Trans Indian Inst Met (December 2012) 65(6):747751

DOI 10.1007/s12666-012-0170-5

TECHNICAL PAPER

TP 2622

Squeeze Infiltration Processing of Functionally Graded

AluminumSiC Metal Ceramic Composites
K. M. Sree Manu V. G. Resmi M. Brahmakumar
P. Narayanasamy T. P. D. Rajan
C. Pavithran B. C. Pai

Received: 29 June 2012 / Accepted: 24 August 2012 / Published online: 28 September 2012
Indian Institute of Metals 2012

Abstract The objective of the present work is on fabrication of functionally graded SiC/Al composite by direct
squeeze infiltration of 6061 aluminum alloy using graded
SiC porous preform prepared by inorganic porogen technique. Graded SiC preform is synthesized by varying the
concentration of inorganic salt mixture and using Al as the
binder. The microstructure analysis indicates the graded
distribution of SiC particle and the melt has infiltrated
completely throughout the preform to form functionally
graded materials. The influence of preform and mold
temperature, liquid metal superheat, squeeze pressure, and
its rate of application plays major role on solidification
microstructures and properties of the composites. The
macro porous graded SiC preforms and the composites
were characterized using SEM, optical microscopy, and
XRD. The major interfacial reaction product is MgAl2O4
spinel which helps in formation of good interface bonding.
Keywords Infiltration
Functionally graded material

Aluminum
SiC
Porous preform

1 Introduction
Functionally graded materials (FGM) are advanced class of
composite materials with a smooth gradient in one or more
properties within in a single component obtained by

K. M. Sree Manu
V. G. Resmi
M. Brahmakumar

P. Narayanasamy
T. P. D. Rajan (&)
C. Pavithran
B. C. Pai
Materials Science and Technology Division, National Institute
for Interdisciplinary Science and Technology, CSIR,
Thiruvananthapuram 695019, Kerala, India
e-mail: tpdrajan@rediffmail.com; tpdrajan@niist.res.in

variation in chemical composition or microstructure in

specific direction [14]. FGM are used for wide spectrum
of applications in different areas such as aerospace, automotive, defense, electronics and communication, electrical,
structural, biomedical, and in general engineering applications. The functionally graded metalceramic composite
components can be processed with different approaches
such as solid, liquid, and deposition process. Among this
the squeeze infiltration is one of the potential techniques to
obtain FGM with high volume of reinforcement having
different layers. It is a liquid state fabrication process in
which preforms are constructed layer by layer with
appropriate gradients in the distribution of constituent
phases with graded porosity and its infiltration with the
liquid metal with or without the application of pressure [5].
Graded preform should have sufficient strength to withstand the squeeze pressure and inter connecting porosity
for the liquid metal to penetrate and get solidified.
The burn-out or decomposition of fugitive pore formers
like organic/polymeric or inorganic materials is an important strategy for producing macro porous ceramic foams
with controlled pore sizes and content [6]. Studies on
infiltration processing of metal matrix composites are done
extensively, however, comparatively very less investigations on infiltration processing of FGM are being carried
out. Spontaneous infiltration of ZrO2 preforms with a graded porous structure had been successfully done for fabrication of functionally graded AlMg/ZrO2 components
[7]. Bilayer-graded AlSiCp composites were prepared by
pressureless infiltration technique [8]. However, literature
on squeeze infiltration processing of Al FGM is very rare.
The present investigation is on synthesizing graded SiC
perform using less expensive inorganic salts as pore former
followed by leaching or burn out to form the porous preform
and direct squeeze infiltration of molten aluminum into

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Trans Indian Inst Met (December 2012) 65(6):747751

Fig. 1 a Sintered graded SiC preform, SEM micrographs of the infiltrated graded composite, b 60 %, c 50 %, d 40 % of SiC

porous SiC graded perform to form functionally graded

AlSiC metalceramic composites.

2 Experimental Methods
Aluminum 6061 alloy was used as the matrix phase for
infiltration and its chemical composition (wt%) was 1.2 Mg,
0.8 Si, 0.40 Cu, 0.25 Zn, 0.15 Ti, 0.35 Cr, 0.7 Fe, 0.15 Mn
and remaining Al. The macro porous graded preforms
were prepared by stacking powder mixture layers containing different volume fraction of SiC (*42 lm) particles,

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sodium chloride particles and aluminum powder as binder.

Different layers of SiC, NaCl, and Al were mixed uniformly
with polyester in acetone medium and evaporated at room
temperature to impart strength to the green body. The three
different layers of ceramic mixtures were stacked together
in a steel mold and compacted using a powder compaction
press. The green ceramic preform was heated in a furnace at
temperature above the melting point of aluminum for 3 h
and after cooling, the salt present in the pellet was removed
by leaching in hot water and followed by drying at 120 C
to obtain the SiC porous graded preform. The design of the
die plays a major role in the complete infiltration of molten

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Fig. 2 a Graded aluminumSiC infiltrated specimen, microstructures of functionally graded Al (6061)SiCp composite by infiltration (b, c, d,
and e)

metal into the preform. The die of 35 mm diameter cavity

was designed and fabricated using tool steel. The SiC preform was preheated at 700 C and placed into the die heated
at 300 C before pouring of liquid molten metal. The above
process was essential to avoid the solidification of liquid
molten metal before complete infiltration of preform occurs.
The magnesium added 6061 aluminum alloy melt had been
prepared in resistance furnace and the melt was poured into
the die where the preform was placed. Subsequently high
pressure was applied on the molten metal for infiltration
into the preform in a hydraulic press. The pressure (MPa)
was maintained for about 56 min until the solidification
was complete. The macro porous graded SiC preforms and
the composites were characterized using JEOL SEM, Leica
optical microscope, and Philips XRD.

3 Result and Discussion

The macrograph of the graded porous SiC preform synthesized by pore former burn out technique is shown in
Fig. 1a. The SEM image of SiC preform having three
different graded layers with continuous and uniform pore
distribution is shown in Fig. 1bd. Figure 1b shows the
first layer of the graded perform having the composition
L1 (60 % SiC40 % NaCl). Figure 1c shows the second

layer of the graded perform having the composition L2

(50 % SiC50 % NaCl). Figure 1d shows the third layer of
the graded perform having the composition L3 (40 % SiC
60 % NaCl).
The macrograph of the infiltrated specimen and microstructure of aluminumSiC composite fabricated by
squeeze infiltration method is shown in Fig. 2a. Graded
distribution of SiC particles are seen in Al (6061) alloy
matrix at four different locations from top to bottom of the
macrograph and which is reflected in the micrographs
shown in Fig. 2b (outer region) to Fig. 2e (inner region) in
12 mm thick casting. Figure 2b shows the outer most layer
having high volume fraction of SiC compared to the other
layers which is formed from completely metal infiltrated
lower porosity region of the preform. Figure 2c shows
the micrograph of second graded preform layer where the
medium porosity is filled with 6061. Figure 2d shows the
third graded layer of composite where the metal gets infiltrated to the preform having high porosity region. The white
region shows the infiltrated 6061 matrix and the gray phase
shows the SiC particles. Finally Fig. 2e shows the microstructure of the interface region between the aluminum
alloy and the SiC functionally graded composite where the
metal gets started to penetrate into the ceramic graded
preform. From the above microstructures it is clear that
matrix aluminum gets penetrated completely throughout the

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Trans Indian Inst Met (December 2012) 65(6):747751

Fig. 4 SEM micrograph of AlSiC metal ceramic FGM showing

good bonding between the matrix and SiC particle

SiC

600

MgAl 2O4
MgO

Al 2O3
Si

Intensity (a.u.)

500

400

300

200

100

0
20

30

40

50

60

70

80

2 theta (degrees)

Fig. 5 XRD pattern of particle extracted from Al/SiC functionally

graded composite using NaOH solution showing interfacial reaction
products

Fig. 3 SEM micrographs of the infiltrated graded composite a 60 %,

b 50 %, c 40 % of SiC

graded SiC layers even into the minute pores in the preform
which shows the complete infiltration. Figure 3 shows the
SEM micrograph of the infiltrated graded composite, which
clearly shows the varying volume percentage of SiC particles in three graded layers. Figure 4 shows the SEM
micrograph of the AlSiC metal ceramic composite with

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high volume fraction, where there is a good interfacial

bonding between the SiC particle and Aluminum. This was
mainly due to the good infiltration and presence of Al binder
used in the porous preform. Studies have shown that the
presence of metallic coating or binders in the surface of
reinforcement generally improves the wettability of the
composites [9].
The XRD pattern of SiC particles extracted from the
AlSiC FGM using NaOH is shown in Fig. 5. Apart from
the major peaks of SiC particles, the peaks of MgAl2O4 and
MgO phase is detected in composite, but the peaks of
brittle and unwanted phase like Al4C3 is not detected. Mg
is a powerful surfactant that scavenges oxygen from the
melt surface and forms MgAl2O4 spinel and MgO at
the Al/SiC interface, thereby enhancing the wettability and

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the effective infiltration of liquid metal into the preform.

Addition of magnesium has to be limited to 4.7 mass% due
to the formation of relatively brittle intermetallic compound such as Al3Mg2. The alumina peak observed in the
composite may be formed during the sintering of SiC
preform containing Al binder, where the surface oxidation
of alumina can occur as well as the oxide formed during the
infiltration of liquid metal. The Si peak corresponds to the
silicon which is present in the alloy which can segregate to
the interface region during the solidification of the metal.

functionally graded composite. The infiltrated AlSiC

graded composite feature a dense and pore free microstructure with a varying SiC particle distribution in the
metal matrix. Only MgAl2O4 spinel and MgO phases were
detected at the interface and no brittle Al4C3 phase is
observed.

4 Conclusion

References

Liquid metal infiltration of ceramic preform is a promising

route to produce metal matrix composites with high volume fraction and uniform distribution of the reinforcement
in the matrix phase, which is not possible in other conventional methods. In the present study a graded preform of
SiC was prepared successfully by inorganic salt porogen
technique. The aluminum is used as the binder, which help
in low temperature binding of the porous preform and also
provides high strength to the porous preform. During
infiltration the Al binder also helps in better wettability
of the SiC particle with the matrix. Squeeze infiltration
method is used to make Al alloy matrix composites with
the controlled process parameters and the liquid metal has
fully infiltrated throughout the graded preform to form the

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Acknowledgments The authors are grateful to the Director and

Members of Materials Science and Technology Division, CSIRNIIST, Trivandrum for their support and help. Mr. M. R. Chandran,
and Mr. P. Guruswamy for the SEM and XRD analysis.

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