reinforcement

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needles have l/d ratio greater than critical l/d ratio

defined for effective load transfer, isotropic distribution
of the needles and their clusters are responsible for
obtaining lower Youngs modulus values than the
predicted values by the model. Moreover Tsai-Halpin
model is more valid for composites having uniformly
distributed reinforcements. Similar observations were
reported by Ranganath et al. [10], where variation in
Youngs modulus with volume fraction of TiB + Ti2C
reinforcements in titanium matrix has been studied.
Using the rule of mixtures for continuous
reinforcements, a large difference in the calculated
modulus values was observed for iso-strain and isostress models [10]. By using Tsai - Halpin equation for
discontinuous reinforcements it was shown that the
equation is valid for only particle aspect ratios nearing
unity. However, with particles having high aspect ratios
(l/d) of 10 20 the equation seems to be invalid, which
is in good agreement with the results obtained in the
present investigation

Elastic
Modulus
(GPa)

IsoStrain

Iso-Stress

(l/d)=10

10

155

166

141

150

162

20

172

201

153

172

195

30

188

236

167

196

228

2.

XRD studies confirmed the presence of TiB and

TiC reinforcements and absence of B4C in titanium
matrix indicating the completion of the in-situ
reaction between titanium and B4C.

4.

Sintered Ti TiB TiC composites exhibited

improved mechanical properties over sintered
titanium compacts processed under similar
conditions.
V. ACKNOWLEDGEMENTS

The Authors are thankful to Director, DMRL for

permitting to carryout the experimental work at DMRL.
We are also thankful to MBG, EMG and SFAG groups
of DMRL for carrying out mechanical testing, SEM and
XRD, respectively. We are grateful to Registrar, JNT
University, Hyderabad for his constant support and
encouragement.

Tsai- Halpin
(l/d)=1

Ti TiB TiC composites are processed using

titanium and B4C powders as raw materials by
pressureless sintering technique.

3. Microstructure of sintered Ti (TiB + TiC)

composites consists of primary and secondary
needles of TiB in the form of isolated needles, and
equiaxed TiC particles.

Table 2 : Elastic modulus values for composites

Vol.%

1.

VI. REFERENCES
1.

S.Ranganath, M. Vijayakumar, J. Subramanyam,

Combustion-assisted synthesis of Ti-TiB-TiC
composite via the casting route, Mater. Sci. Eng.
A.149, pp 253-257 (1992)

2.

K.B. Panda, K.S. Ravichandran, Synthesis of

Ductile TitaniumTitanium Boride (Ti-TiB)
Composites with a Beta- Titanium Matrix: The
Nature of TiB Formation and Composite
Properties,
Metallurgical
and
Materials
Transactions A,Vol.34A, pp1371-1385 (2003)

3.

S.S. Sahay, K.S. Ravichandran, R. Atri, Evolution

of microstructure and phases in in-situ processed
Ti-TiB composites containing high volume
fractions of TiB whiskers J.Mater.Res.; 14; pp
4214-4223 (1999)

4.

B.V. Radhakrishna Bhat, J. Subramanyam, V.V.

Bhanu Prasad, Preparation of Ti-TiB-TiC & TiTiB composites by in-situ reaction hot pressing,
Mater. Sci. & Eng. A Vol. 325, pp 126 -130 (2002)

5.

Z.Y. Ma, S.C. Tjong, L. Gen, In-situ Ti-TiB metalmatrix composite prepared by a reactive pressing
process, Scripta Materialia, Vol. 42, pp 367-373
(2000)

Figure 3 : The relation between reinforcement volume

fraction to the Elastic Modulus of the composites.
IV. CONCLUSIONS
The following conclusions emerge from the present
work

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6.

I. Barin, Thermochemical data of pure substances,

VcH Verlagsgesell Schaft mbH, D-6940,
Weinheim, Germany, Vol. 2, 931, (1993).

7.

K S. Ravichandran, and K. B. Panda, Titanium

Composites with TiB Whiskers
Advanced
Materials & Processes, pp 59-62 Oct. (2002)

8.

9.

S. Gorsse and D. B. Miracle,

Mechanical
properties of Ti-6Al-4V/TiB composites with
randomly
oriented
and
aligned
TiB
reinforcements, Acta Materialia, Vol. 51, pp
2427-2442 (2003)

10. S. Ranganath, A Review on Particulate-Reinforced

Titanium Matrix Composites, J. Mater Sci. Vol.
32, pp 1-16 (1997)

K. B. Panda and K. S. Ravi Chandran,

Determination of elastic constants of titanium
diboride (TiB2) from first principles using FLAPW
implementation of the density functional theory,
Comput Mater Sci. Vol. 35, pp 134-150 (2006)

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