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Advanced Materials Research Vol.

1042 (2014) pp 58-64

(2014) Trans Tech Publications, Switzerland

Submitted: 14.08.2014
Accepted: 14.08.2014

Ultrasonic Cavitation Based Processing of Metal Matrix

Nanocomposites: An Overview
Santanu Sardar1, a, Santanu Kumar Karmakar1,b and Debdulal Das2,c

Department of Mechanical Engineering, Indian Institute of Engineering Science and Technology,

Shibpur, Howrah 711103, West Bengal, India

Department of Metallurgy and Materials Engineering, Indian Institute of Engineering Science and
Technology, Shibpur, Howrah 711103, West Bengal, India

Keywords: Nanocomposite, metal matrix composite, ultrasonic

dispersion, casting, microstructure, mechanical property.

cavitation, nanoparticle,

Abstract. Metal matrix nanocomposites (MMNCs) have emerged as an important class of materials
for structural applications specifically in the automobile and aerospace sectors; however,
development of cost effective mass production technique of MMNCs with requisite operational and
geometrical flexibilities is still a great challenge. Focused research in the last decade has
highlighted that ultrasonic cavitation based processing is the most promising method for
manufacturing of MMNCs with nearly uniform distribution of nanoparticles, having added
advantage of being a liquid-phase route. This article presents an overview on the basic principles
and recent advances in the ultrasonic cavitation based processing of MMNCs with a particular
emphasis on identifying relationships amongst processing variables, microstructural parameters and
mechanical properties. Critical issues of MMNCs fabrication are discussed.
Metal matrix composites (MMCs) are advanced hybrid materials in which tailored properties such
as excellent strength-to-weight ratio, which is not easily attainable in base materials, are realized by
utilizing the better ductility and toughness of the metal/alloy matrix in presence of higher modulus
and hardness of ceramic reinforcement [1,2]. In order to achieve substantial improvement of
strength, conventional MMCs are generally reinforced with 15-60 vol.% of micron-sized Al2O3/SiC
particles [3]. Such high concentration of reinforcement, however, markedly reduces the ductility of
MMCs and hence, limits their widespread application [4,5]. Similar level of strength can be
achieved with much lower concentration of reinforcement (say, 1-5 vol.%) if the size of the ceramic
particles is reduced to the nanometer scale (typically less than 100 nm) as the nanoparticles more
effectively promote particle hardening mechanisms than the micron-sized particles [5-8]. For
example, tensile strength of an Al-1 vol.% Si3N4 (10 nm) composite has been found to be
comparable to that of an Al-15 vol.% SiC (3.5 m) composite [1]. Since, metal matrix
nanocomposites (MMNCs) require less amount of reinforcement; these are expected to exhibit
higher ductility and formability as compared to the micron-sized MMCs [9]. For Mg-SiC
microcomposite (25 m, 10 vol.%) and nanocomposite (50 nm, 1.1 vol.%), Wong et al. [10] have
shown that the tensile strength of the nanocomposite i.e. 203 MPa is not only higher than that of the
microcomposite i.e. 165 MPa, but also the total elongation of the former i.e. 7.6% is significantly
higher than of the latter i.e.1.5%. Therefore, significant efforts have been directed in recent years to
develop MMNCs considering their enormous potential for application in aerospace, automobile and
military industries.
Development of structural components of MMNCs remains great technological challenges. The
common processing technologies are neither reliable nor cost effective to enable mass production of
complex MMNC components with reproducible microstructures and properties [2,11].
Manufacturing of nanocomposites in comparable with microcomposites can also be divided into
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Advanced Materials Research Vol. 1042

two general categories: solid-state and liquid-state. Amongst the solid-state techniques, powder
metallurgy and mechanical milling are the most popular ones and capable to generate uniform nanoscale structure [12]. However, these techniques are very costly and require extensive post
processing. In addition, these methods are also limited to simpler shapes with smaller sizes which
are often inadequate for structural application [1,2]. Amongst the liquid phase techniques, stir
casting method is the most economical one. It has been widely used for near-net-shape processing
of MMCs [6]. Being liquid-phase, this route offers better matrix-particle bonding, easier control of
matrix structure, simplicity in production, vivid selection of materials, flexibility and applicability
to large quantity production of structural components of complex geometry [2,13]. Nearly uniform
dispersion of micron-sized particles is easily achieved by mechanical stirring arrangement in the stir
casting method [2]. However, the similar stirring arrangement fails to disperse nanoparticles even in
small quantity in the liquid metal because of their large surface-to-volume ratio and poor wettability
in melts [6,7,14]. Moreover, the force generated by mechanical stirring is insufficient to break
nanoparticle agglomerates generated due to strong Van der Waals attractive force [1,9,11,15]. In
this regard, it has been observed in the last decade that ultrasonic cavitation based (UTCB) is the
most effective technique to overcome the common problems relating to dispersion of nanoparticles
in the liquid metal. In recent times, UTCB processing has emerged as the most promising method
for cost effective mass production of MMNCs mainly due to the pioneering works by Li and coworkers [2,7,8,11,16]. They have successfully synthesized several high-performance nano Al2O3
[14,17,18] / SiC [2,4,16,19,20] particle reinforced Al [7,11,17,18] and Mg [2,4,6,19-21] matrix
composites by UTCB method. This article presents the state-of-the-art of UTCB technique for
manufacturing of MMNCs.
Ultrasonic Cavitation based Manufacturing
of MMNCs
A General Setup

power supply
Ultrasonic generator



Two types of UTCB systems have been used till
date for manufacturing of MMNCs, these are
contact [2,6,20] and noncontact-type [15]. In Inert gas
case of contact-type, the ultrasonic probe is
dipped into the liquid melt that directly aids to NanoUltrasonic
disperse the nanoparticles in the melt and the particles
developed slurry is subsequently solidified by
conventional route. Whereas for noncontact- Crucible
type, solidification of liquid melt with added
nanoparticles is performed in an ultrasonic Molten
chamber [15]. The contact-type system is the metal
most preferred one considering its simplicity in Furnace
operation and effectiveness to disperse
nanoparticles in melt. Typical contact-type Fig. 1. Schematic presentation of basic set-up
UTCB system is schematically illustrated in used in ultrasonic cavitation based method.
Fig. 1. In general, it consists of an electric
resistance heating furnace for melting light metals/alloys in graphite [6,11,17,22] or steel [4,5]
crucible, nanoparticle feeding system, ultrasonic wave generator with probe and inert gas, like
argon [2,11,14,18] or CO2+ SF6 [4-6,21] purging arrangements. The ultrasonic probe made of
titanium [6,7,13,16] or niobium [4,11,17] alloy is activated by a transducer based on either of the
permendur magnetostrictive alloy [4,11,20] or the piezoelectric [13]. The transducer converts high
power electrical energy to mechanical motion and generates power varying from 450W [21] to 4kW
[11] with frequency ranging from 17.5 kHz [4,11,20] to 20 kHz [5-7,14,23]. In general, loose
nanoparticles are added in the melt, however, Choi et al. [17,18] have introduced a double-capsule
feeding method where the nanoparticles are first wrapped with a thin Al foil and then encapsulated


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in an Al tube. The Al tube is then slowly fed into the melt. Nie et al. [24] have preferred feeding of
preheated nanoparticles into the liquid melt to enhance their wettability with the molten metal. In
order to enhance the dispersion of nanoparticles and to minimize their segregation during
solidification, a few researchers [21,24] have attempted addition of nanoparticles in the semi-solid
state over fully liquid state.
Basic Principle
The UTCB processing involves mainly two important phenomena, i.e., transient cavitation and
acoustic streaming [6,7,19]. The acoustic cavitation is initiated by the high-intensity ultrasonic
waves (above 25W/cm2) that generate strong non-linear effects in liquid [1,2,6]. The effect of such
cavitation includes the formation, growth, pulsating, and collapsing of micro air bubbles that tend to
be trapped inside nanoparticle clusters during the negative and positive pressure cycles [17,20]. The
strong cavitation can create transient (in the order of nanoseconds) micro 'hot spots' that generate
temperature of about 5000 C, pressure of above 1000 atms, and heating and cooling rates above
10 10 K/s [4,5,11]. The severe implosive impact in conjunction with local transient high temperature
can effectively fracture nanoparticle clusters, clean the particle surface and enhance the wettability
between melts and particulates [6,7,16,24]. Acoustic streaming flows throughout the melt and helps
to circulate nanoparticles all over the melt (Fig. 1). The acoustic cavitation starts to develop in the
melt when the acoustic pressure exceeds the cavitation threshold [23]. This threshold value or the
acoustic energy, required to initiate the cavitation, depends upon the purity of the melt with respect
to non metallic solid inclusions and dissolved gases.
Eskin et al. [23] have shown that the more polluted the
melt, the lower is the cavitation threshold value.
Compared to conventional castings, UTCB method
proves to be more reliable for producing
nanocomposites even with system having extreme
difference in thermal coefficients between metal
matrix and ceramic particulates [11,25].
Influence of Processing Parameters
Although extensive research has been conducted to
develop MMNCs by UTCB method, only a few studies
have been reported to understand the influence of
different process variables on the microstructure specifically the dispersion of nanoparticles as well as
the resultant mechanical properties of nanocomposite
in particular [11,24]. Li et al. [11] have shown that the
ultrasonic power of 3 kW yields maximum
nanocomposite, further increase of power decreases
both strength as well as ductility (Fig. 2a). For AZ91SiC nanocomposites, Nie et al. [24] have demonstrated
that ultrasonic stirring time of 5 min shows best
combination of mechanical properties whereas further
increase of stirring time is detrimental for mechanical
properties possibly due to increasing formation of
micro-cavities (Fig. 2b).
Microstructure of MMNCs
High intensity ultrasonic treatment creates cavitation

Fig. 2. Influence of ultrasonic (a) power

and (b) stirring time on mechanical
properties of MMNCs; data taken from
the reports of Li et al. [11] and Nie et
al. [24], respectively.

Advanced Materials Research Vol. 1042


that is sufficient to break nanoparticle clusters in addition to the enhancement of wettability of

ceramic particles in the liquid metal, whereas the generated acoustic streaming helps to disperse
nanoparticles uniformly in the melt within very short duration [6,19]. Figure 3 summarizes the
reported influence of size and amount of particles on grain size of SiC reinforced Mg-based
composites prepared by UTCB method [21,26]. It is evident that the grain size of composites
reduces with increasing volume of reinforcement and the same is more pronounced with decreasing
size of the particles (Fig. 3). This is because of reinforcing particles act as homogeneous nucleating
sites during solidification composite slurry. It is worth to mention here that ultrasonic melt
treatment of alloys prior to solidification, refines melt by eliminating solid non-metallic inclusions
and by degassing to lessen the cavities during casting [7,23]. However, there would be a chance of
formation of micro-cavities in the cast samples after solidification, if the acoustic streaming
becomes too wild on the melt surface, shielded by inert gas [7].
Shen et al. [21] have shown that mixture of micron and nano-sized particles is more effective to
reduce grain size when compared to that of individual particles either of micron or nano-size (Fig.
3). Particles are pushed to the grain boundary by the solidification fronts during casting leading to
the formation of undesirable agglomerates and clusters that adversely affects mechanical properties
of composite materials [11]. Formation of typical necklace-typed particle distribution has been
observed more in nanocomposites in comparison with sub-micron sized composites [5,26]. Such
casting defects can be eliminated to a large extent by suitable post-processing like hot extrusion
[24,26]. Decrease in grain size after extrusion as compared to as-cast condition illustrates the fact
that during hot extrusion, dynamic recrystallization
takes place due to an accumulation of dislocations at the
grain boundaries [21,24,26].
Mechanical Properties of MMNCs
Figure 4 illustrates the variations of tensile properties
with respect to amount of nanoparticles in Al-alloy
[17,18], commercial pure Mg [16,20] and Mg alloys
[4,5,19] matrix composites, all prepared by UTCB
method. Yield strength of MMNCs increases almost
linearly with nanoparticle content within its investigated
range (up to 4 wt.%). Tensile strength is also found to
be increased significantly for all nanocomposites as
compared to the base alloy (Fig. 4). Cicc et al. [22] have Fig. 3. Variation of grain size of UTCB
reported that incorporation of 0.5 wt.% -SiC processed AZ31B nanocomposites in as
nanoparticles (30 nm) in semi-solid state of Zn cast and after extrusion [21,26]. Note
(AC43A) alloy by UTCB process increases strength; that mixed particle sized composite
however, the reported degree of improvement in consists of 1 vol.% of 60 nm and 14
strength is marginal when compared to that of Al or vol.% 10 m particles.
Mg- matrix nanocomposites. One of the unexpected facts of MMNCs produced by UTB based
method is that the ductility of the composites either increases considerably or remains almost same
level when compared to that of the unreinforced base metals/alloys. This is barring the results
reported by Erman et al. [16] where addition of 1 wt.% SiC nanoparticle (55 nm) is found to
diminish the ductility of commercial pure Mg considerably in as cast condition. It has been reported
that uniform distribution of nanoparticles by UTCB technique in the Mg-matrix activates additional
slip systems in otherwise limited number of slip systems of the Mg-alloys, resulting in improved
ductility in the MMNCs.
Cao et al. [4] for Mg-SiC and Nie et al. [5] for AZ91-SiC systems have systematically studied
the influence of nanoparticle content of tensile properties of MMCs. Results of these investigators
assist to infer that the best combination of tensile properties corresponds to composite with 2 wt.%
of nanoparticles. When nanoparticle content is increased to beyond 2 wt.%, both tensile strength


Materials Science and Intelligent Technologies Applications

and elongation are reduced markedly; these

observations have been attributed to increased particle
agglomeration, resulting in degradation of mechanical
properties. In other words, experimental results relating
to microstructure and mechanical properties indicate
that the ultrasonic system, used till date for
manufacturing of MMNCs, could disperse nanoparticle
uniformly up to 2 wt.%. Therefore, dispersion of
higher amount of solid nanoparticles in the liquid
metals still remains a challenge even for UTCB
processes. It is worth to mention here that 2 wt.%.
nanoparticles is often considered sufficient to impart
desirable strength in composite materials considering
their higher effectiveness in promoting particle
strengthening mechanisms, as briefly outlined below.
The enhanced strength and hardness in particulate
reinforced MMNCs can be attributed primarily to the
following four types of strengthening mechanisms: (i)
Orowan strengthening from dislocation bowing by
reinforcing particles, (ii) HallPetch strengthening
from grain refinement, (iii) Taylor strengthening due to
modulus difference between the matrix and the
particle, and (iv) Dislocation forest strengthening
resulting from the mismatch of thermal coefficient
between the matrix and the particulate [25]. Extent of
strengthening by Orowan mechanism depends on the
amount and size of reinforcing particles that effectively
determine the inter-particle spacing. More homogenous
distribution of nanoparticles by UTCB processing is
expected to create the highest strengthening effect by
providing the strongest barriers for a moving
dislocation line per volume percentage of particles
[16,19]. Reinforcing particle acts as heterogeneous
nucleating sites during solidification of MMCs, leading
to the refinement of grain size. This effect increases Fig. 4. Variations of (a) tensile strength
with decreasing particle size for same volume of and (b) elongation to failure with amount
reinforcement. Therefore, MMNCs exhibit higher grain of nanoparticles for Al- and Mgsize strengthening effect as per HallPetch relationship nanocomposites prepared by UTCB
[16,25]. The contribution from the Taylor method.
strengthening mechanism that determines the load-bearing capacity of the composite is more
pronounced for reinforcement with higher modulus value and for better interfacial bond strength
between the particle and the matrix. The interfacial bond strength is expected to be higher for
MMNCs processed by UTCB method, because it is known to develop cleaner particle surface with
enhanced wettability [1,25]. Dislocation forest strengthening is considered to have smaller
contribution than HallPetch and Orowan strengthening, specifically in case of cast MMNCs
[16,25]. Improved strength of nanocomposites over microcomposites is commonly attributed to the
enhanced contribution from one or more of the above-mentioned strengthening mechanisms often
without systematic analyses to delineate their real contribution, which should be the focus of the
future research endeavour.

Advanced Materials Research Vol. 1042


Concluding remarks
The ultrasonic cavitation based manufacturing of MMNCs has been briefly reviewed. Ultrasonic
method develops nanocomposites with more uniform dispersion of nanoparticles due to combined
influence of transient cavitation and acoustic streaming. Being liquid-phase route, this technique is
considered as one of the most promising methods for manufacturing of MMNCs for vivid structural
applications. Recent research has established the utility of this method via laboratory scale
manufacturing of several Al- and Mg-based nanocomposites with significantly improved strength
and ductility. Scale-up of the process in preparing structural components, however, imposes new
challenges. Furthermore, considerable basic research is necessary to understand the relationships of
process variables, developed microstructures and mechanical properties of MMNCs so as to realize
the full potential of this novel processing method.
The assistance received from the Centre of Excellence on Microstructurally Designed Advanced
Materials Development, TEQIP-II to carry out a part of this work is gratefully acknowledged.


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