Manufacturing Methods of

Composites
Dr. M. Balasubramanian
Dept. of Metallurgical & Materials Engg.
Indian Institute of Technology
Chennai - 600 036

Constituents of Composites
Discontinuous phase - Reinforcement
Continuous phase
- Matrix

15 m

SEM micrograph of a fractured composite

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

Fibres: Important Characteristics

A small diameter
Allows a higher fraction
of the theoretical
strength to be achieved

A high aspect ratio

Allows effective load
transfer to fibres

A very high degree of

flexibility
Permits the use of a
variety of techniques for
making composites

Synthetic Fibres

Glass
Carbon
Aramid
Polyethylene
Alumina
Silicon carbide

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

Commercial forms of Glass Fibres

Yarn
Rovings

Chopped Strand Mat

Commercial forms of Glass Fibres (contd.,)

Chopped Strands

Woven Rovings

Carbon fibre
Made from organic precursor fibre
Commonly used precursor fibre is
polyacrylonitrile (PAN)
Other precursor fibres
Rayon
Pitches
Polyvinyl alcohol

Polyimides
Phenolics

Processing of Carbon Fibre from

PAN

Two Approaches to Make High

Modulus Polymer Fibres
Process a polymer with highly
oriented and extended chain
arrangement
Polyethylene fibre

Synthesis followed by extrusion of a

new class of polymers, called liquid
crystal polymers
These have a rigid rod molecular
structure
Aramid fibre

Comparison of fibres

Properties of Reinforcement
Fibres
Properties

PAN-Based
Carbon

Kevlar
49

HM

HS

Diameter (m)

7-10

7.68.6

12

Density (g cm-3)

1.95

1.75

Youngs Modulus (GPa)

Parallel to fibre axis
Perpendicular to fibre
axis

390
12

Tensile strength (GPa)

Strain to fracture (%)
Coefficient of thermal
expansion (10-6 K-1)
Parallel to fibre axis
Perpendicular to fibre
axis

E
Glass

SiC

Al2O3

Boron
(W)

CVD

Nicalon

8-14

100200

10-20

20

100200

1.45

2.55

3.3

2.6

3.95

2.6

250
20

125
-

70
70

430
-

180
-

379
-

385
-

2.2

2.7

2.83.5

1.52.5

3.5

1.4

3.8

0.5

1.0

2.22.8

1.83.2

-0.5 -1
7-12

0.1-0.5
7-12

-2- -5

4.7

5.7

7.5

8.3

59

4.7

Natural Fibres
Natural fibres are also used for making
FRP products.

Some of the common natural fibres

Jute
Banana
Sisal
Pineapple

Coir

Natural Fibres
The primary driving force for these natural
fibre 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

Comparison of Natural Fibres

Property

Jute

Banana

Sisal

Pineapple

Coir

Width or Diameter 20-60

(micron )

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/Lignin
Content (%)

61 /12

65 /5

67 /12

81 /12

43 /45

REINFORCEMENTS

MATRICES

GLASS FIBRE
(1940)

THERMOSET
PLASTICS

BASALT FIBRE
(1965)

THERMOPLASTICS

NATURAL
FIBRES

RUBBER AND
ELASTOMERS

CARBON FIBRE
(1960)

METALS &
ALLOYS

ARAMID FIBRE
(1972)

CEMENTS

BORON FIBRE
(1959)

CARBON

ALUMINA FIBRE
(1962)

STRUCTURAL
CERAMICS

SiC FIBRES &

WHISKERS

GLASS

Si3N4 FIBRES

Polymer Matrix
A polymer is defined as a long-chain
molecule containing one or more
repeating units of atoms, joined
together by strong covalent bonds
A polymeric material is a collection of a
large number of polymer molecules of
similar chemical structure
These molecules are frozen in space,
either in random fashion or in a
mixture of random and orderly
fashions

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

Thermoplastics
Nylons, thermoplastic polyesters,
polycarbonate, polyacetals
used with discontinuous fibres in injection
moulded articles

Polyamide-imide (PAI), polyether-ether

ketone (PEEK), polysulphone (PSUL),
polyphenylene sulphide (PPS), polyether
imide (PEI)
suitable for moderately high temperature
applications with continuous fibres

Processing of Polymer
Composites

Hand lay-up
Resin transfer moulding (RTM)
Filament winding
Pultrusion
Autoclave process
Compression moulding

Hand Lay-up

Hand Lay-up

Cover bench with release sheet

Spread Resin base

Hand Lay-up

Apply surfacing veil

Apply the layer of chopped strand mat

Add more resin

Add resin and apply second mat

Hand Lay-up

Apply woven roving

Add final chopped strand mat

Roll roving into resin

Finish with wax topcoat

Hand Lay-up
Advantages

Problems

Widely used

Labour intensive

Low tooling cost

Low-volume process

Custom shape

Longer cure time required

due to lack of high
temperatures and
pressures to accelerate
the curing

Larger and complex

items can be produced

Good surface finish on

only one side
Quality is purely
dependent on fabricator

Spray-up

Resin transfer molding (RTM)

Closed mold, low pressure
technique

Place the fibre preform in a mold

Inject the liquid resin into the mold
by a pump
Low polymer viscosity, < 1 Pa s
(thermosets such epoxy, polyester)

Thermoplastics have high viscosity

difficult to process by RTM.

Resin Transfer Moulding

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

Resin Transfer Moulding

Advantages:

Problems:

Low skill labour required

Control of resin flow

Low tooling cost

Kinking of fibres

Low volatile emission

Criticality in mould
design

Required design
tailorability

Pultrusion

Pultrusion
Can produce
continuously at a rate of
10 to 200 cm/min.
Pultruded profiles as
wide as 1.25 m with
more than 60 vol. %
fibre can be made.
Example:
A helicopter windshield
post (carbon fiber/vinyl
ester), 1.5 m long.

Pultrusion
Advantages:

Problems:

Minimal kinking of
fibres/fabrics

Improper fibre wetout

Rapid processing

Fibre breakage

Low material scrap

rate

Inadequate cure

Good quality control

Complex die design

Die jamming

Filament winding
Resin-impregnated continuous fiber
or tape is wound on a mandrel in a
precise geometric pattern.
Rotate the mandrel while a delivery
head precisely positions fibers from
a creel on the mandrel surface.

Filament Winding

Filament wound pressure

bottles for gas storage

Prepregs
Pre-impregnated fibres
A thin sheet or lamina of unidirectional fibre/polymer
composite protected on both sides with easily
removable separators
An intermediate stage in the fabrication
Partially cured state with a moderately self-adhesive
tack
Easily obtained with epoxies

Autoclave Process
Very high quality product
Heat & pressure are applied
Removes the entrapped air and helps curing

Generally prepregs are used

Chopped fibres with resin can also be used

Hybrid composites can be produced

High fibre volume fractions can be obtained

a)

b)

a) Autoclave process to make a laminated composite

b) Prepregs of different orientations stacked to form a laminated composite

Sheet Moulding Compounds

Consists of a
polyester resin plus
additives
Additives are
generally fine calcium
carbonate and short
glass fibres
Used in auto body
parts (bumper beams,
radiator support
panels, etc.)

Schematic of compression
moulding

Thermoplastic Matrix Composites

Advantages
Refrigeration is not necessary with a thermoplastic
matrix
Parts can be made & joined by heating
Parts can be remoulded and any scrap can be
recycled
Better toughness & impact resistance

Disadvantages
Processing temperatures are generally higher
Stiff and boardy

Injection Moulding
Generally discontinuous fibres are
used

Mixed with molten matrix material

and injected into the die
Recent development is reinforced
reaction injection moulding

Film Stacking
Fibres with very low resin content are used
Stacked with pure polymer layer
Consolidated by heat & pressure

Pressure is 6-12 MPa & temperature is 275350C for polysulphones and polyetherether
ketone
Moulding cycle with thermoplastic is less
Alternative is to use continuous tows of
commingled carbon fibre/PEEK

Commingled Fibres
Matrix fibre and reinforcement fibre
commingled to produce yarn

Yarn can be woven, knit or filament

wound
Subjected to heat and pressure

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 solid
state

Thermoforming

Diaphragm Forming
Involves the sandwiching of freely
floating thermoplastic prepreg layers
between two diaphragms
Components with double curvatures
can be formed

Constituents of MMC
Metal matrix composites consist
of a metal or an alloy as the
continuous matrix and a
reinforcement that can be
particle, short fibre or whisker
or continuous fibre.

Typical reinforcements used in

metal matrix composites
Type

Particle

Short fibre or
whisker

Continuous
fibre

Aspect
Ratio

Diameter
(m)

Examples

~ 1-4

1-25

SiC, Al2O3, BN,

B4C, Fly ash

~ 10-1000

0.1-25

SiC, Al2O3,
Al2O3+SiO2, C

> 1000

3-150

SiC, Al2O3, C, B,
W

Important Metallic Matrices

Aluminium Alloys
Titanium Alloys
Magnesium Alloys
Copper
Intermetallic Compounds

Processing of MMCs
Many processes for fabricating metal
matrix 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-situ
process of incorporating a
reinforcement phase.

Duralcan Process
A 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 melt

Foundry-grade MMCs
High silicon aluminium alloys (e.g., A356)
Alumina particles

Wrought MMCs
Al-Mg-type alloys (e.g., 6061)
Silicon carbide particles

Stir Casting

Stirring of composite melt with ceramic particles to minimize

settling of the particles during processing.

Squeeze Infiltration
The molten metal is infiltrated into the
reinforcement preform under pressure

This method obviates the requirement of

good 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

Press Forming of Preform

Squeeze infiltration technique of composite fabrication

Diesel engine piston

(Saffil alumina fibre/Al composite)

Made by squeeze casting

Powder Metallurgy
Technique
Mixing

Compaction
Sintering/hot pressing

Powder metallurgy and extrusion

processing of Al/SiCp composites
Powder Metallurgy Manufacturing Route
for SiCp/Al-2080 Composites
P/M Al

SiCp

Vacuum degassing

Blending of gas
atomized powders
Cold Isostatic Compaction

Pressure

Particle reinforced
metal matrix composite

Extrusion

Hot pressing
Graphite die

Diffusion Bonding Process

A solid state processing method

Schematic of diffusion bonding process

The microstructure of SiC fibre/titanium matrix composite

made by diffusion bonding

In-situ Process
Composite material is produced in one
step from an appropriate starting alloy
Reinforcement phase is formed in-situ
Avoiding the difficulties inherent in
combining the separate components

The solidification rate in practice,

however, is limited to a range of
1-5 cm/h for fibre-reinforced
composites
Many particulate reinforced composites
are now-a-days made with this process

Transverse section of in-situ

composites obtained at different
solidification rates
Solidification rates indicated in lefthand top corners (cm/h)

Types of Ceramic Composites

Oxide and Non-oxide Ceramic composites
Silica, alumina, SiC, Si3N4 and other ceramics
are reinforced with carbon, silicon nitride or
silicon 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 as
body implants
Can be used up to 1500C under inert
conditions

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 resistance

Cement composites
Portland cement can be reinforced with
glass, plastics, asbestos or steel fibres
for building and construction industry

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

Limitations of Cold Pressing &

Sintering
The reinforcement phase can form a
connective network throughout the
composite.

This network will resist densification and leads

to a porous microstructure.

Large residual stresses can develop in

composites during sintering due to thermal

expansion mismatch between the
constituent phases.

These stresses can sometimes be large

enough to cause cracking in the composite.

Hot pressing
Simultaneous application of
pressure and high temperature
Pore-free and fine grained compact
Limitations
Difficult to produce complex shapes
Very high pressure can easily damage
fibres

Low production rate

Hot pressing

Similar to die
compaction

But, the whole die set-up

is heated

Die is usually made from

graphite

Allows external induction

heating

Other common die

materials

Refractory metals & their

alloys

If the compact exhibits

incompatible thermal
expansion

Ejected at high
temperature

A cross-sectional view of the uniaxial hot

pressing operation

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 & pressures

up to 200 MPa are possible
Useful for large components, where full
density & isotropic properties are required

Hot isostatic pressing

One variant is to use previously
sintered compacts
Component already has the desired
shape
Densities over 92% TD
Closed pores allow for HIP

Widely used to consolidate

cemented carbides, ceramic
composites, and wear resistant
materials

Reaction bonding process

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

Schematic diagram of directed metal oxidation process of Lanxide Corp.

Chemical Vapour Impregnation

Advantages
Good mechanical properties at high
temperatures
Large, complex shapes can be
produced to a near-net shape
Considerable flexibility in the fibres
and matrices

Disadvantages
Process is slow and expensive

Isothermal chemical vapour

infiltration process

Schematic diagram of a chemical vapour infiltration process with pressure

and temperature gradients (Chawla, Composite Materials)

Sol-gel Processing
A solution containing metal compounds,
e.g., a metal alkoxide, acetate, or
halide, is reacted to form a sol.
This sol can be used to
impregnate/infiltrate reinforcements

The sol is converted to a gel.

The gel is subjected to controlled

heating to produce the desired end
product
a glass, a glass-ceramic, or a ceramic
material.

Sol-gel Processing
Advantages
lower processing temperatures
greater compositional homogeneity
potential for producing unique multiphase
matrix materials
allows processing via liquids of low viscosity

Disadvantages
high shrinkage
results in a large density of cracks in the
matrix
generally, repeated impregnations are
required to produce a substantially dense
matrix

Polymer Infiltration &

Pyrolysis (PIP)
Formation of ceramic matrix
materials by high temperature
pyrolysis of polymeric materials
containing the constituent
elements.

References
1. Chawla, K.K. (2012) Composite
Materials: Science and Engineering,
3rd Edition, Springer Verlag.
2. Mallick, P.K. (2008) Fiber-reinforced
Composites, 3rd Edition, CRC Press,
Boca Raton.
3. Balasubramanian, M. (2013)
Composite Materials and Processing,
CRC Press, Boca Raton.

Thank You