Settling of silicon carbide particles in cast metal matrix composites

A. Ourdjini
*
, K.C. Chew, B.T. Khoo
Faculty of Mechanical Engineering, Universiti Teknologi Malaysia, 81310 Johor Bahru, Malaysia
Abstract
The success of metal matrix composites as potential materials for the manufacture of engineering components depends on closer control
of their microstructure during processing. One of the important factors inuencing the microstructure is settling of the particles during
liquid processing of these composites. In this paper settling of SiC particles in cast aluminium alloy metal matrix composite was studied as
function of particle size, weight fraction and melt temperature during isothermal holding and solidication experiments. Isothermal holding
of A356 aluminium alloy reinforced with 20 wt.% of silicon carbide particles showed that settling occurs at signicantly slower rates than
predicted by theoretical models. The results also showed that the melt temperature appears to have a slight effect on the settling behaviour.
Experiments on settling during mixing and solidication revealed that at low melt temperatures the volume fraction of particles does not
affect the rate of settling but as the melt temperature increases the particles tend to settle when present in lower volume fractions.
# 2001 Published by Elsevier Science B.V.
Keywords: Particle settling; Uniform distribution
1. Introduction
Signicant industrial advantages in reinforcing a light
metal or alloy with a ceramic is the production of a compo-
site material with improved mechanical properties. Metal
matrix composites have a market potential for various
applications, particularly in the automotive industry where
the pressure to use light weight materials has increased
because of environmental issues. Examples of components
that have been manufactured using metal matrix composites
include pistons for diesel engines and connecting rods [1].
These materials have also been shown to possess great
potential for applications in the brake disks for railway
brake equipment [2].
Important metal matrix composites are mostly based on
the aluminiumsilicon casting alloys [35]. Metal matrix
composites display a unique feature in being capable of
providing tailor-made materials with unique combinations
of properties of mechanical properties. Particle-reinforced
aluminium composites, in particular, with their potential as
low cost, when processed by the molten metal mixing route
offer a commercially viable low cost composite components
[3,57].
Their success as potential engineering materials, however,
depends on the control of their solidication structure during
processing. It has been generally accepted that several
important factors inuence the formation of solidication
microstructure in cast particulate composites [5,8,9]. These
are nucleation on particles, particle pushing by the solid/
liquid interface, particle settling in the melt, and chemical
reactions between particles and the matrix.
Uniformity of distribution of particulates is a major factor
in determining the in-service properties of engineering
components made of metal matrix composite [3]. Extensive
experimental and theoretical studies [3,1012] have been
made to investigate this subject. They all conrmed that one
of the most important factors affecting the nal microstruc-
ture is the solidication rate.
Another important factor inuencing the particle distribu-
tion in casting is the settling of SiC particles during melt
holding and during casting due to gravity. Settling of SiC
particles will yield to a non-uniform distribution of reinfor-
cement in the matrix, which in turn has signicant con-
sequences to the mechanical properties.
Models have been proposed to describe the settling
phenomenon of the particles. Stokes developed an expres-
sion for the settling velocity of spherical particles moving
relative to a continuous uid [13].
V
s

d
2
r
s
rg
18m
(1)
where d is the particle diameter, r
s
the density of the particle,
r the density of the liquid, m the viscosity of the liquid and g
the acceleration due to gravity. At higher volume fractions,
Journal of Materials Processing Technology 116 (2001) 7276
*
Corresponding author.
0924-0136/01/$ see front matter # 2001 Published by Elsevier Science B.V.
PII: S0 9 2 4 - 0 1 3 6 ( 0 1 ) 0 0 8 4 3 - 3
particles generally interact with each other reducing in the
process the settling velocity. Richardson and Zaki [14] have
explained the settling of particulates with a size greater than
100 mm, using the hindered Stokes' velocity V
p
.
V
p
V
s
1 C
4:65
(2)
where C is the true concentration of particles.
Several investigators have reported data on the settling of
SiC particle reinforcement in liquid aluminium matrix
composites produced by the molten metal route [13,15,16].
In their investigation on 82 mm SiC particles in an alu-
miniumsilicon alloy (A356), Lafreniere and Irons [15]
measured much lower settling rates than those predicted
by Stokes' law, whereas higher rates of settling were
reported by Gallerneaut and Smith [17] for SiC particles
having diameters ranging from 10 to 155 mm in A356 alloy.
The presence of particles as clusters appeared to be the
reason for the greater settling rates observed. Lloyd and
Chamberlain [18] examined the settling of SiC particulates
in a melt of A356 matrix alloy and reported that the amount
of settling saturates after about 30 min. It has also been
shown that the settling rate is dependent on the reinforce-
ment size, shape as well as the reinforcement volume
fraction. To date no settling analysis has investigated the
effect of temperature on the settling rates of reinforcement
particles. Also, measurements of settling rates have not been
as comprehensive and as conclusive in their support for the
available models.
Reliable data are required to conrm or distinguish
between the available models. The purpose of this paper
is to investigate the settling of SiC particles in a matrix melt
of A356 aluminium matrix alloy during isothermal holding
in the liquid state, and examine the inuence of SiC parti-
culate settling on the microstructure formed during casting
into permanent moulds. Experiments on the settling beha-
viour during isothermal holding were carried out at different
melt temperatures.
2. Experimental procedure
Experiments were carried out to study the effect of
settling on the solidication microstructure. The matrix
alloy used in the present study is an AlSi casting alloy
matrix (A356) reinforced with SiC particles. The composite
materials were fabricated using the semi-solid dispersion
technique. Commercial A356 (Al7% Si0.4% Mg) alloy
reinforced with 7 and 20 wt.% of SiC particles with an
average size of 25 and 65 mm were used to investigate the
particle settling and its inuence on the solidication micro-
structure. The matrix alloy was rst melted in a silicon
carbide crucible in a resistance furnace under a stream of
argon gas to protect the melt against oxidation and helps to
avoid the entrapment of gases. After allowing for melt
homogenisation, the temperature was gradually lowered
until the charge was approximately half solid. This was
followed by the introduction of the preheated particles into
the slurry.
Prior to heat treatment, the particles were ultrasonically
cleaned with acetone and dried to reduce any eventual
adverse chemical reaction between the slurry and particles.
Heating the particles for 2 h at 8508C was used to improve
the wetting properties by removing the adsorbed gases from
the surface of particles. This treatment was found to lead to a
uniform particle distribution in the mechanically stirred
matrix melt [19]. The particles were introduced into the
slurry within a short period of time of about 3 min followed
by stirring in the semi-solid state for another 1015 min.
Then, the melt temperature was raised to above its liquidus
temperature. Two types of experiments were carried out.
1. Isothermal holding of the composite material containing
20 wt.% of 25 and 65 mm SiC particles in the liquid state
at 700 and 7508C for 20 and 40 min. In this experiment,
the molten composite was transferred from the crucible
into small permanent steel moulds (with a 20 mm
diameter and 50 mm length) placed inside a resistance
furnace with the temperature set at either 700 or 7508C.
The longitudinal sections were polished and prepared
for microstructural examination to reveal the transition
interface between the regions with and without particles
and to make measurements on the settling rates.
2. The second experiment consists of casting the composite
material into permanent moulds producing cylindrical
bars with a diameter of 12 and 145 mm long held at
ambient temperature. The composite material consists of
7 and 20 wt.% of 25 mm SiC particles. To examine the
influence of solidification conditions, the composite
melt was poured at two different temperatures of 670
and 7308C and a total of eight bars were produced from
each melt. These bars are denoted as B1B8, where B1
means first cast bar and B8 the last cast bar.
All eight samples from the as-cast bars were sectioned
from three positions (bottom, centre and top), polished and
examined under a Nikkon microscope to characterise the
microstructures with an emphasis on the particle distribution
and settling within the matrix. Weight fraction measure-
ments of all samples was made using an image analyser.
3. Results and discussion
Typical polished longitudinal sections of the ingots con-
taining 20 wt.% of 25 and 65 mm SiC particles, after iso-
thermal holding for 20 and 40 min at 7508C, are shown in
Figs. 1 and 2, respectively. It can be seen even in these
macro-sections that a sharp transition line between metal
with and without particles is displayed. By measuring the
length of the particle-free zone it was possible to measure
the settling rates of particles. The results of the measured
height of the denuded zone are plotted against holding time
for the two different melt temperatures as illustrated in
A. Ourdjini et al. / Journal of Materials Processing Technology 116 (2001) 7276 73
Fig. 3. The results reconcile very well with the literature: as
the holding time of the composite melt is increased the SiC
particles tend to settle more to the lower parts of the ingot.
The effect of holding time on settling is more pronounced
for the larger particles rather than for the smaller ones. This
can be seen from the higher settling rates which continued to
increase with increasing holding time for the 65 mm parti-
cles, whereas for the 25 mm particles the settling reaches a
saturation point after about 20 min. Previous researchers
[13] have reported that the settling of particles tends to
saturate and goes to zero for long holding times and a
stabilised melt would be obtained. The volume percentage
required to reach a stabilised melt depends on the particle
size. This clearly seems to be the case in the present study
since the settling of larger particles only stabilised after
reaching a high weight percentage of about 45 wt.% com-
pared to the initial weight percentage of 20 wt.%. For the
smaller particles the settling rate reached the stabilised
condition after a shorter holding time of 20 min and the
volume percentage at which this stabilised condition was
obtained was estimated to be about 23 wt.% of SiC particles
which is far lower than that observed for the larger particles.
The effect of melt temperature on the settling behaviour
was investigated in the present work and the results plotted
in Fig. 3 clearly show that the settling behaviour is slightly
affected by the melt temperature, particularly the larger
particles. The particles settle faster as the melt temperature
is increased. This is probably due to the higher energy
gained by the particles at higher temperatures, which make
them travel faster and easier in the liquid melt.
Comparison of the measured settling rates with those
predicted by the Stokes' law and the hindered velocity is
shown in Table 1. In all cases the measured rates were much
lower than predicted by both models. This is not in accor-
dance with most of what others have observed. It is of
interest to note, however, that most settling measurements
made to date have used commercial composites. In such
situations, during the remelting complete melting is prob-
ably achieved only after a signicant period of time. If this
Fig. 1. Longitudinal sections of samples with 25 mm isothermally held at
7508C for 20 min (left) and 40 min (right).
Fig. 2. Longitudinal sections of samples with 65 mm isothermally held at
7508C for 20 min (left) and 40 min (right).
Fig. 3. Measured lengths of denuded zone as a function of melt holding
time. (*) 25 mm at 7008C, (*) 65 mm at 7008C, (&) 25 mm at 7508C,
(&) 65 mm at 7508C.
Table 1
Comparison between the measured settling rates with those predicted by
the theoretical models
Settling rate
(cm s
1
)
Particle size 25 mm Particle size 65 mm
T 700

C T 750

C T 700

C T 750

C
Measured value No settling 0.0006 0.0025 0.003
Stokes' law 0.03 0.03 0.20 0.20
Hindered rate 0.013 0.013 0.09 0.09
74 A. Ourdjini et al. / Journal of Materials Processing Technology 116 (2001) 7276
happens, it will eventually lead to higher settling rates even
for small particles.
The experimental results obtained in the present work are
in good agreement with those observed by Lafreniere and
Irons [15] who reported that settling in A356 matrix melt
containing 82 mm SiC particles was much lower than pre-
dicted by the theoretical models.
In the second set of experiments on settling, the aim was
to examine in a qualitative manner the effect of melt
temperature and reinforcement weight fraction on the set-
tling of SiC particles during composite processing and
solidication.
Micrographs of transverse sections obtained from bars B1
and B8 containing 20 wt.% SiC at the two melt temperatures
of 670 and 7308C show no evidence of settling (Figs. 4 and
5). The measured values of weight fractions were within
20 2 wt:%. On the other hand, during solidication of the
composite containing 7 wt.% SiC particles it was observed
that settling has occurred only when the melt was at the
higher temperature of 7308C as shown in Fig. 6. When the
particles are present in high weight percentages there are
strong possibilities that they would interact with each other
yielding to slower settling rates. There is also strong evi-
dence that settling of the particles has actually occurred in
Fig. 4. Micrographs of transverse sections taken from bars containing 20 wt.% SiC particles: melt temperature of 6708C, (a) bar B1 and (b) bar B8
magnification 50.
Fig. 5. Micrographs of transverse sections taken from bars containing 20 wt.% SiC particles: melt temperature of 7308C, (a) bar B1 and (b) bar B8
magnification 50.
A. Ourdjini et al. / Journal of Materials Processing Technology 116 (2001) 7276 75
the crucible during the mixing and stirring process. This is
because when the composites are cast into the cylindrical
bars, the rapid solidication rates prevent the particles from
steeling.
Examination of the solidied samples also revealed that a
more uniformSiCparticles distribution is observed when the
particles are present in high volume fraction rather than low
volume fraction.
4. Conclusion
In conclusion, settling measurements during isothermal
holding showthat the SiCparticles settle at much lower rates
than predicted by the theoretical models. Qualitative exam-
ination of the settling phenomenon shows that composites
reinforced with low volume fractions of particles tend to
settle faster particularly if the melt temperature is high.
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76 A. Ourdjini et al. / Journal of Materials Processing Technology 116 (2001) 7276