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    Manufacturing Methods ofComposites

    Dr. M. BalasubramanianDept. of Metallurgical & Materials Engg.

    Indian Institute of Technology

    Chennai - 600 036

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    Constituents of Composites

    Discontinuous phase - Reinforcement

    Continuous phase - Matrix

    SEM micrograph of a fractured composite

    15 m

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    Constituents

    Reinforcements

    Principal load bearing member

    Matrix provides a medium for binding and holding the

    reinforcements together into a solid

    protects the reinforcement from environmental

    degradation serves to transfer load from one insert to the other

    Provides finish, colour, texture, durability and

    other functional properties

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    Fibres: Important Characteristics

    A small diameter

    Allows a higher fractionof the theoreticalstrength to be achieved

    A high aspect ratio

    Allows effective loadtransfer to fibres

    A very high degree offlexibility

    Permits the use of avariety of techniques formaking composites

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    Synthetic Fibres

    Glass

    Carbon

    AramidPolyethylene

    Alumina

    Silicon carbide

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    Types of Glass Fibres

    %by of

    constituents

    E Glass A Glass C Glass S Glass Z Glass M Glass

    SiO2 52.4-53.2 72.5 65.0 64.0-65.0 60.0 53.7

    Al2O3 14.4-14.8 0.7-1.5 4.0 25.0-26.0 - -

    B2O3 8.0-10.0 - 6.0 - - -

    MgO 4.5 2.5 3.0 10.0 - 9.0

    CaO 17.5 10.0 14.0 - - 12.9

    Na2 * K2O 0.5 13.5-14.0 8.0 - 20.0 -

    Fe2O3 0.4 - - - - -

    F2 0.0 - - - - -

    SO3 - 0.7 - - - -

    BeO - - - - - 8.0

    TiO2 - - - - 5.0 7.9

    CeO2 - - - - - 3.0

    Li2O - - - - - 3.0

    ZrO2 - - - - 15.0 2.0

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    Commercial forms of Glass F ibres

    Rovings

    Chopped Strand Mat

    Yarn

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    Chopped Strands

    Woven Rovings

    Commercial forms of Glass F ibres (contd.,)

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    Carbon fibre

    Made from organic precursor fibre

    Commonly used precursor fibre is

    polyacrylonitrile (PAN)Other precursor fibres

    Rayon

    Pitches Polyvinyl alcohol

    Polyimides

    Phenolics

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    Processing of Carbon Fibre fromPAN

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    Two Approaches to Make High

    Modulus Polymer FibresProcess a polymer with highly

    oriented and extended chain

    arrangement Polyethylene fibre

    Synthesis followed by extrusion of anew class of polymers, called liquidcrystal polymers

    These have a rigid rod molecularstructure

    Aramid fibre

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    Comparison of fibres

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    Properties of ReinforcementFibresProperties PAN-Based

    CarbonKevlar

    49E

    GlassSiC Al2O3 Boron

    (W)

    HM HS CVD Nicalon

    Diameter (m) 7-10 7.6-8.6

    12 8-14 100-200

    10-20 20 100-200

    Density (g cm-3) 1.95 1.75 1.45 2.55 3.3 2.6 3.95 2.6

    Youngs Modulus (GPa)Parallel to fibre axisPerpendicular to fibreaxis

    39012

    25020

    125-

    7070

    430-

    180-

    379-

    385-

    Tensile strength (GPa) 2.2 2.7 2.8-

    3.5

    1.5-

    2.5

    3.5 2 1.4 3.8

    Strain to fracture (%) 0.5 1.0 2.2-2.8

    1.8-3.2

    - - - -

    Coefficient of thermalexpansion (10-6K-1)Parallel to fibre axis

    Perpendicular to fibreaxis

    -0.5 --1

    7-12

    0.1--0.5

    7-12

    -2- -5

    59

    4.7

    4.7

    5.7

    -

    -

    -

    7.5

    -

    8.3

    -

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    Natural Fibres

    Natural fibres are also used for makingFRP products.

    Some of the common natural fibres Jute

    Banana

    Sisal Pineapple

    Coir

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    Natural Fibres

    The primary driving force for these naturalfibre are low cost and recyclable nature.

    Other reasons for their increasing use Weight reduction

    these fibres are half the weight of fibre-glass

    Green movement

    desire for natural products

    Major draw back

    they absorb moisture because of inherent

    porosity

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    Comparison of Natural FibresProperty Jute Banana Sisal Pineapple Coir

    Width or Diameter(micron )

    20-60 80-250 50-200 20-80 100-450

    Density (gms./cc) 1.3 1.35 1.45 1.44 1.15

    Elastic Modulus(GN/m2)

    - 8-20 9-16 34-82 4-6

    Elongation (%) 1-1.2 1.0-3.5 3-7 0.8-1.6 15-40

    Cellulose/LigninContent (%)

    61 /12 65 /5 67 /12 81 /12 43 /45

    REINFORCEMENTS MATRICES

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    REINFORCEMENTS MATRICES

    GLASS FIBRE(1940)

    THERMOSETPLASTICS

    BASALT FIBRE

    (1965)

    THERMO-

    PLASTICS

    NATURALFIBRES

    RUBBER ANDELASTOMERS

    CARBON FIBRE(1960)

    METALS &ALLOYS

    ARAMID FIBRE(1972)

    CEMENTS

    BORON FIBRE(1959)

    CARBON

    ALUMINA FIBRE(1962)

    STRUCTURALCERAMICS

    SiC FIBRES &WHISKERS

    GLASS

    Si3N4FIBRES

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    Polymer Matrix

    A polymer is defined as a long-chainmolecule containing one or morerepeating units of atoms, joinedtogether by strong covalent bonds

    A polymeric material is a collection of alarge number of polymer molecules ofsimilar chemical structure

    These molecules are frozen in space,

    either in random fashion or in amixture of random and orderlyfashions

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    Thermoset Polymers (Resins)

    Epoxies principally used in aerospace

    applications

    Polyester, vinyl esters commonly used in automotive, marine,

    chemical and electrical applications

    Phenolics

    used in bulk moulding compounds

    Polyimides, polybenzimidazoles (PBI),polyphenylquinoxaline (PPQ)

    high temperature aerospace applications

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    ThermoplasticsNylons, thermoplastic polyesters,

    polycarbonate, polyacetals

    used with discontinuous fibres in injection

    moulded articles

    Polyamide-imide (PAI), polyether-etherketone (PEEK), polysulphone (PSUL),

    polyphenylene sulphide (PPS), polyetherimide (PEI)

    suitable for moderately high temperatureapplications with continuous fibres

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    Processing of PolymerComposites

    Hand lay-up

    Resin transfer moulding (RTM)

    Filament winding

    Pultrusion

    Autoclave processCompression moulding

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    Hand Lay-up

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    Hand Lay-up

    Cover bench with release sheet Spread Resin base

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    Apply surfacing veil Add more resin

    Apply the layer of chopped strand mat Add resin and apply second mat

    Hand Lay-up

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    Apply woven roving Roll roving into resin

    Add final chopped strand mat Finish with wax topcoat

    Hand Lay-up

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    Hand Lay-up

    Advantages

    Widely used

    Low tooling cost Custom shape

    Larger and complex

    items can be produced

    Problems

    Labour intensive

    Low-volume process

    Longer cure time requireddue to lack of hightemperatures andpressures to accelerate

    the curing Good surface finish on

    only one side

    Quality is purelydependent on fabricator

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    Spray-up

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    Resin transfer molding (RTM)

    Closed mold, low pressuretechnique

    Place the fibre preform in a mold

    Inject the liquid resin into the moldby a pump

    Low polymer viscosity, < 1 Pa s(thermosets such epoxy, polyester)

    Thermoplastics have high viscosity difficult to process by RTM.

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    Resin Transfer Moulding

    Vacuum infusion: Instead of applying pressure, vacuum is applied to draw resin

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    Resin Transfer Moulding

    Advantages:

    Low skill labour required

    Low tooling cost

    Low volatile emission

    Required design

    tailorability

    Problems:

    Control of resin flow

    Kinking of fibres

    Criticality in mould

    design

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    Pultrusion

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    Pultrusion

    Can producecontinuously at a rate of10 to 200 cm/min.

    Pultruded profiles as

    wide as 1.25 m withmore than 60 vol. %fibre can be made.

    Example:

    A helicopter windshieldpost (carbon fiber/vinylester), 1.5 m long.

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    Pultrusion

    Advantages:

    Minimal kinking of

    fibres/fabricsRapid processing

    Low material scrap

    rate

    Good quality control

    Problems:

    Improper fibre wet-

    outFibre breakage

    Inadequate cure

    Die jamming

    Complex die design

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    Filament winding

    Resin-impregnated continuous fiberor tape is wound on a mandrel in aprecise geometric pattern.

    Rotate the mandrel while a deliveryhead precisely positions fibers froma creel on the mandrel surface.

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    Filament Winding

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    Filament wound pressurebottles for gas storage

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    Prepregs

    Pre-impregnated fibres

    A thin sheet or lamina of unidirectional fibre/polymercomposite protected on both sides with easilyremovable separators

    An intermediate stage in the fabrication

    Partially cured state with a moderately self-adhesivetack

    Easily obtained with epoxies

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    Autoclave Process

    Very high quality productHeat & pressure are applied

    Removes the entrapped air and helps curing

    Generally prepregs are usedChopped fibres with resin can also be used

    Hybrid composites can be produced

    High fibre volume fractions can be obtained

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    a) Autoclave process to make a laminated compositeb) Prepregs of different orientations stacked to form a laminated composite

    a)

    b)

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    Sheet Moulding Compounds

    Consists of apolyester resin plusadditives

    Additives are

    generally fine calciumcarbonate and shortglass fibres

    Used in auto body

    parts (bumper beams,radiator supportpanels, etc.)

    Schematic of compressionmoulding

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    Thermoplastic Matrix Composites

    Advantages

    Refrigeration is not necessary with a thermoplasticmatrix

    Parts can be made & joined by heating

    Parts can be remoulded and any scrap can berecycled

    Better toughness & impact resistanceDisadvantages

    Processing temperatures are generally higher

    Stiff and boardy

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    Injection Moulding

    Generally discontinuous fibres are

    used

    Mixed with molten matrix materialand injected into the die

    Recent development is reinforced

    reaction injection moulding

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    Film Stacking

    Fibres with very low resin content are usedStacked with pure polymer layer

    Consolidated by heat & pressure

    Pressure is 6-12 MPa & temperature is 275-350C for polysulphones and polyetheretherketone

    Moulding cycle with thermoplastic is less

    Alternative is to use continuous tows ofcommingled carbon fibre/PEEK

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    Commingled Fibres

    Matrix fibre and reinforcement fibre

    commingled to produce yarn

    Yarn can be woven, knit or filamentwound

    Subjected to heat and pressure

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    Thermoplastic Tape Laying

    A controllable tape

    head has the tape

    dispensing reels and

    shoes

    Hot shoes heat the tape

    to molten state

    Cold shoes cool the

    tape instantly to solidstate

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    Thermoforming

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    Diaphragm Forming

    Involves the sandwiching of freely

    floating thermoplastic prepreg layers

    between two diaphragms

    Components with double curvatures

    can be formed

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    Constituents of MMC

    Metal matrix composites consistof a metal or an alloy as the

    continuous matrix and areinforcement that can beparticle, short fibre or whiskeror continuous fibre.

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    Typical reinforcements used inmetal matrix composites

    Type Aspect

    Ratio

    Diameter

    (m)

    Examples

    Particle ~ 1-4 1-25 SiC, Al2O3, BN,

    B4C, Fly ash

    Short fibre or

    whisker

    ~ 10-1000 0.1-25 SiC, Al2O3,

    Al2O3+SiO2, C

    Continuous

    fibre

    > 1000 3-150 SiC, Al2O3, C, B,

    W

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    Important Metallic Matrices

    Aluminium Alloys

    Titanium Alloys

    Magnesium Alloys

    Copper

    Intermetallic Compounds

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    Processing of MMCs

    Many processes for fabricating metalmatrix composites are available.

    These processes involve processing

    in the liquid and solid state.Some processes involve a variety of

    deposition techniques

    A recent processing method is in-situprocess of incorporating areinforcement phase.

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    Duralcan ProcessA stir casting process

    8-12 m particles are used

    Too small particles, e.g. 2-3 m,

    Will result in a very large interface region and

    thus a very viscous meltFoundry-grade MMCs

    High silicon aluminium alloys (e.g., A356)

    Alumina particles

    Wrought MMCs

    Al-Mg-type alloys (e.g., 6061)

    Silicon carbide particles

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    Stir Casting

    Stirring of composite melt with ceramic particles to minimize

    settling of the particles during processing.

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    Squeeze Infiltration

    The molten metal is infiltrated into the

    reinforcement preform under pressure

    This method obviates the requirement ofgood wettability

    Have minimal reaction between the

    reinforcement and molten metal

    Short dwell time at high temperature

    Free from common casting defects, such

    as porosity and shrinkage cavities

    Preform Manufacturing

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    Preform Manufacturing

    Press Forming of Preform

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    Squeeze infiltration technique of composite fabrication

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    Diesel engine piston

    Saffil alumina fibre/Al composite)

    Made by squeeze casting

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    Powder Metallurgy

    TechniqueMixing

    Compaction

    Sintering/hot pressing

    Powder metallurgy and extrusion

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    Powder metallurgy and extrusionprocessing of Al/SiCpcomposites

    Vacuum degassing

    Hot pressing

    Pressure

    Graphite die

    Particle reinforcedmetal matrix composite

    P/M Al SiCp

    Blending of gasatomized powders

    Cold Isostatic Compaction

    Extrusion

    Diff i B di P

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    Diffusion Bonding Process

    A solid state processing method

    Schematic of diffusion bonding process

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    The microstructure of SiC fibre/titanium matrix composite

    made by diffusion bonding

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    In-situ Process

    Composite material is produced in onestep from an appropriate starting alloy

    Reinforcement phase is formed in-situ

    Avoiding the difficulties inherent incombining the separate components

    The solidification rate in practice,however, is limited to a range of

    1-5 cm/h for fibre-reinforcedcomposites

    Many particulate reinforced compositesare now-a-days made with this process

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    Transverse section of in-situ

    composites obtained at different

    solidification rates

    Solidification rates indicated in left-hand top corners (cm/h)

    T f C i C it

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    Types of Ceramic Composites

    Oxide and Non-oxide Ceramic composites Silica, alumina, SiC, Si3N4and other ceramics

    are reinforced with carbon, silicon nitride orsilicon carbide fibres/whiskers

    Used for temperatures up to 2000C

    Carbon fibre reinforced carbon

    Used as a high temperature resistant material

    for heat shields, rocket nozzles, etc. and asbody implants

    Can be used up to 1500C under inertconditions

    T f C i C it

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    Types of Ceramic Composites

    Glass and Glass ceramic composites Glass and glass ceramics can be

    reinforced with carbon or metallic fibres

    for improving their impact resistanceCement composites

    Portland cement can be reinforced with

    glass, plastics, asbestos or steel fibresfor building and construction industry

    P i M h d f CMC

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    Processing Methods of CMCs

    Cold pressing and Sintering

    Hot pressing & Hot isostatic pressing

    Reaction bonding process

    Direct oxidation process Chemical vapour impregnation process

    Sol-gel process

    Polymer infiltration & pyrolysis

    Cold Pressing & Sintering

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    Cold Pressing & Sintering

    Li it ti f C ld P i &

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    Limitations of Cold Pressing &Sintering

    The reinforcement phase can form aconnective network throughout thecomposite.

    This network will resist densification and leadsto a porous microstructure.

    Large residual stresses can develop incomposites during sintering due to thermalexpansion mismatch between the

    constituent phases. These stresses can sometimes be large

    enough to cause cracking in the composite.

    Hot pressing

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    Hot pressing

    Simultaneous application ofpressure and high temperature

    Pore-free and fine grained compact

    Limitations

    Difficult to produce complex shapes

    Very high pressure can easily damagefibres

    Low production rate

    Hot pressing

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    Hot pressing

    Similar to diecompaction

    But, the whole die set-upis heated

    Die is usually made fromgraphite

    Allows external inductionheating

    Other common diematerials

    Refractory metals & theiralloys

    If the compact exhibitsincompatible thermalexpansion

    Ejected at high

    temperature

    A cross-sectional view of the uniaxial hotpressing operation

    Hot Isostatic Pressing

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    Hot Isostatic Pressing

    To produce near full density parts and

    complex shapes

    Performed in a pressurized fluid

    High pressure argon or nitrogen is used to

    transfer heat & pressure

    Flexible dies are used

    Glass, steel, stainless steel & tantalum

    Temperatures up to 2200C & pressuresup to 200 MPa are possible

    Useful for large components, where full

    density & isotropic properties are required

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    Hot isostatic pressing

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    Hot isostatic pressing

    One variant is to use previouslysintered compacts

    Component already has the desiredshape

    Densities over 92% TD

    Closed pores allow for HIP

    Widely used to consolidatecemented carbides, ceramiccomposites, and wear resistantmaterials

    Reaction bonding process

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    act on on ng proc ss

    Process steps

    A composite is made with silicon powder Heated to a high temperature in the presence

    of reactive gases

    Matrix shrinkage during densification can

    be avoided Large volume fractions of whiskers or

    fibres can be used

    Multidirectional, continuous fibre preforms

    can be used Low temperature processing

    Great disadvantage of this process

    high porosity

    Directed Oxidation

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    Directed Oxidation

    Schematic diagram of directed metal oxidation process of Lanxide Corp.

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    Chemical Vapour Impregnation

    Advantages

    Good mechanical properties at hightemperatures

    Large, complex shapes can beproduced to a near-net shape

    Considerable flexibility in the fibresand matrices

    Disadvantages

    Process is slow and expensive

    I th l h i l

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    Isothermal chemical vapour

    infiltration process

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    Schematic diagram of a chemical vapour infiltration process with pressureand temperature gradients (Chawla, Composite Materials)

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    Sol-gel Processing

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    Sol-gel Processing

    Advantages

    lower processing temperatures

    greater compositional homogeneity

    potential for producing unique multiphasematrix materials

    allows processing via liquids of low viscosity

    Disadvantages

    high shrinkage

    results in a large density of cracks in thematrix

    generally, repeated impregnations arerequired to produce a substantially densematrix

    P l I filt ti &

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    Polymer Infiltration &Pyrolysis (PIP)

    Formation of ceramic matrixmaterials by high temperature

    pyrolysis of polymeric materialscontaining the constituentelements.

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    References

    1. Chawla, K.K. (2012) CompositeMaterials: Science and Engineering,3rdEdition, Springer Verlag.

    2. Mallick, P.K. (2008) Fiber-reinforcedComposites, 3rdEdition, CRC Press,Boca Raton.

    3. Balasubramanian, M. (2013)Composite Materials and Processing,CRC Press, Boca Raton.

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    Thank You