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Synthesis and characterization of in situ

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DOI: 10.1016/j.matdes.2012.08.008

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Materials and Design 44 (2013) 438445

Contents lists available at SciVerse ScienceDirect

Materials and Design

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

Synthesis and characterization of in situ formed titanium diboride particulate

reinforced AA7075 aluminum alloy cast composites
H.B. Michael Rajan a,, S. Ramabalan b, I. Dinaharan c, S.J. Vijay c
a
Department of Mechanical Engineering, St. Josephs College of Engineering and Technology, Thanjavur 613 403, Tamil Nadu, India
b
EGS Pillay Engineering College, Nagapattinam 611 002, Tamil Nadu, India
c
School of Mechanical Sciences, Karunya University, Coimbatore 641 114, Tamil Nadu, India

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

Article history: In situ fabrication of aluminum matrix composites (AMCs) has gathered widespread attention of
Received 9 July 2012 researchers due to inherent advantages over ex situ methods. Aluminum alloy AA7075 reinforced with
Accepted 8 August 2012 various amounts (0, 3, 6 and 9 wt.%) of TiB2 particles were prepared by the in situ reaction of inorganic
Available online 25 August 2012
salts such as K2TiF6 and KBF4 to molten aluminum. X-ray diffraction patterns of the prepared AMCs
clearly revealed the formation of TiB2 particles without the presence of any other intermetallic com-
Keywords: pounds. The microstructures of the AMCs were studied using optical and scanning electron microscopy.
A. Metalmatrix composites
The in situ formed TiB2 particles were characterized with uniform distribution, clear interface, good
C. Casting
E. Mechanical properties
bonding and various shapes such as cubic, spherical and hexagonal. The formation of TiB2 particles
F. Microstructure enhanced the microhardness and ultimate tensile strength (UTS) of the AMCs.
2012 Elsevier Ltd. All rights reserved.

1. Introduction
Aluminum metal matrix composites (AMCs) emerged from the
perpetual need for lighter weight, higher performance components
in aerospace, aircraft and automotive industries. AMCs are progres-
sively replacing conventional aluminum alloys in many applica-
tions due to superior properties including high wear resistance,
low thermal expansion, high strength to weight ratio, etc. [13].
The ceramic particles SiC and Al2O3 were extensively used as rein-
forcements over a long period since the inception of AMCs. The
advancement of fabrication methods led to the incorporation of
several kinds of potential ceramic particles such as fly ash [4],
SiO2 [5], TiO2 [6], AlN [7], Si3N4 [8], TiC [9], B4C [10], TiB2 [11]
and ZrB2 [12] into the aluminum matrix to prepare AMCs.
The AMCs reinforced with ceramic particles are currently fabri-
cated using various established methods and some specific pat-
ented methods. The conventional methods are powder
metallurgy [13], mechanical alloying [14], stir casting [7,8],
squeeze casting [15], compo casting [16] and spray deposition
[17]. The processing method influences the mechanical behavior
of the AMCs. The successful incorporation of ceramic particles into
the matrix alloy and achieving good bonding between them will
Corresponding author. Mobile: +91 9245664761; fax: +91 4362 282471.
E-mail addresses: hbmichaelrajan@gmail.com, hodmech@sjcet.tnj.edu.in (H.B.
Michael Rajan), principal.egspec@gmail.com, sramabalan@egspec.edu.in (S. Rama-
balan), dinaweld2009@gmail.com, issacdinaharan@karunya.edu (I. Dinaharan),
vijayjoseph.2001@gmail.com, vijayjoseph@karunya.edu (S.J. Vijay).
help to enhance the properties. All processing methods are classi-
fied into two categories which are namely solid state processing
and liquid state processing. Each process has a limitation to pro-
duce AMCs with certain combinations of matrix alloy and ceramic
particles. Therefore lot of research emphasis is given to develop the
processing methods to fabricate AMCs. Liquid method of process-
ing is effective owing to its simplicity, easy of adaption, and appli-
cability to large quantity fabrication. Liquid method of processing
involves either adding ceramic particles externally to the molten
metal or synthesizing in the melt itself. The former is known as
ex situ fabrication while the later is called as in situ fabrication
[18]. The advantages of in situ fabrication includes fine size of cera-
mic particles, good interfacial bonding strength, uniform distribu-
tion of particles, thermodynamically stable particles and low cost
of processing [19,20].
Some studies on aluminum alloy reinforced in situ formed TiB2
particles were reported in the literatures [2130]. Han et al. [21]
prepared Al/TiB2 AMC by the in situ reaction of K2TiF6 and KBF4
to molten aluminum and found uniform distribution of TiB2 parti-
cles in the eutectic structure. Emamy et al. [22] developed Al/TiB2
AMC by the in situ reaction of Al8Ti and Al4B mater alloys and
explained the formation mechanism of TiB2 particles. Wang et al.
[23] produced Al/TiB2 AMC by the in situ reaction of Al4B mater
alloy and electrolytic low titanium aluminum and explained the
grain refinement behavior of TiB2 particles. Zhao et al. [24] pre-
pared Al/(TiB2 + Al2O3) hybrid AMC by the in situ reaction of
K2TiF6, KBF4 and CuO to molten aluminum and observed the distri-
bution of TiB2 particles along the grain boundaries interweaved

0261-3069/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2012.08.008
 Author's personal copy

H.B. Michael Rajan et al. / Materials and Design 44 (2013) 438445 439

with CuAl2 phase. Kumar et al. [25] synthesized Al7Si/TiB2 AMC Table 2
by the in situ reaction of K2TiF6 and KBF4 to molten aluminum The amount of salts added to molten aluminum.

and reported significant improvement in tensile strength and wear TiB2 (wt.%) 0 3 6 9
resistance of the AMCs in comparison to the base alloy. Ramesh K2TiF6 (g) 0 107 220 342
et al. [26,27] fabricated AA6063/TiB2 AMC by the in situ reaction KBF4 (g) 0 135 278 430

of Al10Ti and Al3B mater alloys and studied the effect of various
stoichiometric ratios of mater alloys on the formation and mechan-
ical properties of the AMCs. Mallikarjuna et al. [28] employed exo-
thermic reaction process using K2TiF6 and KBF4 salts to produce
AA2014/TiB2 AMC and investigated the effect of reaction time on
the grain size and wear rate of the AMCs. Xue et al. [29] reported
that the addition of CeO2 to the in situ reaction of K2TiF6 and
KBF4 lead to improved distribution of TiB2 particles and property
enhancement of Al/TiB2 AMC. Li et al. [30] developed Al/TiB2
AMC by the in situ reaction of Ti sponge and Al3B mater alloy
and analyzed the orientation relationships between Al and TiB2
using an edge-to-edge matching model .
In this work, an attempt is made to fabricate aluminum alloy
AA7075 reinforced with TiB2 particles by the in situ reaction of
K2TiF6 and KBF4 salts to molten aluminum and study the effect of
TiB2 content on microstructure and mechanical properties of Fig. 1. Stir casting facility.
AA7075/TiB2 AMCs. Aluminum alloy AA7075 (AlZnMgCu) is
one of the strongest aluminum alloys in industrial use today due
to high strength to weight ratio and natural aging characteristics. 3. Results and discussions
The alloy derives its strength from precipitation of Mg2Zn and Al2-
CuMg phases [31]. Among various ceramic reinforcements, TiB2 is a 3.1. X-ray diffraction analysis of AA7075/TiB2 AMCs
promising candidate for AMCs due to several desirable properties.
TiB2 is a refractory compound which exhibits excellent features Aluminum alloy AA7075 reinforced TiB2 particulate composites
such as high melting point, high hardness and high modulus char- were successfully synthesized by the in situ reaction of K2TiF6 and
acteristics. TiB2 does not react with aluminum to form reaction KBF4 salts to molten aluminum. The XRD patterns of the prepared
product at the interface of reinforcement and matrix [32]. composites are shown in Fig. 2. The diffraction peaks of TiB2 parti-
cles are clearly seen and the intensity of the peaks increases as TiB2
content is increased. The in situ reactions as given in the following
2. Experimental procedure equations resulted in the formation of TiB2 particles. It is also ob-
served in Fig. 2 that the peaks of aluminum in the composites
AA7075 rods were placed in a coated graphite crucible and are slightly shifted to higher 2h compared to that of aluminum
heated using an electrical furnace. The chemical composition of due to the formation of TiB2 phase in the aluminum matrix.
AA7075 aluminum alloy is presented in Table 1. A coating was ap-
plied inside the crucible to avoid contamination. The measured K2 TiF6 13=3Al ! Al3 Ti 4=3AlF3 2KF 1
quantities of inorganic salts K2TiF6 and KBF4 as given in Table 2
were added into the molten aluminum to produce TiB2. The tem-
perature of the molten aluminum was maintained at 850 C which 2KBF4 3Al ! AlB2 2AlF3 2KF 2
was stirred intermittently for 40 min. The composite melt was
poured into a preheated die after the removal of slag. Castings
were taken with various amounts of (0, 3, 6 and 9 wt.%) of TiB2 par- Al3 Ti AlB2 ! TiB2 4Al 3
ticles. The experimental set up is shown in Fig. 1. The sequence of TiB2 formation can be summarized as follows
Specimens were prepared from the castings to carry out [22,27]:
microstructure and mechanical characterization. The specimens
were polished using standard metallographic technique and
etched with Kellers reagent. The etched specimens were ob-
served using an optical microscope and a scanning electron
microscope (SEM). X-ray diffraction patterns (XRD) were re-
corded using Panalytical X-ray diffractometer. The microhardness
was measured using a microhardness tester at 500 g load ap-
plied for 15 s. The tensile specimens were prepared as per ASTM
E8M-04 standard [33] having a gauge length of 40 mm, a gauge
width of 7 mm and a thickness of 6 mm. The ultimate tensile
strength (UTS) was estimated using a computerized universal
testing machine. The fracture surfaces of the failed tensile spec-
imens were observed using SEM.

Table 1
Chemical composition of AA7075 aluminum alloy.

Element Si Fe Cu Mn Mg Cr Ni Zn Ti Zr Al
wt.% 0.10 0.23 1.48 0.07 2.11 0.22 0.01 5.29 0.07 0.02 Balance
Fig. 2. XRD patterns of AA7075/TiB2 in situ composites.
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440 H.B. Michael Rajan et al. / Materials and Design 44 (2013) 438445
Fig. 3. Optical micrographs of AA7075/TiB2 in situ composites containing TiB2: (a) 0 wt.%, (b) 3 wt.%, (c) 6 wt.% and (d) 9 wt.%.
 The introduction of K2TiF6 and KBF4 to molten aluminum forms
intermetallic compounds namely Al3Ti and AlB2 respectively
which act as source for Ti and B atoms.
 Boron atoms move towards Al3Ti particles.
 Reaction takes place between Ti and B atoms in a gap from Al3Ti
surface to form TiB2.
 Owing to smaller size, boron atoms start diffuse through TiB2
particles.
 Dissolution of Al3Ti particles due to natural cracking and frag-
mentation of Al3Ti particles which lead to increased rate of
TiB2 formation.
 Formation of TiB2 particles after complete reaction.
It is evident from Fig. 2 that there is no trace of Al3Ti or AlB2
which indicates that the reaction is complete. Sufficient holding
time and proper mole ratio of inorganic salts are required for com-
plete reaction [34]. Though the furnace temperature was set to
850 C, the local melt temperature increases to 900920 C be-
cause of the exothermic nature of the in situ reaction. It is possible
to encounter the loss of boron atoms in AlB2 at high temperature.
Therefore, KBF4 was added 20% in excess of the theoretical mole ra-
tio in the present work. Insufficient boron atoms will make the
reaction (3) incomplete leaving brittle Al3Ti in the composite. Ab-
sence of Al3Ti peaks in Fig. 2 further indicates that the in situ
formed TiB2 particles are in equilibrium with molten aluminum
and thermodynamically stable. The in situ formed TiB2 particles
do not decompose to form any other compounds. The interface be-
tween aluminum alloy and TiB2 particles tends to be free when no
other compounds are present.
3.2. Microstructure of AA7075/TiB2 AMCs
The optical photomicrographs of the fabricated AMCs are
shown in Fig. 3. The optical photomicrograph of as cast AA7075
is revealed in Fig. 3a. The microstructure is composed of solidifica-
tion induced dendritic structure. The high rate of cooling known as
super cooling during solidification formed such a structure. The
dendritic structure exhibits elongated primary a-Al dendritic arms
having high aspect ratio. The average spacing between dendritic
arms is measured to be around 4050 lm. The alloying elements
of AA7075 such as Zn and Mg are noted to be higher than that of
their solubility limit. As a result the intermetallic phases like
MgZn2, MgZn, AlZn, Al2CuMg and Al2Mg3 etc. are formed around
the dendrites during casting.
The optical photomicrographs of AA7075 reinforced in situ
formed TiB2 particles are revealed in Fig. 3bd. The grain refining
action of TiB2 particles is clearly seen. As the amount of TiB2 parti-
cles increases the grain size reduces. TiB2 particles entirely modi-
fied the dendritic structure of as cast AA7075. The grain
refinement can be attributed to the following two causes. The a-
Al experiences resistance to growth due to in situ formed TiB2 par-
ticles during the solidification process. The aluminum grains solid-
ify on TiB2 particles which act as a nucleus. The overall
microstructure can be thought of as islands of soft aluminum ma-
trix surrounded by hard TiB2 particles region. It is further evident
from Fig. 3 that the grain size of AA7075/TiB2 AMC reduces when
weight percentage of TiB2 particles is increased. As weight percent-
age of TiB2 particles increases, the number of TiB2 particles in-
crease. More nucleation sites are created when the number of
TiB2 particles increases due to constitutional under cooling zone
in front of the particles. Increased number of particles offers en-
hanced resistance to the grain growth of aluminum matrix result-
ing in grain refinement.
It can be seen from Fig. 3 that most of the TiB2 particles are lo-
cated in inter granular regions. The distribution of TiB2 particles in
the melt is influenced by convection current in the melt, move-
ment of the solidification front against particles and buoyant mo-
tion of particles [35]. The velocity of the solidification front
 Author's personal copy
H.B. Michael Rajan et al. / Materials and Design 44 (2013) 438445
influences the particle to be distributed in intra or inter granular
regions. When the velocity of the solidification front is below a
critical velocity, the particles are pushed by the solidification front
leading to inter granular distribution and vice versa. The critical
velocity is a function of the particle size and the temperature gra-
dient. Observing the TiB2 particle distribution it appears that the
particles are pushed by the solidification front leading to inter
granular regions.
The SEM micrographs of the fabricated AMCs are presented in
Fig. 4. The micrographs show no common casting defects such as
porosity, shrinkages or slag inclusion which showcases the quality
of castings. The in situ formed TiB2 particles are distributed nearly
homogeneously in the aluminum matrix. Such kind of particulate
distribution is an essential requirement to achieve better mechan-
ical properties of the AMCs. The solidification process dictates the
distribution of TiB2 particles in the aluminum matrix. The density
variation between the matrix material and ceramic particle play
Fig. 4. SEM micrographs of AA7075/TiB2 in situ composites at lower magnification containing TiB2: (a) 3 wt.%, (b) 6 wt.% and (c) 9 wt.%.
441
a crucial role during solidification. It is a well known fact when
the density of ceramic particle is higher compared to matrix mate-
rial, it starts to sink in the molten matrix. The ceramic particle
should suspend in the molten matrix for a long time to obtain
homogenous distribution. It is reported that if the density variation
between matrix and ceramic particle is more than 2 g/cm3, the
ceramic particle can suspend for a long time in the melt [21]. In
our present work, the density variation between aluminum matrix
and TiB2 particle is nearly 2 kg/cm3. Therefore, the sinking rate of
in situ formed TiB2 particles is negligible and TiB2 particles sus-
pend in the melt for a long time. On the other hand, the wetting ac-
tion between molten aluminum and TiB2 particles offers resistance
to the free movement of TiB2 particles. The above said factors lead
to a better distribution of TiB2 particles.
The SEM micrographs of the fabricated AMCs at higher magni-
fication are presented in Fig. 5. The in situ formed TiB2 particles ex-
hibit various shapes such as spherical, hexagonal and cubic. Some
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442 H.B. Michael Rajan et al. / Materials and Design 44 (2013) 438445

Fig. 5. SEM micrographs of AA7075/TiB2 in situ composites at higher magnification containing TiB2: (a) 3 wt.%, (b) 6 wt.% and (c) 9 wt.%.

investigators observed the shape of TiB2 particles to be hexagonal

[2527,32] while some other reported spherical and cubic struc-
ture [21,29,30]. It is evident from Fig. 5a and b that the interface
between the TiB2 particles and the matrix is clean and well bonded
to matrix alloy. The presence of clear interface can be attributed to
the formation of particles within the melt itself and thermody-
namic stability of the TiB2 particles. When a ceramic particle be-
haves thermodynamically unstable in the aluminum melt, it
produces undesirable compounds at the particle to matrix inter-
face [7,36]. A pure interface is needed to increase the load bearing
capability of the AMCs and enhance the mechanical and tribologi-
cal properties. The increase in local melt temperature due to the
in situ reaction causes good bonding between the TiB2 particle
and the matrix. Fine size of TiB2 particles is seen in Fig. 5. The aver-
age size of TiB2 particle was measured to be less than 2 lm. Chen
et al. [37] reported that TiB2 particle has high nucleation rate and
sluggish growth kinetics which results in fine size of particles. Fig. 6. Effect of TiB2 content on microhardness of AA7075/TiB2 in situ composites.
 Author's personal copy

H.B. Michael Rajan et al. / Materials and Design 44 (2013) 438445 443

Fig. 7. Effect of TiB2 content on: (a) tensile strength and (b) elongation of AA7075/TiB2 in situ composites.

Fig. 8. Fracture morphology of AA7075/TiB2 in situ composites containing TiB2: (a) 0 wt.%, (b) 3 wt.%, (c) 6 wt.%, (d) 9 wt.% and (e) 9 wt.%.

The SEM micrographs of the AMCs as shown in Fig. 4 consist of 9 wt.% TiB2 AMC is presented in Fig. 5c. Most of the particles in
both uniformly distributed single TiB2 particles as well as TiB2 clus- the cluster are sub-micron in size. Several ultrafine particles also
ters. A magnified view of a single cluster observed in AA7075/ can be observed. The behavior of clusters formed during in situ
 Author's personal copy
444 H.B. Michael Rajan et al. / Materials and Design 44 (2013) 438445
reaction is different to those clusters commonly present in ex situ
composites. When particles are added externally, clusters are
formed due to several factors including poor wettability, insuffi-
cient stirring and density variation between the matrix alloy and
ceramic particle. Further, local melt temperature drops as particles
are added externally. The bonding between particles in clusters is
weak which leads to poor mechanical properties [38]. But particles
in clusters formed by in situ reaction exhibit good bonding. The
exothermal in situ reaction creates good bonding between parti-
cles in clusters.
3.3. Mechanical properties of AA7075/TiB2 AMCs
The effect of weight percentage of in situ formed TiB2 particles
on micro hardness and UTS is respectively presented in Figs. 6 and
7. In situ formed TiB2 particles considerably enhance the micro
hardness and UTS of AA7075/TiB2 AMCs. The strengthening of
AA7075 by in situ formed TiB2 particles can be explained as fol-
lows. When the AMC bear a load, the interaction between disloca-
tions and TiB2 particles resist the propagation of cracks. During
solidification of the AMC, strain fields are created around TiB2 par-
ticles due to the difference of the thermal expansion coefficient be-
tween the aluminum alloy and TiB2 particle. The in situ process
generates defect free TiB2 particles which preserve their integrity
during tensile loading. TiB2 particle refines the grains of aluminum
alloy which provides more area to resist the load. The homoge-
neous distribution of TiB2 particles provides Orowan strengthening
[39]. The clear interface and good bonding delay the detachment of
particles from the aluminum matrix. Hence, the microhardness
and UTS of AMC are enhanced by TiB2 particles. More the weight
percentage of TiB2, more will be the effect of the above factors
which further increases the mechanical properties. As shown in
Fig. 4b, the elongation of the AMCs drops when TiB2 particle weight
percentage is increased. Similar results were reported by Han et al.
[21]. The grain refinement and reduction of ductile matrix content
when the weight percentage of TiB2 particles are increased reduces
the ductility of the AMCs.
The fracture morphology of the tensile tested specimens of
AA7075/TiB2 AMCs are presented in Fig. 8. The fracture morphol-
ogy of the matrix alloy AA7075 in Fig. 8a shows larger and uni-
formly distributed voids which indicate ductile fracture. The
fracture morphology of the developed AA7075/TiB2 AMCs
(Fig. 8bd) show smaller size voids compared to that of matrix al-
loy which indicate macroscopically brittle fracture and microscop-
ically ductile fracture. The in situ formed TiB2 particles refined the
grain size of aluminum alloy and reduced the ductility which re-
sulted in smaller size voids. The ductile shear bands in the fracture
morphology indicate that some amount of ductility is retained by
the AMC. The magnified view of the fracture morphology of
AA7075/9 wt.% TiB2 AMC is shown in Fig. 8e. TiB2 particles remain
intact in several places which gives evidence to the existence of
good bonding between the aluminum matrix and in situ formed
TiB2 particles.
4. Conclusions
AA7075/TiB2 AMCs were successfully synthesized by the in situ
reaction of inorganic salts such as K2TiF6 and KBF4 to molten alu-
minum. The in situ reaction resulted in the formation of TiB2 par-
ticles. No other intermetallic compounds in significant quantity
were detected. Most of the TiB2 particles were located in inter
granular regions. The microstructures of the developed AMCs re-
vealed a uniform distribution of TiB2 particles having clear inter-
face and good bonding. The in situ formed TiB2 particles
displayed various shapes such as cubic, spherical and hexagonal.
The mechanical properties of the AMCs improved when the con-
tent of TiB2 particles was increased.
Acknowledgements
The authors are grateful to the Department of Mechanical Engi-
neering, Karunya University, Coimbatore, India for providing the
facilities. One of the authors, Mr. I. Dinaharan acknowledges
Department of Science and Technology, Govt. of India for providing
INSPIRE fellowship. The authors are also thankful to Mr. T. Mukilan,
Mr. T.A.S. Nirmal, Mr. U. Sethusudhan and Mr. C. John Kennedy for
their assistance offered to execute the above work.
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