Materials Science and Engineering A 534 (2012) 688–692

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Materials Science and Engineering A

journal homepage: www.elsevier.com/locate/msea

High temperature tensile properties of in situ TiBw/Ti6Al4V composites with a

novel network reinforcement architecture
L.J. Huang a , L. Geng a,∗ , H.X. Peng b , B. Kaveendran a
a
School of Materials Science and Engineering, Harbin Institute of Technology, P.O. Box 433, Harbin 150001, China
b
Advanced Composites Centre for Innovation and Science (ACCIS), Department of Aerospace Engineering, Bristol University, Bristol BS8 1TR, United Kingdom

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

Article history: TiB whisker reinforced Ti6Al4V (TiBw/Ti64) composites with a novel network reinforcement architecture
Received 3 May 2011 have emerged due to their superior combination of superior room temperature tensile properties. In the
Received in revised form 27 October 2011 present study, their superior high temperature tensile properties and special strengthening mechanisms
Accepted 9 December 2011
were further investigated. At 500 ◦ C, the tensile strength of the as-sintered 5 vol.%, 8.5 vol.% and 12 vol.%
Available online 16 December 2011
TiBw/Ti64 composites increased by 36.9%, 40.5% and 44.8% compared with that of the monolithic Ti64
alloy. Moreover, the tensile elongations are close to 10% at 500 ◦ C and 20% at 700 ◦ C. The maximum
Keywords:
service temperature of the TiBw/Ti64 composites can be increased to 600 ◦ C while retaining the strength
Titanium matrix composites (TMCs)
High temperature tensile property
of the monolithic Ti64 alloy the alloy at 400 ◦ C. This is attributed to the network boundary strengthening
Network microstructure mechanism as elucidated by the microstructure–property–fractographic analysis.
Branched whisker © 2011 Elsevier B.V. All rights reserved.
Network boundary strengthening

1. Introduction As a typical member of MMCs family, titanium matrix com-

Following the footsteps of conventional engineering alloys,
metal matrix composites (MMCs) have been always designed and
manufactured to possess a homogeneous distribution of reinforce-
ment [1–4]. Discontinuously reinforced metal matrix composites
(DRMMCs) with a homogeneous microstructure exhibit a certain
improvement in various properties in relative to their monolithic
matrix materials [5]. However, after much investigation conducted
by tailoring the composite microstructure of DRAMCs in the past
two decades, it becomes clear that a homogenous microstructure
can only exploit a limited strengthening effect of reinforcement;
the mechanical properties can be further improved by tailoring the
microstructure at a higher level [6,7]. Work reported by Lu [8] also
concluded that the strength to toughness ratios of composites can
be further enhanced by assembling metals with other components
in a controlled way to form a novel reinforcement or hierarchical
structure, compared with a conventional or homogeneous compos-
ite structure.
∗ Corresponding author. Tel.: +86 451 86418836; fax: +86 451 86413922.
E-mail addresses: ljhuanghit@yahoo.com.cn (L.J. Huang),
genglingroup@gmail.com (L. Geng).
posites (TMCs) offer a combination of good mechanical properties
and high temperature durability that render them attractive mate-
rials for automotive, aerospace and military applications [9–11].
Discontinuously reinforced titanium matrix composites (DRTMCs),
especially those fabricated by in situ methods such as powder met-
allurgy (PM) and melting techniques are sought-after because of
their superior isotropic properties and low cost [12–14]. How-
ever, irrespective of the processing methods used, the overall aim
has always been to trying to obtain a homogeneous microstruc-
ture [15,16]. The reality is that many TMCs with a homogeneous
microstructure exhibit a limited property improvement or even
inferior mechanical properties, such as extreme brittleness, par-
ticularly for TMCs fabricated by the conventional PM technique
[3,4,16–18].
One potential solution to this is to manipulate the DRTMCs
microstructure at a high level, such as a novel network microstruc-
ture created using a simplified PM technique [1,2]. This network
microstructure offers a combination of superior tensile strength
and ductility at room temperature [1,2]. Nevertheless, in many
industrial applications, high temperature tensile properties are
desirable for TMCs. Therefore, the unique microstructural char-
acteristics, high temperature tensile properties and strengthening
mechanisms of the superior TiBw/Ti64 composites with a network
microstructure are further investigated in this present work. It is

0921-5093/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2011.12.028
 L.J. Huang et al. / Materials Science and Engineering A 534 (2012) 688–692 689

Table 1
Chemical compositions of the composites and the monolithic Ti64 alloy (wt.%).

Material Al V B Fe Si O C N H Ti

Ti64 6.42 4.12 – 0.16 0.024 0.12 0.013 0.008 0.004 Bal.
V5D200 6.22 3.99 0.97 0.40 0.024 0.15 0.016 0.010 0.004 Bal.
V8D110 6.09 3.92 1.62 0.38 0.028 0.18 0.015 0.011 0.004 Bal.
V12D65 5.99 3.83 2.29 0.48 0.030 0.18 0.017 0.011 0.006 Bal.

found that the network boundary strengthening effect can be bet- Microstructural characterizations were performed using a scanning
ter exploited by introducing TiBw reinforcement into the network electron microscope (SEM, Hitachi S-4700).
boundary region, which overcomes the drawback of grain bound-
ary weakening effect at high temperatures observed in traditional
3. Results and discussions
engineering alloys.

3.1. Microstructural characteristics

2. Experimental procedure
As reported in [1,2], in order to fabricate TiBw/Ti64 compos-
ites with a network reinforcement architecture, large Ti64 powders
(D = 200 ␮m) fabricated by gas atomized process and fine TiB2
powders (3 ␮m) fabricated by self-propagating high-temperature
synthesis were selected and low-energy milled at a speed of
200 rpm for 8 h, instead of high-energy milling employed in con-
ventional PM processes. The milling processes were carried out
under a protective Argon atmosphere. Subsequently, the milled
mixtures were hot pressed in vacuum (10−2 Pa) at 1200 ◦ C under
a pressure of 20 MPa for 60 min. TiB whisker reinforcement were
in situ synthesized via the following reaction [5]:
Ti + TiB2 → 2TiB
In order to further investigate the unique microstructure,
three TiBw/Ti64 composites were fabricated in the present
study, namely, 5 vol.% TiBw/Ti64 (200 ␮m), 8.5 vol.% TiBw/Ti64
(110 ␮m) and 12 vol.% TiBw/Ti64 (65 ␮m), these composites were
denoted as V5D200, V8D110 and V12D65, respectively. In order
to demonstrate the advantages of the network microstructure, the
monolithic Ti64 alloy was also prepared using the same processing
parameters and raw material. The analyzed chemical compositions
of the prepared composites and the monolithic Ti64 alloy are given
in Table 1. As shown in the Table 1, with increasing volume fraction
of TiBw reinforcement, the overall contents of Al and V elements in
the composites are decreased; however, their local contents in the
matrix are increased [1].
High temperature tensile tests were carried out using
an Instron-1186 universal testing machine at a constant
crosshead speed of 0.5 mm/min (corresponding strain rate is
5.5 × 10−4 s−1 ). A total of five tensile specimens with dimen-
sions of 15 mm × 5 mm × 2 mm were tested for each composite.
Fig. 1 shows the OM micrographs of the monolithic Ti64 alloy
and the V5D200 composite. As shown in Fig. 1a, the typical wid-
manstätten microstructure is formed and the size of the primary ␤
grains is much larger (∼900 ␮m) than that of the as-received Ti64
powder. For the ␣ + ␤ or near ␣ two-phase Ti alloys, the formation of
the widmanstätten lamellar microstructure is common after cool-
ing from above the ␤ transus temperature, which is believed to be
harmful to the mechanical properties of titanium alloys [19]. The
formation of much large primary ␤ grains indicates that the loose
Ti64 powders merged during hot-press sintering process, and sub-
sequently the new primary ␤ grains were formed from the merged
␤ phase. It can be clearly seen from Fig. 1b that the synthesized
TiBw reinforcement is distributed around the deformed Ti64 parti-
(1) cles, forming a “grain boundary”-like structure with a “grain” size
of about 200 ␮m which is simply equal to the size of as-received
Ti64 particles. Due to the existence of the TiBw network, the coars-
ening of the primary ␤ grain is limited in the Ti64 matrix region
which are much smaller than the ␤ grain formed in the monolithic
alloy (Fig. 1a) [12]. It is worth pointing out that the primary ␤ grain
in the composites can be further decreased by selecting different
particle size of Ti64 powders, such as 110 ␮m and 65 ␮m.
Fig. 2 shows the SEM micrographs of TiBw/Ti64 composites with
a network microstructure at different magnifications and reveals
the following unique features.
(1) The overall network unit, as shown in Fig. 2a, can be divided
into a TiBw-rich network boundary region with a well defined
boundary width and a TiBw-lean matrix region [2]. This is to say,
the microstructure consists of a 3D continuous strong network
phase encapsulating a soft matrix phase. This structure effec-
tively corresponds to the well-known Hashin–Shtrikman (H–S)
upper bound [20,21] that can exploit a superior strengthening
effect.

Fig. 1. Optical micrographs of (a) the monolithic Ti64 alloy showing the typical widmanstätten microstructure and (b) the V5D200 composite showing a network microstruc-
ture.
690 L.J. Huang et al. / Materials Science and Engineering A 534 (2012) 688–692

Fig. 2. SEM micrographs of TiBw/Ti64 composite with a network microstructure at different magnifications revealing the network and TiB whisker morphologies. (a) Network
structure [2]. (b) Dowel structure and self-joining structure of TiBw. (c) Multibranched structure. (d) Mechanical locking, self-jointing structure and claw structure.

(2) The ␣ phase in the TiBw-lean region was refined and equiaxed
due to the limited primary ␤ grain and the constraint from
the stiff network boundary [1,22,23], which is expected to
improve the mechanical property of the matrix compared with
the widmanstätten lamellar microstructure of the monolithic
Ti64 alloy (Fig. 1a) [19].
(3) TiB whiskers grew into the neighboring Ti64 particles like
dowel connectors (Fig. 2b and c) owning to its special B27
structure [3,24], resulting in a strong and gradient boundary
connecting the neighboring Ti particles, which can be viewed
as a reinforced grain boundary.
(4) Many TiB whiskers are inter-connected by self-joining which is
equivalent to a longer effective length of TiBw (Fig. 2b).
(5) In Fig. 2c, TiBw with two hierarchical branches are discovered
for the first time, this is formed from the reaction with poly-
crystal TiB2 particles retained during the low-energy milling
process. In the meantime, TiB whisker cluster is formed due to
the relatively high local volume fraction of raw TiB2 materials
[25].
(6) In Fig. 2d, a single TiB whisker joins with a vertical one forming a
“T” junction. Unusually, the same TiB whisker also mechanically
locks with another vertical one in a different plane to construct
a three-dimensional (3D) spatial TiBw structure. A branched
“claw-like” TiBw structure is also observed in the Fig. 2d.
efficiency of TiB whiskers, in a similar way to that of multibranched
junctions of carbon nanotubes [27] and cross-linked fibers [25].
3.2. Tensile behavior and strengthening mechanisms
Fig. 3 shows the comparisons of high temperature tensile
strength, between the monolithic Ti64 alloy and the TiBw/Ti64
composites with a network reinforcement architecture. As
expected both the monolithic Ti64 alloy and the TiBw/Ti64 compos-
ites depict a decrease in tensile strength as the testing temperature
is increased from 400 ◦ C to 700 ◦ C, which is mainly caused by matrix
softening. By comparing the high temperature tensile strength of
the present TiBw/Ti64 composites with that of TiBw/Ti composites
[28], it can be concluded that the matrix property plays an impor-
tant role in determining the high temperature tensile strength of
the composites.
The high temperature tensile strength of the composites is
increased with increasing the volume fraction of reinforcement
[12] and decreasing Ti64 particle size. As shown in previous work

During the sintering process, the growing TiB whiskers fre-

quently encounter other whiskers due to the relatively high local
volume fraction of raw TiB2 particles in the boundary region. The
self-joining structure is formed when the crystal orientations of the
touching TiB whiskers are similar [25,26]. It has also been observed
that different crystal orientations can lead to the formation of a
mechanical locking structure as shown in Fig. 2d. The likely reason
for the formation of a claw-like structure is that different whiskers
simultaneously grow from one parent polycrystal TiB2 material
along different directions.
The above network structure, dowel-like structure, branch
structure, self-joining structure, mechanical locking and claw-
like structure collectively construct a unique 3D network which Fig. 3. Comparison of high temperature tensile strength between the TiBw/Ti64
is believed to be beneficial to further exploit the strengthening composites with network microstructure and the monolithic Ti64 alloy.
 L.J. Huang et al. / Materials Science and Engineering A 534 (2012) 688–692
Fig. 4. Comparison of high temperature tensile fracture elongation between the
TiBw/Ti64 composites with network microstructure and the monolithic Ti64 alloy.
[2], all the composites (V5D200, V8D110 and V12D65) possess
almost identical local volume fraction of reinforcement (18.1 vol.%,
18.8 vol.% and 18.0 vol.%) in the network boundary region, i.e.,
they have similar “grain boundary” region containing TiB whiskers.
That implies that, for the composites with network architecture,
decreasing the Ti64 particle size is equivalent to increasing the
total volume fraction of the network boundary region. Therefore,
the conventional ‘grain boundary strengthening mechanism’ in tra-
ditional alloy systems can operate. We denote this as ‘network
boundary strengthening mechanism’. It is worth pointing out that,
unlike the grain boundary weakening effect in traditional alloys
at elevated temperature, the network boundary containing TiB
whisker still plays an important strengthening effect even at much
higher temperatures.
Turning to the V5D200 composite, whose tensile strength
of 672 MPa, 517 MPa and 326 MPa at 500 ◦ C, 600 ◦ C and 700 ◦ C
increased by 36.9%, 36.1% and 27.3% compared with that of the
monolithic Ti64 alloy (491 MPa, 380 MPa and 256 MPa), respec-
tively. Thus, considering the modest 5 vol.% reinforcement and
comparing with the high temperature tensile strength of the
Fig. 5. High temperature tensile fractographs of 12 vol.% TiBw/Ti64 composite with a network microstructure at different temperatures. (a) 500 ◦ C, (b) 600 ◦ C, (c) 700 ◦ C.
691
composites with a homogeneous microstructure [29], the incre-
ment is rather significant. This improvement can be mainly
attributed to (i) the network architecture, (ii) a refined primary ␤
grain and (iii) the branched 3D TiBw structure. In addition, accord-
ing to Tamirisakandala’s work [30,31], it is likely that the increased
␤ transus accelerates the improvement of the tensile strength.
All the composites with a network microstructure exhibit supe-
rior high temperature strength which justifies the effort in tailoring
the reinforcement architecture for improved high temperature ten-
sile strength of the composites. A similar trend is found in Sen’s
work [12]. It should be noted that the strengthening efficiency
decreases with increasing the testing temperature, especially at
700 ◦ C where it decreases sharply, this is most likely because of the
profound softening of the matrix alloy. Based on the same strength
level, the maximum service temperature of the present composites
is increased to 600 ◦ C from 400 ◦ C of the monolithic Ti64 alloy.
Fig. 4 shows the high temperature tensile fracture elongations of
as-sintered composites and the monolithic Ti64 alloy. Firstly, the
elongations of the composites are always lower than that of the
monolithic Ti64 alloy due to the introduction of TiBw reinforce-
ment. Secondly, the elongation decreases with increasing volume
fraction of TiBw reinforcement, which can be attributed to the
increasing volume fraction of TiBw reinforcement and the decreas-
ing particle size of Ti64 alloy matrix. Thirdly, at relatively higher
testing temperature, the elongations of the composites are closer
to that of Ti64 alloy due to the matrix softening (Fig. 3). It is worth
noting that an elongation close to 10% at 500 ◦ C and over 15% at
700 ◦ C is still remarkable and that the elongation of all the compos-
ites and Ti64 alloy can be further enhanced by the subsequent hot
deformation, such as hot extrusion or forging.
Fig. 5 shows typical fractographs of the V12D65 composite at dif-
ferent temperatures. It can be seen from Fig. 5a and b that the main
crack still follows the network boundaries, i.e., fracture occurred
through the TiBw-rich boundary. The rather rough fracture surface
indicates a torturous crack propagation path due to the network
architecture, which is similar to the room temperature fracture
features [2]. However, a different fracture feature is observed on
the fracture surface as seen from Fig. 5c, the large matrix parti-
cle tears, which demonstrates different toughening mechanism. On
the one hand, this phenomenon indicates that the network bound-
ary strengthening effect still remains; while on the other hand, this
692 L.J. Huang et al. / Materials Science and Engineering A 534 (2012) 688–692
strengthening effect remarkably decreases due to similar transcrys-
talline fracture at 700 ◦ C. This is in consistent with the observed
sharp decrease of strength and the sharp increase of elongation at
700 ◦ C.
4. Conclusions
TiBw/Ti64 composites with network reinforcement architec-
ture have been fabricated and evaluated focusing on their high
temperature tensile properties. This work has led to the following
conclusions:
(1) The branched structure and the network distribution of TiBw
reinforcement formed during the low energy milling process
are beneficial to its strengthening efficiency. This has led to the
superior high temperature tensile properties.
(2) At 500 ◦ C, the tensile strength of the composites is increased by
up to 44.8% in relative to the monolithic matrix alloy. This is
largely attributed to the effective network boundary strength-
ening mechanism.
(3) The maximum service temperature of the TiBw/Ti64 compos-
ites can be increased to 600 ◦ C while retaining the same strength
of the monolithic Ti64 alloy at 400 ◦ C.
Due to its superior combination of strengthening and tough-
ening effects at room and high temperatures, the novel network
reinforcement architecture is likely to prevail in the field of
MMCs.
Acknowledgements
This work is financially supported by the National Natural Sci-
ence Foundation of China (NSFC) under grant no. 51101042, the
Fundamental Research Funds for the Central Universities under
grant no. HIT. NSRIF. 201131, the 50th-class General Financial Grant
from the China Postdoctoral Science Foundation under grant no.
2011M500653 and the Royal Society (RS)-NSFC International Joint
Project under grant no. 51011130206. Huang was supported to
study at the University of Bristol for one year through the China
Scholarship Council (CSC). HXP is a Visiting Professor of Harbin
Institute of Technology, Harbin, PR China.
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