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Ceramics International
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A R T I C L E I N F O A B S T R A C T
Keywords: Metal/ceramic composites are in high demand in several industries because of their superior thermo-mechanical
a) Interpenetrating metal/ceramic composites properties. Among various composite types, the interpenetrating phase composites (IPCs) with percolating
b) Processing metallic and ceramic phases offer manifold benefits, such as a good combination of strength, toughness, and
c) Porous ceramics
stiffness, very good thermal properties, excellent wear resistance, as well as the flexibility of microstructure and
d) Mechanical properties
e) Thermal properties
processing route selection, etc. The fabrication of metal/ceramic IPCs typically involves two steps - i) processing
f) Material property maps of an open porous ceramic body, and ii) infiltration of metallic melt in the pores to fabricate the IPC. Although
significant progress has been made in recent years for developing both porous ceramics and melt infiltration
methods, to the best of the knowledge of the authors, no review article summarizing all the aspects of processing
and properties of IPCs has been published till date. This review article is aimed at filling this gap. Starting with a
brief introduction about the current status and applications of IPCs, the various processing routes for fabricating
open porous ceramic preforms and melt infiltration techniques have been discussed. Subsequently, the data
available for various important physical, mechanical, and thermal properties for IPCs have been critically
analyzed to thoroughly understand their dependence on various structural and processing parameters. To
compare the properties of IPCs with other relevant materials, seven different Ashby material property maps have
been used, and the domains for IPCs have been created in them. For each map, the concept of material indices
has been employed to critically discuss how IPCs perform in relation to other material classes for various op
timum design conditions. Finally, a detailed future outlook for further research on IPCs has been provided.
1. Introduction mechanical, thermal, and electrical properties between the metallic and
the ceramic phases confers MMCs with a high degree of tailorability.
Over the past several decades, metal matrix composites (MMC) have They exhibit high specific strength and stiffness together with good
evolved into versatile and robust engineering materials with immense fracture properties like toughness, fatigue, and impact resistance,
commercial viability in various markets. This transformation was made essential for structural and load-bearing applications. Their high ther
possible by comprehensive research in materials development and in mal conductivity and low coefficient of thermal expansion are often of
novations in sustainable manufacturing techniques over many years. In primary importance for thermal management applications [8,9]. They
2020, the global MMC market size accounted for 8395 metric tonnes, also display a reasonable degree of electrical conductivity and resistance
estimated at USD 360 million, and was forecast to grow at a rate of 6.4% to corrosion and erosion. MMCs are in high demand in the aerospace,
compounded annually from 2020 to 2027 [1]. MMCs typically consist of automotive, recreational, and infrastructure industries because of their
a ceramic reinforcement phase (SiC, Al2O3, B4C, TiC, graphite, NbC, superior mechanical reliability and energy efficiency [10].
TaC, TiB2, and WC) and a metallic alloy (Al, Mg, Ni, Cu, Fe, and Ti) Based on the reinforcement architecture, metal/ceramic composites
[2–5]. The choice of metallic and ceramic materials is based on their are traditionally classified into various categories - particulate, short
compatibility and the intended final properties. In MMCs, under fiber- or whisker-reinforced, continuous fiber-reinforced, and layered or
external loading conditions, an efficient load transfer occurs from a laminated composites [11]. The effect of reinforcement morphology on
relatively softer and ductile metallic phase to the stiffer and stronger macroscopic behavior for these composite types has been extensively
ceramic reinforcement [6,7]. The significant difference in physical, researched both experimentally and theoretically. The presence of
* Corresponding author.
E-mail address: siddhartha@metal.iitkgp.ac.in (S. Roy).
https://doi.org/10.1016/j.ceramint.2021.09.232
Received 29 July 2021; Received in revised form 11 September 2021; Accepted 22 September 2021
Available online 23 September 2021
0272-8842/© 2021 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Please cite this article as: Navya Kota, Ceramics International, https://doi.org/10.1016/j.ceramint.2021.09.232
N. Kota et al. Ceramics International xxx (xxxx) xxx
ceramic particles in a metallic matrix results in higher strength, hard Fig. 1. The research and development of IPCs have gained momentum
ness, and wear resistance in particulate composites [12,13]. However, mainly over the past couple of decades, primarily under the impetus of
poor interfacial bonding, unnecessary reinforcement clustering, and the simultaneous thrust in porous ceramics research [26,27], as metal/
formation of interfacial reaction products and internal voids may ceramic IPCs are commonly produced by infiltrating open-porous
significantly reduce the resulting composite properties. Short fiber ceramic preforms with metallic alloys. The continuous metallic
reinforced composites, although superior to their particulate reinforced network ensures efficient crack-bridging, whereas the ceramic network
counterparts, their formability is usually inferior, and also, the isotropic aids in the decentralization of stress and efficient load transfer and offers
nature is mainly restricted to the plane of the fibers [14]. Maximum dimensional stability at elevated temperatures. Thus, IPCs display an
property enhancement is obtained in continuous fiber-reinforced com excellent combination of strength and toughness, wear, fatigue resis
posites [15,16]. However, difficulties during processing and ductility tance [28,29], etc. They also possess lower CTE and thermal hysteresis
and toughness constraints limit their use to somewhat exotic applica and are more resistant to thermal cycling damage in comparison to
tions. Moreover, continuous fiber-reinforced composites exhibit rela particle reinforced composites [30–32].
tively high anisotropy, and the properties are deficient in the direction All these shreds of evidence of property improvement make IPCs
transverse to the fiber direction. Layered composite systems have potentially attractive candidates for creating multi-functional compos
garnered attention because the constituents are alternating layers ites and structural systems for several applications. Some of the impor
ranging from thicknesses of a few nm up to macroscopic laminates [17]. tant application fields where IPCs have already been proven to be
Compared to the particulate or fiber-reinforced composites, attractive are shown in Fig. 2. IPCs have a distinct potential for auto
metal-ceramic laminates are often relatively easy to produce, and the motive applications such as braking systems in automobiles and emer
elastic properties can readily be predicted using established gency brake pads for high-speed trains [33], high-temperature [34,35],
micro-mechanical models. and thermal management applications such as heat-sink base plate for
These conventional reinforcement architectures result in the electronic packaging [36,37], high cycle fatigue applications [38],
embedment of discrete and isolated phases discontinuously dispersed in vibration-damping applications for seismic resistant structures [39],
a matrix. Subsequently, the interconnectivity of the constituent phases lightweight armors for defense applications [40,41], nuclear protective
in composite materials was also considered. This has resulted in the materials and battery electrode materials [42,43], IC engine piston
development of a newer class of composites, metal/ceramic inter crowns, cylinder liners, connecting rods, turbine compressors, etc. The
penetrating phase composites (IPCs), also referred to as C4 and 3-3 development of IPCs also presents incentives for assessing the theoret
composite materials [18,19]. In IPCs both phases are topologically ical understanding of composites regarding the dependence of transport
co-continuous and three-dimensionally percolating, exhibiting an properties on volume fraction and phase connectivity.
intertwining network structure [20–25], as shown schematically in Due to their numerous potential benefits, IPCs are currently subject
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section has two parts. In the first part, the various processing routes
employed for fabricating porous ceramic preforms relevant for IPCs are
discussed, while the second part describes the different melt infiltration
techniques for fabricating IPCs. In section 3, various physical, mechan
ical, and thermal properties of IPCs have been discussed individually
from the available research data. Wherever relevant, the compiled re
sults have been compared with various micromechanical models for
composite materials. As one of the primary aims of this review is to
compare IPCs with other material classes (such as metals, ceramics, and
other composites), extensive use of the Ashby material property maps
and the concept of material indices have been employed in this section.
Finally, in section 4, some future research directions for further devel
oping IPCs are proposed.
2.1.1. Freeze-casting
The freeze-casting technique, also referred to as the ice templating
process, is a versatile method to fabricate a wide range of open porous
ceramics, including silicon carbide [62–64], alumina [65,66],
yttria-stabilized zirconia [67,68], silica [69,70], silicon nitride [71,72],
boron carbide [73], etc. An exhaustive review of the processing of
freeze-cast porous ceramic structures is reported by Scotti et al. [50]. As
shown schematically in Fig. 4, the process involves preferential nucle
ation and growth of ice crystals when a defined thermal gradient
(sub-zero temperature) is applied to freeze an aqueous ceramic slurry
directionally. As the continuous solvent crystals form and grow within
the slurry, they reject the suspended ceramic particles from the pro
gressing solidification front so that the particles are entrapped in be
tween the crystals by natural segregation. Once the solidification ends,
Fig. 3. No. of research articles published each year on IPCs (source: Sco sublimation is performed under reduced pressure to convert the solidi
pus database). fied solvent into the gaseous state. Correspondingly, a porous ceramic
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Fig. 4. Schematic diagram of the freeze casting technique: (a) Mold with a ceramic slurry, (b) Growing ice crystals, (c) Completely grown ice crystals, (d) Porous
structure after sublimation, and (e) Lamellar porous ceramic after sintering.
foam consisting of unidirectionally aligned macroporous channels, The advantages of the freeze-casting technique include easy sintering
which is a direct replica of the frozen solvent structure, results. Subse without burning of any material and eco-friendly nature without
quent pressureless sintering ensures the porous ceramic structure pos releasing any harmful toxic substances. The range of porous ceramics
sesses sufficient mechanical strength and integrity [51]. produced by this method reveals that the fundamental principles that
The porous ceramic bodies thus developed typically exhibit a dictate the porous structure formation depend more on physical than
lamellar structure. The microstructural features of the porous bodies chemical interactions, making the technique highly flexible. On the flip
depend upon the freeze-casting parameters. A faster cooling rate at a side, freeze-cast porous ceramics often exhibit directional pore structure
lower freezing temperature results in a finer lamellar structure due to and multi-modal pore size distribution. As a result, the ceramic foam
the nucleation of more ice crystals [52,74,75]. Fig. 5 depicts typical properties perpendicular to and parallel to the freezing directions can be
microstructures of the freeze-cast Si3N4 ceramic preform and the evo considerably different, which may result in significant anisotropy in the
lution of the microstructure along the freezing direction. The freezing final product.
conditions and ceramic content in the slurry are the primary variables Table 1 summarizes the processing parameters used in some of the
controlling the microstructural parameters such as the content, research works for fabricating porous ceramics via the freeze-casting
morphology, and orientation of the final porosity. The choice of a suit process.
able solvent is influenced by its freezing temperature range, fluid vis
cosity, minimal solidification-related volume changes, and high 2.1.2. Use of replica templates
solid-state vapor pressure for ease of sublimation. Apart from water, Replica methods, often referred to as the lost mold process or
tert-butyl alcohol [76], liquid carbon dioxide [77], and camphene-based Schwartzwalder method [85], have been frequently utilized to produce
slurries [65] are also used as solvents. Further addition of solidification reticulated porous ceramics (RPCs) with large interconnected pores. The
modifiers like glycerol and polystyrene can prove helpful in reducing the process typically involves impregnating the ceramic slurry into a highly
viscosity and surface tension of the concentrated slurries and prevent porous replica template, generally made of organic sponges, until a thin
defect formation [78]. uniform ceramic layer is formed over the struts of the original cellular
Fig. 5. Combined image showing the effect of process parameters on the lamellar structure of porous Si3N4 ceramics fabricated via freeze-casting process. The left-
hand side SEM images show the evolution of the lamellar structure parallel to the freezing direction with distance from the cold plate. The bottom images show the
micro CT images of the porous preform at different heights from the cold plate. The two plots show the variation of the measured lamella spacing and lamella width
with distance from the cold plate (image courtesy Dr. Karl Günter Schell, IAM-KWT, Karlsruhe Institute of Technology, Germany).
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Fig. 7. (a) Reticulated SiC foam, (b) SEM image of SiC foam indicating hollow strut, (c) SEM image of SiC foam strut surface indicating interconnecting porous
nature, and (d) XRD pattern of the SiC foam [87] (cited images have been reproduced with due permission from the publisher).
Fig. 8. Process flow chart along with the schematic for the fabrication of ceramic foam using preceramic polymer route.
in a furnace at appropriate temperatures [114,115]. The process flow with a high degree of porosity. Therefore, non-aqueous gel-casting with
chart, along with the schematic for the fabrication of ceramic foam using organic solvents with lower surface tension, such as tert-butyl alcohol
the gel-casting process, is shown in Fig. 9. and ethylene glycol, can also be employed [116–118]. Gel-casting has
Gel-casting is highly effective for rapidly producing near-net-shaped also been used in combination with appropriate amounts of sacrificial
porous ceramics with high yields and reproducibility (Fig. 10). How pore-forming agents (PFA) such as PMMA, gas-filled thermally
ever, since the process involves toxic chemical reagents, it poses a threat expandable microspheres, potato starch, etc. [115,119].
to the worker’s health and the environment upon prolonged exposure or Porous Si3N4 foams were produced by gel-casting followed by sin
release. Also, the significant amount of drying shrinkage of green bodies tering under N2 gas pressure in [116]. [121] fabricated porous YSZ
caused by the high surface tension of water (72.1 mN/m) during (52–76 vol%) by tert-butyl alcohol (TBA)-based gel-casting technique.
aqueous gel-casting limits its usage to manufacturing porous ceramics [118] prepared highly porous SiC ceramics by ethylene glycol-based
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Fig. 9. Process flow chart along with the schematic for the fabrication of ceramic foam using the gel-casting technique.
Fig. 10. SEM micrographs of 27% dense gel-cast alumina foam with 200 μm average cell size [120] (cited images have been reproduced with due permission from
the publisher).
gel-casting method. It was found that the ethylene glycol-based gels subsequent drying of the gelled part to form a green body, and finally,
exhibited an excellent gelation behavior with rapid polymerization. polymer burnout and sintering of the green bodies to give rise to porous
Also, unlike most organic solvents, where precipitation polymerization ceramics. The amount of gas incorporated into the ceramic slurry during
resulted in low green body strength, in this case, rapid solution poly the foaming process affects the overall porosity of the porous ceramics.
merization led to the increased strength of green bodies. [122] produced By optimizing the foam stability and setting kinetics, pore sizes in the
highly porous SiC ceramics by gel-casting technology using suspension range of 35 μm to 1.2 mm and porosities in the range of 40–97 vol% can
emulsions of aqueous cyclohexane. Porous alumina was prepared by a be obtained using foam-gel-casting. Also, this method generates porous
similar gel-casting method combined with the suspension emulsification structures with nearly flaw-less struts and hence marked improvement
process in [123]. [124] developed porous YSZ ceramics using TBA sol in mechanical properties.
vent for suspension formation during gel-casting along with PMMA Preceramic polymer suspensions are also utilized instead of ceramic
microspheres as PFAs. [125] successfully prepared porous Si3N4 ce slurries in the direct foaming method [128]. Open macroporous SiC
ramics employing aqueous gel-casting and the addition of Si3N4 foams (59–85 vol%) were fabricated from polycarbosilane preceramic
poly-hollow microspheres as PFAs. [111] utilized iso-butane gas-filled polymer and a chemical blowing agent (azodicarbonamide) under N2
co-polymeric microspheres as PFAs combined with a gel-casting process gas pressure in [129]. However, using this foam-gel-casting technique, it
to produce complex-shaped microporous alumina ceramics. The process is difficult to produce porous ceramics with porosity greater than 90%.
involved a temperature-induced expansion of the microspheres before Porous mullite ceramics with an open porosity up to 92.9 vol% were
the polymerization step. fabricated by solidifying an Al2O3 gel mixed with SiO2, followed by the
Instead of conventional gel-casting, direct foaming is also employed sublimation of ice crystals under a low pressure [130]. A novel in-situ
in combination with gel-casting, i.e., foam-gel-casting, to produce foam-gel-casting-freeze-drying technique was also used to fabricate
highly porous ceramic bodies [126,127]. The direct foaming process highly porous (92.2–95.8 vol%) Y2SiO5 ceramics in [131].
involves the foaming of a ceramic suspension through the direct incor
poration of gas or air bubbles by vigorous mechanical agitation or stir 2.1.4. Use of sacrificial pore-forming agents (PFA)
ring, which are then stabilized by the addition of surfactants. This is A frequently used method for producing porous ceramics with a high
followed by foam structure stabilization through in-situ polymerization, vol% of open porosity is through the pyrolysis of sacrificial PFAs that are
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Fig. 11. Process flow chart along with the schematic for the fabrication of ceramic foam using sacrificial pore formers.
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Table 2 chemical synthesis, also called reaction bonding [165,166]. Such reac
Summary of research carried out on porous ceramics synthesized using PFAs. tively generated ceramic foams are different from the starting materials,
Porous PFA Porosity Sintering Ref which are thermodynamically compatible with each other. Table 3
ceramic (vol%) parameters summarizes the research on porous ceramics prepared by partial sin
Al2O3 Waste coffee grounds 35–54 1500 ◦ C, 2 h [61] tering of ceramics through powder metallurgy.
(0–50 wt%),
Si3N4 Naphthalene (5–30 wt%) 40–66 1700–1850 ◦ C, 1 [151] 2.1.6. 3-D printing or additive manufacturing
MPa N2, 2 h During the past decade, rapid prototyping (RP) or solid free-form
Si3N4 Phosphoric acid (H3PO4) 42–63 1000–1200 ◦ C, [152]
N2, 2 h
fabrication (SFF) technologies based on 3-D printing methods have
SiC H3PO4 (5–30 wt%) 58.3–78.2 1200 ◦ C, 2 ◦ C/ [153] revolutionized the manufacturing processes with the inherent capability
min, 2 h to fabricate objects in virtually any shape, size, or morphology. Additive
Al2O3 Carbon black (0–30 wt 33–68 1550 ◦ C, 2 ◦ C/ [154] manufacturing (AM) is a highly customizable direct digital fabrication
%) min, 3 h
technology that involves precise layer-by-layer fabrication of three-
Al2O3 Polyvinylpyrrolidone 30–45 1500 ◦ C, 10 h, [155]
(PVP) (10–20 wt%) 3 ◦ C/min dimensional components. 3D CAD model of the component is first
YSZ PMMA 7.29–51.6 1550 ◦ C, 2 h, [156] made, and the actual fabrication takes place by adding successive layers
1 ◦ C/min of the materials with the desired composition on top of each other.
Al2O3 Rice Husk (5–40 wt%) 20–66 1700 ◦ C, 2 h [157] Complex 3-D porous ceramics with highly regular or periodic architec
Al2O3 Carbonized rice husk 26.8–82.4 1600 ◦ C, 2 h, [158]
(0–30 wt%) 5 ◦ C/min
tures can be fabricated by several AM techniques such as fused filament
Al2O3 Starch 22–53 1570 ◦ C, 2 h, [134] fabrication (acronym FDM or FFF) [172,173], ink-jet printing
2 ◦ C/min [174–176], stereolithography (SLA) [177,178], selective laser melting
Al2O3 Corn starch (3–18 wt%) 46–64 1400–1700 ◦ C [159] (SLM) [179], etc. Compared to the conventional processing routes dis
Si3N4 Potato starch (0–30 vol 52–66 1750 ◦ C, 5 h, [160]
cussed in the previous sub-sections, AM techniques offer better control
%) 10 ◦ C/h
Ti2AlC NaCl 40 1400 ◦ C, 4 h, Ar [161] of complex pore structures and interconnectivity because of improved
flexibility, efficiency, repeatability, and sustainability of the process [57,
180,181].
further research on porous ceramics synthesized using sacrificial PFAs. Robotic deposition of a colloidal Al2O3-5 vol% ZrO2 gel-based ink
was used to create an alumina tower structure with 3-D periodic cubic
2.1.5. Partial sintering of ceramic powders symmetry, consisting of 30 alternating 0/90 layers of parallel rods in
Homogeneous porous ceramic structures can be produced by ter [176]. The entire procedure was controlled by a custom-designed
minating the sintering of green powder compact before complete direct-write program (RoboCad 3.2). After the completion of assem
densification, i.e., partial sintering. The pore size, morphology, distri bling the entire component, the tower structures were dried and sin
bution, and microstructure of porous ceramics depend upon the sinter tered. The top view of a sintered Al2O3 tower is seen in Fig. 14a, while
ing parameters (temperature, pressure, time, atmosphere), size of the schematic illustrating the tower creation process can be seen in
starting powders, and the type and quantity of additives used. Porous Fig. 14b. The tower architecture is shown in Fig. 14c and d as a side view
bodies of Al2O3, SiC, Si3N4 have been produced by this method [162, and a 3-D schematic diagram, respectively.
163]. Typically, porous ceramic bodies with porosities below 60 vol% 3D interconnected honeycomb-like porous silica preforms were
can be fabricated through partial sintering of green bodies. Also, the prepared by the direct FFF process in [173]. 55 vol% fused SiO2 loaded
percentage of closed pores is relatively high, and so the preforms are in polypropylene (PP) based thermoplastic binder was used as feedstock
characterized by low pore connectivity. The process flow chart, along material for continuous filament extrusion and subsequent spooling.
with the schematic for the fabrication of ceramic foam using the partial Fused deposition of the extruded filaments was then performed at
sintering process, is shown in Fig. 13. 235οC, according to the CAD files given. Once the green porous ceramic
Porous ceramics have also been fabricated by pulse electric current parts were prepared, they were subjected to a binder removal and sin
sintering (PECS), also known as spark plasma sintering (SPS) technique tering treatment.
[164]. The process involves rapid heating of ceramic powders up to a 3-D honeycomb porous mullite ceramic preforms have been fabri
required temperature, generally in a graphite die, under externally cated by an indirect FFF process, a hybrid methodology that combines 3-
applied pressure. The electric discharge in the voids between the powder D printing of polymer inks with replication or lost mold approach [182].
particles gives rise to local resistance heating. The consolidation phase is A negative replica of the desired porous ceramic component is first
restricted to the initial stages of sintering to obtain relatively small neck designed and constructed as a preceramic polymer mold using the FFF
growth between the particles and retain significant porosity inside the
material. Also, highly homogeneous open porous ceramics can be suc
cessfully prepared by combining partial sintering with in-situ solid-state Table 3
Summary of research carried out on porous ceramics prepared by partial sin
tering of ceramic powders.
Porous ceramic Porosity (vol Sintering parameters Ref
%)
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Fig. 14. (a) Top view of the alumina tower fabricated by robotic deposition, (b) an idealized schematic illustrating the layering pattern, (c) side view of the tower
architecture, and (d) an idealized 3-D schematic [176] (cited images have been reproduced with due permission from the publisher).
technique, which is then impregnated with an aqueous ceramic slurry. section 2 and the corresponding pore morphologies is given in Fig. 16.
These are then subjected to a binder-removal and sintering treatment to
generate the porous ceramic preform. The polymeric mold design de 2.2. Melt infiltration techniques
termines the size, distribution, and connectivity of the pores in these 3-D
honeycomb structures. The major advantage of the indirect FFF method After the open porous ceramic preforms are made, the next step in
is that it allows for a flexible design and fabrication of porous structures, the fabrication of IPCs involves infiltrating the porous body with molten
allowing for the simultaneous tailoring of both the macrostructures and alloy. Two primary variants of melt infiltration techniques are used for
the microstructures (Fig. 15). Indirect FFF may also be used to create this purpose: pressureless or capillarity-driven infiltration [184–186],
non-uniform or functionally graded porous ceramics of varying size, wherein the capillary action acts as the driving force for the melt to be
shape, and connectivity at different heights of the structure. [183] uti spontaneously drawn into the preforms, and pressure-assisted or forced
lized a similar hybrid methodology combining 3D printing with slurry infiltration [36,187–191], wherein an external pressure is applied to
replication and reactive silicon infiltration to fabricate near-net-shaped overcome insufficient wettability between liquid metal and ceramic
macroporous Si–SiC structures. preform. Unless the melt has a near-zero wetting angle with the ceramic
A schematic showing the summary plot of porosities and pore size preform material, an external pressure must be applied to push the melt
ranges of porous ceramic preforms for the processing routes discussed in into the preform. It is advisable to choose an infiltration procedure
Fig. 15. Top view of (a) Porous mullite preforms having different pore shapes and (b) controlled-porosity mullite preforms having different shapes and sizes [182]
(cited images have been reproduced with due permission from the publisher).
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Fig. 18. Optical micrographs of the Al2O3/Al–10Mg IPCs spontaneously infiltrated in (a) 25% N2, (b) 55% N2, and (c) 100% N2 (balance argon) [203] (cited images
have been reproduced with due permission from the publisher).
Fig. 19. SEM micrographs of IPCs made by spontaneous infiltration of Al–10Mg alloy in (a) Alumina foam, (b) Mullite foam, (c) and (d) Spinel foam [120] (cited
images have been reproduced with due permission from the publisher).
spontaneous infiltration of molten Al alloy into porous SiC preforms spontaneous infiltration in [211]. The resultant IPCs retained the
under controlled temperatures of 900–950 οC for 2 h. TiCx/Cu–Cu4Ti lamellar structure of the porous Al2O3–ZrO2 preforms. [80] fabricated
IPCs were synthesized by pressureless infiltration of molten Cu at 1200 Al–Si–Mg/SiC lamellar IPCs by freeze-casting and pressureless infiltra
ο
C into non-stoichiometric TiC0.5 porous preforms that were prepared by tion. The molten Al–12Si–10Mg alloy spontaneously infiltrated into the
in-situ solid-state reaction between Ti and carbon black, together with porous SiC preform with an average infiltration rate of 0.24 mm/min at
using PVB as pore former [145]. Excellent wettability between Cu and 950 ◦ C in an N2 atmosphere. (Cu, Ni)/(75–86 vol%) TiB2 IPCs were
TiC0.5 assisted in spontaneous infiltration. It was observed that the successfully fabricated by an indirect downward pressureless melt
metallic phase of the IPC thus produced contained Cu and a new phase infiltration at 1400–1500 ◦ C in [212].
Cu4Ti, which was formed by the reaction between TiC0.5 and Cu. [210] Pressureless infiltration has also been performed under reactive
fabricated SiC/Al7075 IPCs by pressureless infiltration technique. The conditions. Reactive metal penetration (RMP), referred to by the trade
infiltration was carried out at 800 ◦ C to ensure the melt’s better fluidity. name ONNEX™ [33], is a low-cost reactive infiltration method for
Al–12Si–10Mg/Al2O3–ZrO2 interpenetrating composites with an initial manufacturing metal/ceramic IPCs, in the absence of an external pres
ceramic loading of 30 vol% and different Al2O3/ZrO2 weight ratios (1:9, sure [22,213–216]. It involves a liquid-phase displacement reaction, for
3:7, 5:5, 7:3 and 9:1) were prepared by freeze casting followed by example, between aluminum and silica at 800–1200 ◦ C when a
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net-shaped pure silica glass precursor is immersed into a molten double RMP technique in [222,223]. Two steps were involved - firstly,
aluminum bath. Since silica is thermodynamically unstable in the molten aluminum was reactively penetrated into silica preforms at
presence of aluminum, it gets reduced by it, and alumina forms. The 1200 ◦ C, obtaining an Al(Si)/Al2O3 composite; subsequently, reactive
ceramic precursor is chosen such that its density is significantly lower penetration of Ni was performed in an argon atmosphere at 1700 ◦ C,
than that of alumina so that upon transforming, a volumetric contraction leading to the substitution of Al with NiAl.
occurs. As a result, about 25% open volume is created in alumina in the
form of microscopic voids and cracks [217], which are subsequently 2.2.2. Gas pressure infiltration
wetted and penetrated by the flowing melt. Thus, the molten metal The gas-pressure infiltration technique utilizes pressurized gas,
transgresses and has continued access to fresh precursors so that the usually from an inert gas, as the driving force to overcome the perme
reaction can proceed through the whole ceramic body, i.e., until the ation resistance for the impregnation of molten metal into an open-
SiO2 phase is wholly consumed. The resultant Al2O3/Al interpenetrating porous ceramic preform. As shown schematically in Fig. 20, first, the
phase composite thus formed retains the shape and dimensions of the chamber containing the porous preform and metal billets are evacuated.
silica precursor, except for an isotropic volume shrinkage of around 1%. Next, the temperature inside the chamber is increased to melt the
The silicon precipitated at the infiltration front forms an Al–Si alloy, metallic alloy billets. The melt covers the porous preform completely,
thereby further improving the wettability and the process kinetics. and subsequently, a pre-set gas pressure is applied to infiltrate the melt
Cordierite [218], mullite, and other silicate ceramics [219,220] can also inside the pores of the preforms [187,224–234]. The initial vacuum is
be used as precursor materials. essential to remove entrapped gases from within the porous preform,
A comparative study on the fabrication of Al2O3/Al IPCs by reactive which otherwise would pose a barrier to melt infiltration. For successful
melt penetration (RMP) using SiO2 preform and direct pressureless infiltration, the process parameters such as temperature, applied pres
infiltration into Al2O3 preforms was reported in [221]. To ensure sure, and pressure application time need to be carefully selected. Gas
reasonable wetting conditions, Si and Mg doping was applied to the pressure infiltration requires a lower infiltration temperature compared
aluminum alloy along with a constant supply of N2 gas. It has been found to the pressureless infiltration technique, as due to the added gas pres
out that the infiltration kinetics was better in the case of the RMP route sure, the dependence on spontaneous wetting is lesser, and so the tem
with an infiltration rate of about 0.6 mm/h against a rate of 0.35 mm/h perature needs to be only high enough to ensure complete alloy melting.
for the direct pressureless infiltration route. [173] fabricated Al/alu With the pressure chamber’s low acquisition cost, increased operational
mina IPCs by in-situ pressureless reactive metal infiltration of molten flexibility, and precise control of the process parameters, gas
Al5052 alloy into porous silica preforms produced by the fused depo pressure-assisted melt infiltration is an ideal route for economically
sition of ceramics (acronym FDC or FFF) process. The reactive infiltra producing near-net-shaped IPCs. The only added cost is the cost of the
tion was carried out at 1150 ◦ C for 1 h to ensure the complete reaction of pressurized gas. Also, because of the short contact time of the molten
the silica with the aluminum alloy and the formation of α-Al2O3. [182] alloy and ceramic preform, non-coated preforms can be directly used for
utilized the same methodology to prepare aluminum/alumina IPCs by infiltration.
reactive infiltration of aluminum into porous mullite preforms at Al/Al2O3 (70 vol%) IPCs with a highly regular architecture was
1050 ◦ C. Near-net shaped NiAl(Si)/Al2O3 IPCs were fabricated by the produced by gas-pressure infiltration of molten aluminum into an Al2O3
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tower in [176,235]. The Al2O3 tower preform with periodic cubic porous ceramic preform. Once the pre-heated ceramic preform is placed
symmetry of simple tetragonal (ST) shape was prepared by the inside the die cavity, molten alloy is poured over the preform. The entire
direct-write assembly. Pure aluminum melt infiltration was performed system is pressurized under a hydraulic upper punch to the maximum
at 750◦ C under an argon pressure of 3.5 MPa, and the resulting IPC was squeeze pressure (Fig. 22), and the pressure is maintained during the
directionally solidified. [236] manufactured Ni3Al/Al2O3 (70–85 vol%) solidification process. After the completion of the alloy solidification,
IPCs by the gas pressure infiltration method. The infiltration was the composite thus formed is ejected from the die. The high squeeze
executed at 1550 ◦ C under an Ar gas pressure of 10 MPa for about pressures employed in the process enable deep melt penetration and
30–210 min. [237] fabricated SiC/Al IPCs at a temperature of 750 ◦ C filling up of tiny micropores in the preform’s cell walls.
and a gas pressure of 10 MPa. Molten Al6063 alloy was infiltrated into The squeeze infiltration process consists of three visible phases [194,
3-D porous SiC preform, prepared using a sacrificial pore-forming agent. 239]. In the preliminary phase, the ceramic preform’s threshold capil
Inert gas pressure-assisted infiltration method was used to produce lary resistance must be surpassed by the externally applied pressure for
Al12Si/Al2O3 IPCs in [187]. At 750 ◦ C and 4–10 MPa Ar gas pressure, initiating the melt infiltration. Following that, a stable melt flow phase
molten Al12Si alloy completely covered the porous Al2O3 preform to occurs during which the pressure increases linearly with respect to
facilitate infiltration. Optical images and scanning electron micrograph infiltration time until the molten alloy has filled the preform. Towards
of the fabricated IPC are shown in Fig. 21. The fabricated composites the end of this phase, the pressure rises to the maximum level, i.e.,
were of very high quality, with only very few micropores remaining. penetrating-through pressure. Subsequently, in the third and final
[208] infiltrated Al–13Si–9Mg alloy into wood-derived porous SiC or phase, the residual air is removed with micropores, too, getting filled up
bio-SiC preforms. Infiltration was carried out at a temperature of 750 ◦ C with the molten alloy. It is critical to customize the preform’s porosity to
under 3.5 MPa argon gas pressure. Al/TiC IPCs with varied ceramic achieve a high permeability and an adequate compressive strength. High
contents (15, 25, and 35 vol%) were fabricated in [238]. Ar gas pressure permeability is advantageous because it reduces the hydrodynamic
of 2 MPa was used for aluminum melt infiltration. A similar gas-pressure pressure and hence the melt flow resistance; however, too high a
infiltration procedure was employed in [81] to fabricate lamellar porosity results in low compressive strength, leading to preform damage
TiC/Al–7Si–5Cu IPCs. The porous scaffolds had varying solid content in during the infiltration.
the range of 25–35 vol% before infiltration. It was observed that the Selection of the correct applied pressure and other squeeze-casting
formation of Al4C3 at the interface improved the wettability and facili parameters is essential for fabricating near-net-shaped IPCs with a
tated the spontaneous infiltration of molten Al alloy into the porous TiC defined microstructure. Although preheating of the ceramic preform is
preforms. essential to avoid any premature melt solidification, excessively high
temperatures would lead to undesirable chemical reactions at the metal/
2.2.3. Squeeze infiltration ceramic interface that decelerate the squeeze infiltration kinetics [240].
The squeeze infiltration technique utilizes high pressure, typically in On the flip side, the generation of high squeeze pressures needed in the
the range of 50–100 MPa, for rapid infiltration of liquid alloy into a process makes the use of heavy equipment inevitable. Although a high
Fig. 21. Optical micrographs of alumina/Al12Si IPC fabricated by gas pressure infiltration – (a) at 50x and (b) at 1000x, and (c) SEM image of the composite [187]
(cited images have been reproduced with due permission from the publisher).
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applied pressure helps to avoid porosity in the final composite, it may pulse electric current sintering (PECS) method (Fig. 24a) under addi
also lead to deformation or cracking of the porous ceramic preform. tional applied pressure. A porous SiC preform, prepared by conventional
Fig. 23 shows typical micrographs of squeeze-cast SiC/2024Al [79] and sintering, was sandwiched between two aluminum discs. Then, pulsed
alumina/Al12Si [133] IPCs. Fig. 23a-d depicts optical micrographs of electric current was applied at 660 ◦ C for 2 min under a uniaxial pressure
lamellar metal/ceramic IPCs, fabricated from freeze-cast preforms of 20 MPa to carry out aluminum melt infiltration. This method’s main
having different lamellar spacings with the same reinforcement volume benefit is its rapid fabrication of dense materials at low temperatures,
fraction. The alumina preform was synthesized by pyrolyzing the PFAs and at relatively short processing periods.
and sintering the green compact, and it had both micropores and mac Table 4 lists some further research works involving squeeze-casting
ropores, which were melt-penetrated during squeeze infiltration of ceramic preforms for IPC fabrication.
(Fig. 23e and f).
Two different freezing temperatures were used in [248] to fabricate 2.2.4. Vacuum infiltration
the alumina preforms, and the micrographs show the microstructure of The vacuum infiltration technique involves melt infiltration into
the faces normal to the freezing direction. For preforms freeze-cast at porous ceramic preforms under a negative suction pressure (Fig. 25).
− 10 ◦ C, a coarser structure consisting of lamellar domains having di Firstly, the metallic alloy in the crucible is melted in a resistance furnace.
mensions in millimetre range is observed. In comparison, the micro Simultaneously, a constant N2 gas supply is given to the porous ceramic
structure of the preforms freeze-cast at − 30 ◦ C is finer, and the domains preform. The vacuum is then turned on, and the ceramic preforms are
are much smaller, and lamellae are significantly thinner. Both micro immersed in the melt. After the completion of infiltration, the composite
graphs appear to be fully dense, suggesting good infiltration and a lack material is removed from the unit and air-cooled to room temperature
of significant residual porosity. [241] synthesized SiC/Al IPCs by a novel [249]. The applied vacuum, infiltration time, and temperature are the
Fig. 23. Micrographs of the squeeze-cast SiC/2024Al (a–d) [79] and alumina/Al12Si IPCs: (e) Light optical micrograph and (f) SEM micrograph [133] (cited images
have been reproduced with due permission from the publisher).
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Fig. 24. Schematic of the melt infiltration process by (a) Pulse electric current sintering method (Based on [241]) and (b) Centrifugal casting method (Based
on [11]).
Table 4
Summary of research carried out on IPCs fabricated by squeeze infiltration technique.
Ceramic Preform fabrication method Metallic Preform & die pre-heating temperature Molten alloy temperature Infiltration pressure Ref
alloy (◦ C) (◦ C) (MPa)
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Fig. 26. (a), (b) SEM images of zirconia/Al IPC cross-section perpendicular to the freezing direction, and (c), (d) SEM images of zirconia/Al IPC sample cross-section
parallel to the freezing direction [253]. Arrows show the presence of defects. (cited images have been reproduced with due permission from the publisher).
modifications of the methods already discussed, have been developed horn are the critical process parameters. It has been discovered that
for IPC fabrication. A brief review of these latest developments is pro when a system is subjected to ultrasonic vibration, the contact angle
vided in this section. decreases, improving wettability [255]. Magnesium’s addition to
In the ultrasonic infiltration method, acoustic cavitation, i.e., bub aluminum alloy melt further improves wettability and thereby the
bles, are generated when the molten alloy is ultrasonically stimulated infiltration kinetics [256]. [254] fabricated metal/ceramic IPCs by
through a horn in the melt. The gases dissolved in the melt and those ultrasonic-assisted infiltration of molten Zn–5Al alloy at 500 ◦ C into
entrapped in the ceramic foam form the bubble nuclei. When such a freeze-cast ZrB2–SiC. The ultrasonication system was operated at a fre
bubble collapses, a pressure wave is generated near the melt, thereby quency of 20 kHz and a power of 1 kW. It has been observed that an
assisting in the molten alloy penetration into the porous ceramic pre ultrasonication duration of 300 s efficiently improved wettability and
form. Ultrasonic power of the transducer and the hole diameter in the facilitated infiltration through the ultrasonic capillary and cavitation.
Fig. 27. Ultrasonic-assisted infiltration mechanism: (a) Prior to ultrasonication; (b) Infiltration process [254] (cited images have been reproduced with due
permission from the publisher).
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Fig. 27 demonstrates that ultrasonic-assisted infiltration is a feasible and and distortion of the ceramic lamellae along with a significant reduction
promising method for the fabrication of non-wetting metal/ceramic of properties [248]. Metal-ceramic IPCs were fabricated by pressure die
IPCs. casting of Al9Si3Cu alloy melt into porous Al2O3 preforms in [188].
In the Lorentz force infiltration technique, molten alloy is infiltrated A novel P/M technique using aluminum powder and silica fiber
into the porous ceramic preform under electromagnetic force. These needles as raw materials, followed by hot extrusion and heat treatment
forces are generated by exposing the melt to a high-frequency transient at 600 ◦ C, was employed to fabricate Al–Si/Al2O3 IPCs in [263]. Inter
magnetic field, which causes strong eddy currents to form in the melt penetrating phases were produced during the heat treatment as a result
[257]. These induced eddy currents interact with the applied pulsating of an intense interfacial reaction. The original fiber morphology was
magnetic field to generate a Lorentz force density field on the con retained in the final composite [264,265]. fabricated inter
ducting melt, thereby allowing it to penetrate the preform. The intensity metallic/ceramic IPCs by a novel pressureless reaction sintering method,
and frequency of the magnetic pulse and the number of discharges are during which attrition milled metal oxides, and aluminum powder
the critical process parameters. compacts reacted to form metal-aluminide/alumina composites ac
The centrifugal infiltration technique utilizes a centrifugal force to cording to the reaction,
infiltrate molten alloy into porous preforms (Fig. 28); the schematic of
the centrifugal casting method is given in Fig. 24b. In this method, the MeaOb + (2b/3 + c) Al → MeaAlc + (b/3) Al2O3
porous ceramic preform is placed at the end of a mold having an elon Metal oxides such as TiO2, Fe2O3, Nb2O5 were used as starting ma
gated runner loaded with the melt to be infiltrated. High rotational terials. Mechanical alloying of the powder mixtures was carried out in a
speeds of the runner generate a centrifugal pressure (up to 15 MPa) to high-energy planetary ball mill under an argon atmosphere. Pressureless
overcome the threshold pressure for the penetration of melt into the sintering was performed under a carefully controlled vacuum of 0.1 Pa
preform, and the metal head in the runner decreases with the progres at 1300–1530 ◦ C, during which the metal oxide reduction by aluminum
sion of infiltration [258]. Because of the complete infiltration, this occurred. It was reported that because of the highly exothermic nature
method is instrumental in minimizing the quantity of molten alloy in the of the reaction, high composite densification could be achieved through
runner and avoiding a large amount of scrap metal, i.e., to achieve careful process control at temperatures in the range of 400–800 ◦ C.
near-net-shape processing. Alumina-Aluminum alloy IPCs were fabri [266] demonstrated solid-state binder jet additive manufacturing
cated by the centrifugal infiltration method in [86,259–261]. Porous (acronym BJAM or BJT) and reactive sintering post-processing for
alumina preforms, produced by the polymer replication method, were fabricating metal/ceramic IPCs. During reactive sintering of Ni-based
pre-heated to 250–350 ◦ C and then centrifugally infiltrated with molten super alloy INCONEL 625, a reaction between the Cr alloying element
Al12Si alloy at 720–740 ◦ C using a rotational velocity of 4000–4200 in the alloy and the binder forms an interconnected carbide reinforcing
rpm. Composite castings with a percolation structure were obtained as a phase Cr3C2 throughout the Ni matrix.
result of the centrifugal force acting on the liquid Al12Si alloy surface.
Furthermore, thorough examinations using SEM and EDS demonstrated
3. Properties of IPCs
the complete filling of the cells, as well as the absence of structural
defects and discontinuities at the metal-ceramic interface [261].
Several studies have carried out systematic studies of different
The pressure die infiltration technique involves melt penetration into
physical, mechanical, and thermal properties of IPCs. A detailed sum
a porous ceramic preform positioned inside a solid die by applying
mary of the various properties of IPCs is provided in this section. The
pressure using a movable piston. The infiltration speed, applied piston
section is divided into two subsections:
pressure, and die temperature are the most critical process parameters
Section 3.1 - thorough description of various properties as a function
[262]. One of the significant benefits of this method is its ability to
of ceramic content and other processing and structural parameters is
fabricate, with great precision, complex geometry components. How
provided in this section. Further, this section also provides correlations
ever, since this method’s infiltration speed is relatively higher than that
of Young’s modulus, and CTE of IPCs with relevant micromechanical
of the squeeze-casting and gas pressure infiltration process, IPCs fabri
models.
cated by the pressure die infiltration method often exhibit fragmentation
Section 3.2 – for different property combinations, domains for IPCs
have been created in Ashby material property maps to compare with
other material families. Further, the concept of material indices has been
discussed to evaluate the performance capability of IPCs for various
design and loading conditions.
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manufactured IPC, which drastically lowers the FS value [177]. The use
of refractory metals and ceramic reinforcement with similar CTEs will
lead to strong interfacial bonding in IPCs and high FS values [34]. The
presence of a substantial amount of residual porosity in IPCs [38,222]
significantly reduces the FS values as compared to the non-porous IPCs
[215]. Further, IPCs with interconnected pores show very low FS values.
Interconnected pores act as large flaws and provide local stress con
centrations and favorable crack propagation paths, thus lowering the FS
[25]. Besides, the existence of a brittle ceramic network around the
reinforcement grains provides favorable paths for crack propagation in a
brittle manner with lowering the FS [229]. In [145], the intermetallic’s
special root structure in the interior of the TiC0.5 grains resulted in
higher FS values. In IPCs fabricated using ultrasonic-assisted infiltration,
with increasing the duration of ultrasonication, micro defects like voids
and interfacial debonding can be avoided, and correspondingly, FS in
Fig. 30. Plot showing the correlation between the IPC Young’s modulus values
with theoretical model predictions.
creases [254]. Optimization of the preform pore size is an important
parameter, which affects the FS of the IPCs. A decrease in preform pore
size enhances the FS; however, after a certain pore size, large inner
stresses will be induced at the interface that deteriorates the interface
combination. Moreover, at too small a pore size, infiltration becomes
difficult, and correspondingly, the FS decreases [245]. The FS values of
the IPCs fabricated using freeze-cast ceramic preforms show significant
anisotropy, with higher values along the freezing direction of the pre
form (marked as longitudinal) than in the perpendicular direction
(marked as transverse) [79,225]. Further, the finer lamellar micro
structure leads to an improvement in FS values [79]. The FS values of the
IPCs also depend on the preform’s strength; increasing with increasing
strength of the preform [42]. Finally, aging heat treatment also affects
the strength of the IPC. [204] reported higher FS after T6 treatment in
IPCs fabricated via pressureless infiltration due to the precipitation of
Mg2Si and a cleaner interface.
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of a propagating crack decreases, and correspondingly the KIC value the lesser probability of the presence of a critical defect [176,248,278].
decreases. This phenomenon also controlled the reduction in flexural The difficulty in infiltrating the molten alloy into ceramic preforms
strength of IPCs at high ceramic contents, as reported earlier. Besides, using pressureless infiltration may result in a significant amount of re
the KIC of the composites depends strongly on the orientation of the sidual porosity in the fabricated IPC, thereby resulting in a lower CS
notch to the interconnected metallic/intermetallic particles. Parallel [19]. As already discussed for FS, the use of ultrasonication during
orientation results in higher KIC values than normal orientation. Another infiltration can significantly improve the wettability of the system and
reason for higher toughness values may be attributed to the large notch assists in spontaneous infiltration through the ultrasonic capillary and
width, which leads to an overestimation of the KIC values [35]. Apart cavitation actions. Moreover, by increasing the duration of the ultra
from the microstructure alone, the type of thermal residual stresses and sonication, the microdefects like voids and interfacial debonding can be
contiguity of the ceramic phase also influence the KIC. High tensile re avoided, resulting in improved CS [254].
sidual stress and low contiguity of ceramic phase cause the crack to Ref. [248,278] have shown that the IPCs fabricated using freeze-cast
propagate in the metallic phase and at the interface, leading to a good ceramic preforms exhibits a pronounced anisotropy. Due to the pre
KIC value [24]. Refinement of the lamellae thickness improves the KIC of dominantly continuous ceramic lamellae along the freezing direction,
IPCs due to the lower probability of the existence of a critical defect in the compressive strength along this direction is much higher. Although
finer ceramic lamellae. Further, the incorporation of brittle elements much lower CS is observed along transverse directions, due to the
into the metallic matrix lowers the KIC of IPCs [234]. Ref. [79,225] show presence of ceramic bridges joining the adjacent lamellae, the
that the KIC values of the IPCs fabricated using freeze-cast ceramic compressive strength improves in comparison to the values predicted by
preforms show significant anisotropy, with higher values along the micromechanical models. In [80], the addition of mixed oxide
freezing direction of the preform than in the normal direction. (Al2O3–MgO) into the lamellar SiC preforms has resulted in enhanced
As with FS, the combination of refractory metals and ceramic rein CS. This was attributed to the presence of chemically formed rein
forcement having similar CTEs leads to strong interfacial bonds, thereby forcement phases such as MgAl2O4 and MgO, thereby improving the
improving the fracture toughness of the IPC [34]. The existence of a interfacial bonding between the ceramic and metallic alloy phases.
brittle network around reinforcement grains may reduce the metal Similar to FS, improper sintering of the ceramic reinforcement in pow
bridging effect, and correspondingly, cracks may propagate in a brittle der injection molding leads to voids in the composite, and if the metallic
manner along this network, resulting in lower KIC values [229]. Further, fraction is too little to fill these voids, pores result. This leads to the
the presence of a pore network interconnected in all three dimensions lowering of the CS values at large ceramic contents [23]. Further, the CS
provides a favorable path for crack propagation, significantly reducing of IPC can be varied significantly by changing the morphology of the
the KIC of the IPC [25]. Apart from the volume fraction of ceramic pores in the ceramic preform used for infiltration. Preforms consisting of
reinforcement alone, the intrinsic KIC of the reinforcement is also an a combination of large pores along with a high volume fraction of small
important factor affecting the toughness of IPCs. Generally, the use of pores result in good infiltration of the molten metallic alloy, resulting in
high KIC ceramic as reinforcement in IPCs will result in higher toughness high CS [226]. Lastly, the incorporation of SiC particles into the SiC
[186]. Furthermore, the presence of a special root structure of inter foam/Al IPC has resulted in higher CS than composites reinforced solely
metallic in the interior of the TiC0.5 further increases the KIC by plastic by the SiC particles [243].
deformation during the crack propagation [145].
3.1.5. Coefficient of thermal expansion (CTE)
3.1.4. Compressive strength (CS) The thermal expansion behavior of IPCs has been studied extensively
Fig. 33 plots the compressive strength of IPCs against the ceramic due to their vast potentials for thermal management applications in the
content. Similar to the FS data in Fig. 31, data for the CS also display a electronic packaging industry [279,280], as well as their lower CTE
large scatter. However, as the CS of ceramics is higher than their FS, the values than particle reinforced MMCs [30]. The study of thermal
IPCs also possess a higher CS. Furthermore, as with FS, apart from only expansion behavior of IPCs, or in general MMCs, is inherently compli
the ceramic content, distribution of the ceramic and metallic phases in cated due to the interplay between numerous factors such as phase ar
the IPC, as well as preform and IPC fabrication methods, have a strong chitecture, composite microstructure, reinforcement volume fraction,
influence on the CS. Some of these aspects are discussed below. presence of processing induced thermal residual stress, content of mi
Generally, preforms with a considerable degree of residual closed cropores and defects in the microstructure, initiation of plastic defor
porosity and cracks result in significant residual porosity and cracks in mation and/or damage during thermal expansion, etc. Most of these
the manufactured IPC, and drastically lowers the CS value [177]. Be factors are extremely difficult to control, and several operate concur
sides, the microstructure of the ceramic preform also has a strong in rently, making the overall material behavior rather complicated. A
fluence – a finer microstructure generally results in a higher CS due to summary plot showing the CTE of IPCs vs. ceramic content is shown in
Fig. 33. Summary plot of the results available for compressive strength vs. Fig. 34. Summary plot of the results available for CTE vs. ceramic content for
ceramic content for IPCs from different research articles. IPCs from different research articles.
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Fig. 34. Fig. 35. Among the models considered, the rule of mixtures (ROM)
The CTE of the IPCs strongly depends upon the type and volume model follows the simple mixing principle. While the Kerner model
fraction of ceramic reinforcement. Generally, due to the much lower corresponds to composites with discontinuous spherical reinforcements,
CTE of the ceramic phase, with increasing ceramic content, CTE of the the Turner model represents the composites having a percolating rein
IPC decreases. As evident from Fig. 34, compared to Al2O3 IPCs, lower forcement morphology representative for IPCs. A detailed description of
CTEs have been reported for the IPCs with SiC reinforcement. This can these models can be found in [281–283]. For the model calculations, as
be attributed to the much lower CTE value of SiC in comparison to Al2O3 with E, the matrix is always taken as pure Al, and the material properties
(see Table 5). Among the results shown in this figure, lowest CTEs are of the constituent phases used for calculations are given in Table 5.
observed in IPCs reinforced with diamond [37]. This can be attributed to Fig. 35 shows that the CTE values of the alumina reinforced IPCs fit
the very low intrinsic CTE of diamond, which imposes a strong very well between Kerner and Turner models, whereas the Turner model
constraint on the thermal expansion of the matrix and lowers the CTE. fits best to the reported values for SiC reinforced IPCs. It is worth
For similar ceramic content, the CTE value of the IPC in [187] is considering that most of the works whose values are reported here had
lower than in [24]. This can be attributed to the different metallic an Al-alloy matrix. The CTE of these alloys is almost always lower than
matrices used in these IPCs. Alloying of the metallic matrix with ele pure Al, and correspondingly, the model curves will be shifted further
ments having a lower CTE than the metal results in a lower CTE in the downward. Additionally, several SiC-based IPCs have CTE much lower
IPC. Besides, the microstructure of the IPCs also has a strong influence than even the Turner model, which cannot be attributed solely to the
on the expansion behavior. Microstructure with numerous and large metallic alloy with a lower CTE. This can probably be attributed to the
metallic alloy-rich regions free from ceramic phase experience reduced presence of microvoids in IPCs, resulting from incomplete infiltration,
restraining effect of the reinforcing phase, and generally display a higher interfacial debonding because of solidification shrinkage, and thermal
CTE [187]. Also, the presence of a considerable degree of porosity in the residual stresses due to CTE mismatch between metallic matrix and
manufactured IPC lowers the CTE value due to the filling up of these reinforcement. As discussed elaborately by Balch et al. [284], these
pores by the plastically deforming metallic alloy during the thermal microvoids help in relieving the local constraint, and plastically
expansion [177]. Processing and/or microstructure induced anisotropy deformed metal expands into these voids, thus lowering the CTE of the
in preform stiffness have been reported to lead to strong CTE anisot IPCs below the model predictions.
ropies in IPC. Higher stiffness along the longitudinal direction of the
preform than in the transverse direction restricts the thermal expansion 3.1.6. Thermal conductivity (TC)
of the composite and results in lower CTE [31,32]. For thermal management applications, along with a low CTE of the
The use of ceramic preform fabricated using robotic deposition for material, a high thermal conductivity (TC) is essential to ensure good
IPC manufacturing results in lower CTE because of the uniform three- heat dissipation. IPCs with SiC reinforcement have been deemed as
dimensional spatial periodicity of the preform, which provides effec potential candidates due to the low CTE and high TC of SiC. Fig. 36 plots
tive restrainment for thermal expansion of composite [176]. The sig the TC of several IPCs from different research papers vs. their corre
nificant fluctuations in the CTE values in [25] can be attributed to the sponding ceramic content.
microstructural variations. The IPC fabrication using a ceramic preform Due to the lack of sufficient data and pronounced scatter in TC of
coated with a lower CTE metal results in a lower CTE than an un-coated IPCs, establishing a definite trend is difficult. However, owing to the
ceramic preform [36]. During heating of the composite, the plastically higher TC of SiC over Al2O3, for similar ceramic content, IPCs reinforced
deformed metal expands into the pores, thus reducing the CTE of IPC. with SiC possess higher TC. At very high ceramic content in the pre
Proper control of the preform pore size is a necessary parameter, which forms, the size of the interconnected pore channel decreases. Corre
strongly affects the CTE of the IPC. With a reduction of pore size, the spondingly, complete infiltration of the molten metal in the preform
constraining effect on the matrix thermal expansion increases, thereby becomes difficult, and uninfiltrated regions may remain in the IPC,
reducing the CTE of the IPC [245]. However, with a further reduction of lowering the TC of the composite [237]. Ref. [204] reported an increase
the pore size, large inner stresses will be induced at the interface, which in TC after the T6 treatment. This was attributed to an improved
may deteriorate the interface region. Further, at too small pore sizes, microstructure of the alloy matrix and a cleaner interface. Both these
infiltration becomes difficult [245]. Further, infiltration of the preform factors would significantly reduce the electron scattering and improve
with lower CTE metal alloy remarkably reduces the composite CTE the TC of the composite. Further, [36] reported a reduction of the IPC’s
[193]. TC as a result of the pre-coating of the preform with lower TC metal. As
To further understand the thermal expansion behavior of the IPCs, with other properties already discussed, TC of IPCs fabricated using
the CTE values of the alumina reinforced, and SiC reinforced IPCs are preforms having directional porosity exhibit a pronounced anisotropy
compared with three well-established micromechanical models in [184,193]. Generally, the continuous channels for the transmission of
Fig. 35. Plot showing the correlation between the reviewed CTE values with Fig. 36. Summary plot of the results available for thermal conductivity vs.
theoretical model predictions. ceramic content for IPCs from different research articles.
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Fig. 38. Modified strength vs. density plot [297]. Fig. 40. Modified specific modulus vs. specific strength plot [297].
c) Young’s modulus vs. strength (Fig. 39) and specific modulus vs.
specific strength (Fig. 40)
denotes the ability of a material to absorb energy while still elastic, and a
higher than ceramics, and several values are even comparable to those of
high value of this parameter is important to make springs. Fig. 39 shows
metals. For conventional design of structural components, a KIC mini
that due to their higher E, IPCs are inferior to metals in this respect.
mum of 20 MPa√m is often considered as a minimum requirement, and
some IPCs can actually satisfy this criterion, albeit at a significantly
d) Fracture toughness vs. modulus plot (Fig. 41) ( )
/
reduced E. The parameter GIC ≈ K2Ic E are denoted as toughness
Consideration of fracture toughness (KIC) is of fundamental interest
for damage tolerant designs. For IPCs, the comparison of KIC values with contours with a slope of 0.5, and this is a measure of the apparent
ceramics has tremendous practical relevance. Ceramics are very brittle fracture surface energy. The plot shows that the toughness of IPCs is
due to their low KIC, and if IPCs can improve that, the application fields almost two orders of magnitude higher than the common ceramics.
can be expanded significantly. Fig. 41 shows that while for IPCs, KIC and However, the plot shows that both the toughness and fracture toughness
E are inversely proportional to each other, generally, KIC of IPCs are of particle reinforced MMCs are higher than IPCs.
Fig. 39. Modified Young’s modulus vs. strength plot [297]. Fig. 42. Modified fracture toughness vs. strength plot [297].
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bearing applications, without affecting their strength and stiffness. PRCs Metals Ceramics
However, solely in terms of fracture resistant behavior, IPCs are inferior E vs. ρ Superior Superior Comparable
to particle reinforced MMCs. FS vs. ρ Comparable Comparable Comparable
E vs. FS Superior Comparable Comparable
Specific E vs. specific FS Superior Superior Comparable
f) CTE vs. thermal conductivity plot (Fig. 43)
KIC vs. E Slightly inferior Comparable Superior
KIC vs. FS Comparable Slightly inferior Superior
The CTE vs. thermal conductivity plot is of fundamental interest for CTE vs. TC Superior Superior Comparable
applications requiring frequent temperature inversions. Specifically for
thermal management applications, the material should ideally have a
low CTE and high thermal conductivity for good thermal shock resis future research are identified and discussed elaborately. A schematic of
tance. Contours of constant (λ/α) are plotted in Fig. 43, and a high value the brief layout showing the important future trends for IPCs is given in
of this parameter is essential for good thermal shock resistance. Metals, Fig. 44.
although having a high thermal conductivity, generally have a high CTE, As discussed in section 2 of this review, fabrication of IPCs is a
too. The plot shows that IPCs outperform most metals, and even particle multistep process and it is essential to modernize and standardize the
reinforced MMCs, both due to their lower CTE and higher (λ/α). processing technologies into fully automated assembly lines to ensure
Based on this thorough review, tabular comparisons of the perfor economical production of IPCs with reproducible microstructure and
mance of IPCs with respect to other relevant material classes discussed properties. Thankfully, due to the growing interest in this field, an en
in this work are given in Table 6 and Table 7. gineer’s toolkit for articulating the structure/property correlations in
IPCs has evolved considerably in both analytical and experimental
4. Future research directions methods. The advent of modern technologies such as micro computed
tomography, advanced ultrasonic methods, etc., has made it possible for
This article has made an effort to present an account of the different the visualization, characterization, and representation of the geomet
processing techniques for fabricating metal/ceramic IPCs, emphasizing rical parameters and the topological relationships between the different
the methods used for manufacturing the porous ceramic preforms and constituents. The discussion of section 3 shows that the percolating
the various melt infiltration strategies. Also, the different thermo- three-dimensional network structure of IPC is very effective in over
mechanical properties of IPCs affecting their performance are dis coming the issue of strength-toughness inversion observed in several
cussed in detail, along with their detailed comparison with other rele conventional materials. The advantage of phase interconnectivity is
vant existing materials, using Ashby plots. Although significant progress particularly felt in specific applications where two or more differing
has already been achieved in developing interpenetrating phase com properties, such as mechanical strength and electrical conductivity, can
posite materials, a lot of future research is still needed to transcend them be optimized in the same component. The exploration of other syner
from materials having high potentials to materials with definite indus gistic properties that rely on phase interconnectivity necessitates the
trial applications. In this section, some potential areas for directing development of various IPCs and systematic analysis of their properties.
Although the characteristics of IPCs are fundamentally dependent
upon the microstructure of the porous preforms, producing porous
bodies with a regular and controllable pore structure using the existing
fabrication routes is challenging. Further research is required to reduce
the number of processing stages, usage of only biocompatible and non-
toxic reagents, developing processing techniques that do not need sub
sequent pyrolysis and sintering, and, of course, reduce the costs asso
ciated with the porous ceramic synthesis. Advancements in additive
manufacturing techniques can fabricate preforms with well-controlled
architectures, including porosity, periodicity, and the topology and
spatial distribution of composite structures based upon user-defined
CAD designs. Stereolithography-based methods using photosensitive
polymer solutions could be used. Such methods can be used more easily
to construct periodic IPCs with improved mechanical properties. The
application of fluid mechanics to develop reliable simulation of the
molten alloy flow through the pores of the preforms using different melt
infiltration methods can further aid in developing optimum processing
parameters.
Fig. 43. Modified CTE vs. thermal conductivity plot [297].
25
N. Kota et al. Ceramics International xxx (xxxx) xxx
Further research can be pursued on specialized configurations of porous ceramic preforms and the various melt infiltration strategies.
IPCs, such as those with hierarchical and gradient structures to suc Detailed property analyses carried out within the scope of this review
cessfully fabricate functionally graded (FG) IPCs. Although functionally highlights the ability to fabricate IPCs with a vast range of properties for
graded materials are subject to extensive current research [332,333], the same material systems by varying the composition and microstruc
IPCs with graded structures are still at a very rudimentary stage. The ture distributions. Systematic plotting of the reviewed IPC properties in
development and subsequent characterization of hybrid metal/ceramic several Ashby material property maps, as well as the use of contours of
IPCs, consisting of more than two constituent phases for different material indices has made it possible to compare the IPCs with metals,
properties, has further potentials. IPCs fabricated using preforms pro ceramics, and particle reinforced MMCs, the materials which IPCs could
duced from nano-sized ceramic particles could reveal some interesting potentially replace in various applications. Finally, several potentially
results concerning the melt infiltration kinetics, interfacial behavior, significant areas for future IPCs studies have been identified.
bonding strength at the metal-ceramic interface, and overall composite
properties. Declaration of competing interest
Secondary processing routes, such as joining and machining opera
tions of metal/ceramic IPCs with a 3-D continuous network structure, The authors declare that they have no known competing financial
are going to be challenging due to the vastly different thermal, physical, interests or personal relationships that could have appeared to influence
and mechanical properties of the constituents and the presence of a large the work reported in this paper.
volume fraction of hard ceramic reinforcements. Although electric
discharge machining is commonly used to cut metallic materials, it is Acknowledgement
often difficult in MMCs due to the low electrical conductivity of many
ceramic material components. So, there is a compelling need to develop The work has been funded by the Indian Institute of Technology
advanced joining and machining techniques. Near-net shaping of com Kharagpur, India under ISIRD grant number "HCT".
ponents is going to be one viable solution for the problem of challenging
machining.
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