Unit 1_Chapter 3

Metal and Ceramic Matrix Composites

Content Suggested Additional reading
Types of MMCs, base metals selection; 3.1_Metal matrix composites – From science
important metallic matrices to technological significance;
Processing-liquid state and solid state
processes 3.2_ Characteristic Behaviour of Aluminium
Interfaces in MMCs; Need for Metal Matrix Composites: A Review;
production of MMC’s and its
applications. 3.3_Recent progress in production of metal
Types of CMCs, processing of CMCs-cold matrix composites by stir casting -An
pressing and sintering, hot pressing, Overview.
reaction bonding processes.
Fabricating processes- Liquid and solid
state processes, Applications of CMCs.

3.1_Metal matrix composites – From science to technological significance; D.B.Miracle,

Composites Science and Technology, Volume 65, Issues 15–16, December 2005, Pages
2526-2540 [https://www.sciencedirect.com/science/article/abs/pii/S0266353805002058]

3.2_ Characteristic Behaviour of Aluminium Metal Matrix Composites: A Review; Manish

Shukla et.al.
[https://www.researchgate.net/profile/Dr_Mohan_Pradhan2/publication/323988729_Characteristic
_behaviour_of_aluminium_metal_matrix_composites_A_review/links/5dca64c5458515143503d835
/Characteristic-behaviour-of-aluminium-metal-matrix-composites-A-review.pdf]

3.3_Recent progress in production of metal matrix composites by stir casting -An

Overview.[ https://www.sciencedirect.com/science/article/pii/S2214785319335886]
Metal and Ceramic Matrix Composites :

Introduction, types of matrix and reinforcements:

Topic outcomes:
The topic outcomes are as following:
1. List the various types of MMC’s and explain the significance of various
matrices and reinforcements used.
2. Discuss various base metals and their selection criteria.
3. Discuss the importance of MMC’s as candidate materials in aerospace
and automotive domain.
4. Discuss the influence of process parameters in various processes used
for fabricating CMCs.
5. Justify that CMC’s can be tailored to get the desired directional
properties.

Metal Matrix Composite (MMC) is a material consisting of a metallic matrix combined with

a ceramic (oxides, carbides) or metallic (lead, tungsten, molybdenum) dispersed phase.

 Aluminum Matrix Composites (AMC)

 Magnesium Matrix Composite

 Titanium Matrix Composite

 Copper Matrix Composites

Base metals selection; How and Why?

Based on the application requirements, for ex. High strength even at elevated temperatures; High
stiffness (modulus of elasticity); Low density; etc. the Properties of Matrix materials are chosen.

 Aluminum Matrix Composites (AMC): This is the widest group of Metal Matrix Composites.
Matrices of Aluminum Matrix Composites are usually based on aluminum-silicon (Al-Si) alloys and on
the alloys of 2xxx and 6xxx series.
Aluminum Matrix Composites (AMC) are reinforced by:
  Alumina (Al2O3) or silicon carbide (SiC) particles (particulate Composites) in amounts 15-70
vol%;
 Continuous fibers of alumina, silicon carbide, Graphite (long-fiber reinforced composites);
 Discontinuous fibers of alumina (short-fiber reinforced composites);
Aluminum Matrix Composites are manufactured by the following fabrication methods:
 Powder metallurgy(sintering);
 Stir casting;
 Infiltration.
The following properties are typical for Aluminum Matrix Composites:
 High strength even at elevated temperatures;
 High stiffness (modulus of elasticity);
 Low density;
 High thermal conductivity;
 Excellent abrasion resistance.
Aluminum Matrix Composites (AMC) are used for manufacturing automotive parts (pistons, pushrods,
brake components), brake rotors for high speed trains, bicycles, golf clubs, electronic substrates, cors
for high voltage electrical cables.

 Magnesium Matrix Composite

Magnesium Matrix Composites are reinforced mainly by silicon carbide (SiC) particles (particulate
composites)
The following properties are typical for Magnesium Matrix Composites:
 Low density;
 High stiffness (modulus of elasticity);
 High wear resistance;
 Good strength even at elevated temperatures;
 Better creep resistance.
Magnesium Matrix Composites are used for manufacturing components for racing cars, lightweight
automotive brake system, aircraft parts for: gearboxes, transmissions, compressors and engine.

 Titanium Matrix Composite

Titanium Matrix Composites are reinforced mainly by:
 Continuous monofilament silicon carbide fiber (long-fiber reinforced composites);
 Titanium boride (TiB2) and titanium carbide (TiC) particles (particulate composites).
Powder metallurgy (sintering)is used for fabrication of Titanium Matrix Composites.
The following properties are typical for Titanium Matrix Composites:
 High strength;
 High stiffness (modulus of elasticity);
 High creep resistance;
 High thermal stability;
 High wear resistance.
Titanium Matrix Composites are used for manufacturing structural components of the F-16 jet’s
landing gear, turbine engine components (fan blades, actuator pistons, synchronization rings,
connecting links, shafts, and discs), automotive engine components, drive train parts, general machine
components.
  Copper Matrix Composites
Copper Matrix Composites are reinforced by:
 Continuous fibers of carbon (**C**), silicon carbon (SiC), tungsten (W), stainless steel 304
(long-fiber reinforced composites);
 Silicon carbide particles (particulate composites).
Powder metallurgy (sintering) and infiltration technique are used for fabrication Copper Matrix
Composites.
The following properties are typical for Copper Matrix Composites:
 Low coefficient of thermal expansion;
 High stiffness (modulus of elasticity);
 Good electrical conductivity;
 High thermal conductivity;
 Good wear resistance.
Copper Matrix Composites are used for manufacturing hybrid modules, electronic relays, electrically
conducting springs and other electrical and electronic components.

An overview of Processing MMCs-liquid state and solid state processes:

Liquid state and solid state processes:

Liquid state fabrication of Metal Matrix Composites involves incorporation of dispersed phase into a
molten matrix metal, followed by its Solidification. In order to provide high level of mechanical
properties of the composite, good interfacial bonding (wetting) between the dispersed phase and the
liquid matrix should be obtained. Wetting improvement may be achieved by coating the dispersed
phase particles (fibers). Proper coating not only reduces interfacial energy, but also prevents chemical
interaction between the dispersed phase and the matrix.
The methods of liquid state fabrication of Metal Matrix Composites:

 Stir Casting

 Infiltration

 Gas Pressure Infiltration

 Squeeze Casting Infiltration

 Pressure Die Infiltration

 Stir Casting
Stir Casting is a liquid state method of composite materials fabrication, in which a dispersed phase
(ceramic particles, short fibers) is mixed with a molten matrix metal by means of mechanical stirring.
Stir Casting is the simplest and the most cost effective method of liquid state fabrication.
The liquid composite material is then cast by conventional casting methods and may also be processed
by conventional Metal forming technologies.
Stir Casting is characterized by the following features:
 Content of dispersed phase is limited (usually not more than 30 vol.%).
 Distribution of dispersed phase throughout the matrix is not perfectly homogeneous:
1. There are local clouds (clusters) of the dispersed particles (fibers);
2. There may be gravity segregation of the dispersed phase due to a difference in the densities of the
dispersed and matrix phase.
 The technology is relatively simple and low cost.
Distribution of dispersed phase may be improved if the matrix is in semi-solid condition. The method
using stirring metal composite materials in semi-solid state is called Rheocasting. High viscosity of the
semi-solid matrix material enables better mixing of the dispersed phase.

 Infiltration
Infiltration is a liquid state method of composite materials fabrication, in which a preformed dispersed
phase (ceramic particles, fibers, woven) is soaked in a molten matrix metal, which fills the space
between the dispersed phase inclusions. The motive force of an infiltration process may be either
capillary force of the dispersed phase (spontaneous infiltration) or an external pressure (gaseous,
mechanical, electromagnetic, centrifugal or ultrasonic) applied to the liquid matrix phase (forced
infiltration). Infiltration is one of the methods of preparation of tungsten-copper composites.
The principal steps of the technology are as follows:
 Tungsten Powder preparation with average particle size of about 1-5 µm.
 Optional step: Coating the powder with nickel. Total nickel content is about 0.04%.
 Mixing the tungsten powder with a polymer binder.
 Compacting the powder by a molding method (Metal injection molding, die pressing, isostatic
pressing). Compaction should provide the predetermined porosity level (apparent density) of
the tungsten structure.
 Solvent debinding.
 Sintering the green compact at 2200-2400F (1204-1315C) in Hydrogen atmosphere for 2 hrs.
 Placing the sintered part on a copper plate (powder) in the infiltration/sintering furnace.
 Infiltration of the sintered tungsten skeleton porous structure with copper at 2100-2300F
(1100-1260C) in either hydrogen atmosphere or vacuum for 1 hour.

 Gas Pressure Infiltration

Gas Pressure Infiltration is a forced infiltration method of liquid phase fabrication of Metal Matrix
Composites, using a pressurized gas for applying pressure on the molten metal and forcing it to
penetrate into a preformed dispersed phase.
Gas Pressure Infiltration method is used for manufacturing large composite parts. The method allows
using non-coated fibers due to short contact time of the fibers with the hot metal. In contrast to the
methods using mechanical force, Gas Pressure Infiltration results in low damage of the fibers.

 Squeeze Casting Infiltration

Squeeze Casting Infiltration is a forced infiltration method of liquid phase fabrication of Metal Matrix
Composites, using a movable mold part (ram) for applying pressure on the molten metal and forcing
it to penetrate into a performed dispersed phase, placed into the lower fixed mold part.
Squeeze Casting Infiltration method is similar to the Squeeze casting technique used for metal alloys
casting.

Squeeze Casting Infiltration process has the following steps:

 A preform of dispersed phase (particles, fibers) is placed into the lower fixed mold half.
 A molten metal in a predetermined amount is poured into the lower mold half.
 The upper movable mold half (ram) moves downwards and forces the liquid metal to infiltrate
the preform.
 The infiltrated material solidifies under the pressure.
 The part is removed from the mold by means of the ejector pin.

The method is used for manufacturing simple small parts (automotive engine pistons from
aluminum alloy reinforced by alumina short fibers).
  Pressure Die Infiltration
Pressure Die Infiltration is a forced infiltration method of liquid phase fabrication of Metal Matrix
Composites, using a Die casting technology, when a preformed dispersed phase (particles, fibers) is
placed into a die (mold) which is then filled with a molten metal entering the die through a sprue and
penetrating into the preform under the pressure of a movable piston (plunger).
Solid state processes:
Solid state fabrication of Metal Matrix Composites:

Solid state fabrication of Metal Matrix Composites is the process, in which MMCs are formed as a
result of bonding matrix metal and dispersed phase due to mutual diffusion occurring between them
in solid states at elevated temperature and under pressure. Low temperature of solid state fabrication
process (as compared to Liquid state fabrication of MMCs) depresses undesirable reactions on the
boundary between the matrix and disperse phases. MMCs may be deformed also after sintering
operation by rolling, Forging, pressing, Drawing or Extrusion. The deformation operation may be either
cold (below the recrystallization temperature) or hot (above the recrystallization temperature).
Deformation of sintered composite materials with dispersed phase in form of short fibers results in a
preferred orientation of the fibers and anisotropy of the material properties (enhanced strength
along the fibers orientation).

There are two principal groups of solid state fabrication of Metal Matrix Composites:

 Diffusion bonding
 Sintering

Diffusion Bonding:
Diffusion Bonding is a solid state fabrication method, in which a matrix in form of foils and a dispersed
phase in form of long fibers are stacked in a particular order and then pressed at elevated
temperature. The finished laminate composite material has a multilayer structure. Diffusion Bonding
is used for fabrication of simple shape parts (plates, tubes).
Variants of diffusion bonding are roll bonding and wire/fiber winding:
Roll Bonding is a process of combined Rolling (hot or cold) strips of two different metals (e.g. steel and
aluminum alloy) resulted in formation of a laminated composite material with a metallurgical bonding
between the two layers. Wire/fiber Winding is a process of combined winding continuous ceramic
fibers and metallic wires followed by pressing at elevated temperature.
The microstructural changes during diffusion bonding process, as well as a schematic illustration of
how the product looks like are shown in the following figures respectively.
Sintering:

Sintering fabrication of MMCs is a process, in which a powder of a matrix metal is mixed

with a powder of dispersed phase in form of particles or short fibers for subsequent
compacting and sintering in solid state (sometimes with some presence of liquid).

Sintering is the method involving consolidation of powder grains by heating the “green” compact part
to a high temperature below the melting point, when the material of the separate particles diffuse to
the neighboring powder particles.
In contrast to the liquid state fabrication of Metal Matrix Composites, sintering method allows
obtaining materials containing up to 50% of dispersed phase.
When sintering is combined with a deformation operation, the fabrication methods are called:
 Hot Pressing Fabrication of Metal Matrix Composites;
 Hot Isostatic Pressing Fabrication of Metal Matrix Composites;
 Hot Powder Extrusion Fabrication of Metal Matrix Composites;

The following figure shows the transformation of a green compact into a fully sintered state.
In-situ fabrication of Metal Matrix Composites:

In situ fabrication of Metal Matrix Composite is a process, in which dispersed (reinforcing) phase is
formed in the matrix as a result of precipitation from the melt during its cooling and Solidification.
Different types of Metal Matrix Composites may be prepared by in situ fabrication method:

1. Particulate in-situ MMC – Particulate composite reinforced by in-situ synthesized dispersed phase
in form of particles.
Examples: Aluminum matrix reinforced by titanium boride (TiB2) particles, magnesium matrix
reinforced by Mg2Si particles.

2. Short-fiber reinforced in-situ MMC – Short-fiber composite reinforced by in-situ synthesized

dispersed phase in form of short fibers or whiskers (single crystals grown in form of short fibers).
Examples: Titanium matrix reinforced by titanium boride (TiB2) whiskers,
Aluminum matrix reinforced by titanium aluminide (TiAl 3) whiskers.

3. Long-fiber reinforced in situ MMC – Long-fiber composite reinforced by in situ synthesized

dispersed phase in form of continuous fibers.
Example: Nickel-aluminum (NiAl) matrix reinforced by long continuous fibers of Mo (NiAl-9Mo alloy).
Dispersed phases of in situ fabricated Metal Matrix Composites may consist of intermetallic
compounds, carbides, borides, oxides, one of eutectic ingredients.
Advantages of in situ Metal Matrix Composites:
 In-situ synthesized particles and fibers are smaller than those in materials with separate
fabrication of dispersed phase (ex-situ MMCs). Fine particles provide better strengthening
effect;
 In-situ fabrication provides more homogeneous distribution of the dispersed phase particles;
 Bonding (adhesion) between the particles of in situ formed dispersed phase and the matrix is
better than in ex-situ MMCs;
 Equipment and technologies for in situ fabrication of MMCs are less expensive.

Disadvantages of in-situ MMCs:

 Choice of the dispersed phases is limited by thermodynamic ability of their precipitation in
particular matrix;
 The size of dispersed phase particles is determined by solidification conditions;

Unidirectional solidification of a eutectic alloy (alloy of eutectic composition) may result in formation
of eutectic structure, in which one of the components has a form of long continuous filaments.
Types of CMCs, Processing of CMCs:

Ceramic Matrix Composites

Ceramic Matrix Composite (CMC) is a material consisting of a ceramic matrix combined with
a ceramic (oxides, carbides) dispersed phase. Ceramic Matrix Composites are designed to
improve toughness of conventional ceramics, the main disadvantage of which is brittleness.
Ceramic Matrix Composites are reinforced by either continuous (long) fibers or
discontinuous (short) fibers.

Short-fiber (discontinuous) composites are produced by conventional ceramic processes from an

oxide (alumina) or non-oxide (silicon carbide) ceramic matrix reinforced by whiskers of silicon carbide
(SiC), titanium boride (TiB2), aluminum nitride (AlN), zirconium oxide (ZrO2) and other ceramic fibers.
Most of CMC are reinforced by silicon carbide fibers due to their high strength and stiffness (modulus
of elasticity).
Whiskers incorporated in a short-fiber Ceramic Matrix Composite improve its toughness resisting to
cracks propagation. However a character of failure of short-fiber reinforced materials is catastrophic.
Long-fiber (continuous) composites are reinforced either by long monofilament of long multifilament
fibers. The best strengthening effect is provided by dispersed phase in form of continuous
monofilament fibers, which are fabricated by chemical vapor deposition (CVD) of silicon carbide on a
substrate made of tungsten (W) or carbon (C) fibers. Monofilament fibers produce stronger interfacial
bonding with the matrix material improving its toughness. Failure of long-fiber Ceramic Matrix
Composites is not catastrophic.

Typical properties of long-fiber CMCs:

 High mechanical strength even at high temperatures;

 High thermal shock resistance;

 High stiffness; High toughness; High thermal stability;
 Low density; High corrosion resistance even at high temperatures.

CMCs may be produced by traditional ceramic fabrication methods including mixing the powdered
matrix material with the reinforcing phase followed by processing at elevated temperature: hot
pressing, sintering. Such fabrication routs are successfully employed for preparing composites
reinforced with a discontinuous phase (particulate or short fibers).
However the composites reinforced with continuous or long fibers are rarely fabricated by
conventional sintering methods due to mechanical damage of the fibers and their degradation caused
by chemical reactions between the fiber and matrix materials at high sintering temperature.
Additionally sintering techniques result in high porosity of the fiber reinforced composites.
Ceramic matrix composites reinforced with long fibers are commonly fabricated by infiltration
methods.
In this group of fabrication techniques the ceramic matrix is formed from a fluid (gaseous or liquid)
infiltrated into the fiber structure (either woven or non-woven).
Prior to the infiltration with a ceramic derived fluid the reinforcing fibers surface is coated with a
debonding interphase providing weak bonding at the interface between the fiber and matrix
materials. Weak bonding allows the fiber to slide in the matrix and prevents brittle fracture.

Matrix material for long-fiber (continuous fiber) composite may be silicon carbide ceramic, alumina
(alumina-silica) ceramic or carbon.
 Silicon carbide matrix composites are fabricated by chemical vapor infiltration or liquid phase
Infiltration methods of a matrix material into a preform prepared from silicon carbide fibers.
Silicon carbide matrix composites are used for manufacturing combustion liners of gas turbine
engines, hot gas re-circulating fans, heat exchangers, rocket propulsion components, filters for hot
liquids, gas-fired burner parts, furnace pipe hangers, immersion burner tubes.
 Alumina and alumina-silica (mullite) matrix composites are produced by sol-gel method, direct
metal oxidation or chemical bonding.
Alumina and alumina-silica (mullite) matrix composites are used for manufacturing heat
exchangers, filters for hot liquids, thermo-photovoltaic burners, burner stabilizers, combustion
liners of gas turbine engines.
 Carbon-Carbon Composites are fabricated by chemical vapor infiltration or Liquid phase
infiltration methods of a matrix material into a preform prepared from carbon fibers.
Carbon-Carbon Composites are used for manufacturing high performance braking systems, refractory
components, hot-pressed dies, heating elements, turbojet engine components.

Fabricating processes- solid and Liquid state processes

Solid state fabrication of CMCs:

To put a rigidized or densified matrix in place, the precursor of the matrix has to be positioned within
the mass of reinforcement. This can be done by a number of methods:
(i) Powder dispersion
(ii) Liquid precursors
(iii) Gaseous infiltration
Powder dispersion is a popular solid state process of fabricating CMCs.

Impregnating the reinforcement with a suspension of matrix precursor in powder form, either by
passing the reinforcement through a slurry or by pressure impregnation of a preform, or by
electrophoretic infiltration. The powder dispersion method is the most widely used where a simple
approach using substances of known composition or characteristics is required. Most types of matrix
can be positioned using this method. Normally it requires that the fibre or whisker architecture is
opened up so that powder particles can completely surround each reinforcing element, and that there
is sufficient powder entrained for the densified matrix to fill the space around the reinforcement to
an adequate degree, usually completely. Matrix precursors entrained in this way, even if sinter-active,
tend to be reluctant to sinter to full density because of the restraint posed by the nonshrinking
reinforcement structure, and hot-pressing, usually uniaxial, is required to close voids between
reinforcing elements. This process does not readily lend itself to complex shapes generally plate
shapes with planar reinforcement are easiest to produce because the reinforcement is not greatly
distorted and thus it is not particularly versatile for producing components with complex architecture

Liquid infiltration, directed oxidation, in-situ chemical reaction techniques:

Fabrication of Ceramic Matrix Composites by Liquid phase Infiltration:

The methods of fabrication of Ceramic Matrix Composites, utilizing infiltration of a liquid into long
continuous fibers, are as follows:
 Infiltration of molten ceramic;

 Slurry Infiltration Process (SIP);

 Reactive Melt Infiltration (RMI);

 Polymer Infiltration and Pyrolysis (PIP).

Infiltration of molten ceramic:

Infiltration of molten ceramic into a fiber preform is limited by low viscosity of molten ceramics and
by high temperature causing chemical interaction between the molten matrix and the dispersed phase
(fibers). This process (similar to Liquid state fabrication of MMCs) is sometimes used for fabrication
glass matrix composites.

Slurry Infiltration Process (SIP):

Slurry Infiltration Process (SIP) involves the following operations:

 Passing fibers (tow, tape) through a slurry containing particles of the ceramic matrix;

 Winding the fibers infiltrated by the slurry onto a drum and drying;
 Stack of the slurry impregnated fibers in a desired shape;
 Consolidation of the matrix by hot pressing in Graphite die at high temperature.

Reactive Melt Infiltration Process (RMI)

Reactive Melt Infiltration Process (RMI) is used primarily for fabrication of silicon carbide (SiC) matrix
composites (Fabrication of Ceramic Matrix Composites by Liquid Silicon Infiltration (LSI)). The process
involves infiltration of carbon (C) containing preform with molten silicon (Si). Infiltration is usually
capillary forced. Carbon of the impregnated preform reacts with liquid silicon, forming silicon carbide
(SiC). Resulting matrix consists of silicon carbide and some residual silicon.
When liquid aluminum (Al) is used for infiltration of a preform in oxidizing atmosphere, alumina-
aluminum (Al2O3 – Al) matrix is formed (Fabrication of Ceramic Matrix Composites by Direct Oxidation
Process). Reactive Melt Infiltration method is fast and relatively cost effective. Materials fabricated by
RMI method possess low porosity and high thermal conductivity and electrical conductivity.
CMCs Processing: Sol-gel and polymer pyrolysis

Fabrication of Ceramic Matrix Composites by Sol-gel process:

 Sol-gel Infiltration - description

 Sol-gel Infiltration process
 Advantages and disadvantages of Sol-gel Infiltration
Sol-gel Infiltration – description:
Sol-Gel process of a fabrication of CMCs involves preparation of the matrix from a liquid colloidal
suspension of fine ceramic particles (sol), which soaks a preform and then transforms to solid
(gel).Colloidal suspension is formed as a result of chemical reaction when very small particles with
radii up to 100 nm (nanoparticles) precipitate within a liquid (water or organic solvent)
Liquid sols have a low viscosity therefore they easily infiltrate into the preform. At elevated
temperatures sols containing organometallic compounds (e.g. alkoxides) undergo cross-linking
(polymerization) by either the polycondensation or hydrolysis mechanism. Polymerization converts
sol into gel – a polymer structure containing liquid. Gels may be transformed into Ceramics at relatively
low temperature, which reduces the probability of the reinforcing fiber damage. Alumina matrix
ceramic composites may be prepared from alumina gel, which forms in hydrolysis (decomposition as
a result of reaction with water) of aluminum alkooxides. Since the amount of ceramic in gels is
relatively low they undergo significant shrinkage after drying. The densification of the ceramic matrix
is commonly increased by repeating the infiltration-drying cycle several times until the desired density
is achieved. Further increase of the volumetric yield of ceramic of a Sol-Gel may be achieved by an
addition of ceramic particles.

Sol-gel Infiltration process:

 Fabrication of the prepreg. The reinforcing fibrous material is immersed into the sol. The sol

wicks into the porous structure of the reinforcing phase. Vacuum/pressure may be applied to
assist the infiltration process.
 Lay-up. The prepreg is shaped by a tooling (mold).
 Gellation and drying. The sol is heated to 150°C (302°F). It is converted into gel, which is then
dried at a temperature up to 400°C (752°F). Water, alcohol and organic volatile components
are removed from the material.
 Repeated re-infiltration and gelation. The sol infiltration-gelation cycle is repeated several
times until the desired densification is achieved.
 Firing. The ceramic matrix is consolidated (sintered) at the firing temperature.
Advantages and disadvantages of Sol-gel Infiltration
Advantages of Sol-Gel Infiltration:
 less reinforcing fiber damage due to low processing temperature;
 Controllable matrix composition; Low equipment cost;
 Low machining cost due to near-net-shape fabrication; Large and complex parts may be
fabricated.
Disadvantages of Sol-Gel Infiltration:
 Possible matrix cracking because of large shrinkage;
 Multiple infiltration-gelatin cycles are required in order to increase the ceramic yield;
 Low mechanical properties; High cost of sols.

Polymer Infiltration and Pyrolysis (PIP):

Polymer Infiltration and Pyrolysis (PIP) is the method of fabrication of CMCs comprising an infiltration
of a low viscosity polymer into the reinforcing ceramic structure (e.g. fabric) followed by pyrolysis:
heating the polymer precursor in the absence of oxygen when it decomposes and converts into a
ceramic.

The Ceramics produced from polymers by pyrolysis are called polymer derived ceramics.
 Preceramic polymers
 Polymer Infiltration and Pyrolysis (PIP) process
 Advantages and disadvantages of Polymer Infiltration and Pyrolysis (PIP)
Preceramic polymers:
Preceramic polymers (polymer precursors) are the Polymers, which can be converted into Ceramics
by pyrolysis.
Molecules of preceramic polymers are commonly contain carbon (C) and/or silicon (Si) but may also
contain nitrogen (N), oxygen (O), boron (B), aluminum (Al), titanium (Ti).
Polymer Infiltration and Pyrolysis (PIP) technique is used mainly for fabrication Composites with
silicon carbide (SiC) matrices from polycarbosilanes (silicon derived polymer precursors):
polymethylsilane (PMS) and allhydridopolycarbosilane. The yield of SiC of the precursors is about
65%.
Polysilazane may be converted into SiCN or Si3N4 with ceramic yield up to 90%.
Carbon matrices composites are fabricated by pyrolysis of either carbon thermosetting resins
(phenolics, ruran resin, oxidized polystyrene, polyvinyl alcohol) or thermoplastic resins (pitches or
coal tar). The carbon yield of these resins is 50-60%.

Polymer Infiltration and Pyrolysis (PIP) process:

 Fabrication of pre-impregnated material (prepreg). The reinforcing fibers are impregnated

with a resin and then dried or cured to B-stage (partial curing). In such condition the viscosity
of the polymer is increased and the prepreg may be shaped (laid-up).
 Lay-up. The prepreg is shaped by a tooling (mold).
 Molding. The laid-up prepreg is molded. Various molding methods may be used. In the bag
molding a rigid lower mold is combined with a flexible upper mold (bag), which is pressed
against the prepreg by either atmospheric pressure (vacuum bag mold) or increased air
pressure (gas pressure bag mold). The pressurized preform is cured in an autoclave. A
combination of a pressure with an increased temperature may also be achieved in
compression molding.
 Infiltration of a preceramic polymer. The pores of the reinforcing structure are filled with a
low viscosity solution of a preceramic polymer when the preform is immersed into it. The
infiltration process is driven by the capillary forces therefore it is commonly conducted at
normal pressure, however it may also be vacuum- or pressure-assisted.
 Pyrolysis. Pyrolytic decomposition of the preceramic polymer is performed in the atmosphere
of Argon at a temperature in the range 1472-2372°F (800-1300°C). Nitride matrices (e.g.
silicon nitride) are fabricated in the atmosphere of Nitrogen (N2) or Ammonia) (NH3). Volatile
products such as CO, Hydrogen (H2), CO2, CH2, H2O are released as a result of pyrolysis forming
a porous structure of the resulting ceramic matrix. The value of the ceramic yield is
determined by the weight loss (amount of the released volatiles).
 Multiple re-infiltration and pyrolysis. The infiltration-pyrolysis cycle is repeated 4-10 times in
order to decrease the residual porosity of the ceramic matrix.

Advantages and disadvantages of Polymer Infiltration and Pyrolysis (PIP)

Advantages of Polymer Infiltration and Pyrolysis (PIP):
 Fibers damage is prevented due to the processing at a relatively low temperature;

 Good control of the matrix composition and the microstructure;

 Reinforcing phase of different types (particulate, fibrous) may be used;
  Net shape parts may be fabricated;
 Matrices of various compositions (silicon carbide, silicon nitride, silicon carbonitride) may be
obtained;
 No residual silicon is present in the matrix.
The disadvantages of the Polymer Infiltration and Pyrolysis (PIP):
 The fabrication time is relatively long due to the multiple infiltration-pyrolysis cycle;

 There is a residual porosity decreasing the mechanical properties of the composite;

 Relatively high production cost (higher than in Liquid Silicon Infiltration method).