Lecture: 5-6

Processing Techniques
Ceramic Materials- Science and Engineering- Carter & Norton

MME 467
 Powder Processing Techniques

(Reduction of particle size, traditional ceramics)

(Exceptional control, advanced ceramics)
(Expensive, nano particles of nonoxides)

Lecture 5 Powder Processing

 Types of Powders
 Primary particles (can not be easily broken into small
units)
 Agglomerates (are clusters of bonded primary
particles, soft and hard agglomerates )
 Particles ( general term for both)
 Granules (large agglomerates,0.1-1 mm in diameter)
 Flocs (clusters, in a liquid, held electrostatically)
 Colloids
 Aggregates

Lecture 5 Powder Processing

 MECHANICAL METHOD MECHANICAL MILLING

Ball Milling
Adv: simple and inexpensive
Disadv: no ultrafine particles,
impurities.

Jet Milling
Size reduction in a high-velocity fluid, usually
either compressed air or superheated
steam.

The powder is added to the fluid and

injected into the grinding chamber at sonic or
near-sonic velocity.
collecting the fine powder that is mixed into
the gas stream.

Lecture 5 Powder Processing

 MECHANICAL METHOD
Vibration Milling

Powder is vigorously shaken.

The collisions between the media are much more
violent than they are in ball milling
 this can shorten milling times.

Attrition Milling

Agitated ball milling,

Differs from conventional ball milling in that
the milling chamber does not rotate.
Instead, a slurry containing the particles and
media is stirred continuously

Lecture 5 Powder Processing

 Chemical Method- Spray Drying
At first precursors of ferrites, titanates are
produced
Fine droplets produced by an atomizer are
sprayed into a drying chamber .

The flow pattern of the hot air determines

the completeness of moisture removal
Finally the particles are carried out of the
chamber in the air stream
 Captured in a bag or another form of
collector.

Then sintering .

Variables:
Droplet size, concentration and composition, temperature and chamber design

Lecture 5 Powder Processing

 Chemical Method- Solgel Process
Advantage

 It uses relatively low temperatures.

 It can create very fine powders.
 It produces compositions not possible by solid-state fusion.

Disadvantage
The cost of the raw materials (the chemicals) may be high

There is often a large volume shrinkage and cracking during drying and firing.

Lecture 5 Powder Processing

 Chemical Method- Solgel Process

Lecture 5 Powder Processing

 Chemical Method- Solgel Process
In ceramic synthesis, two different sol-gel
routes have been identified and depend
on the gel structure.

• Particulate gel—using a network of

colloidal particles

• Polymeric gel—using an array of

polymeric chains

Lecture 5 Powder Processing

 Chemical Method- Solgel Process
Alkoxides have the general formula M(OR)z
where M is usually a metal, but can also be a nonmetal such as Si,
and R is an alkyl chain.

The first alkoxide to be synthesized was silicon tetraisopentoxide

(formerly called silicon tetraisoamyloxide), made by a reaction
between silicon tetrachloride and isopentanol (formerly isoamyl
alcohol):

Lecture 5 Powder Processing

 Chemical Method- Solgel Process1

Three-necked flask (contains the mixed solutions)

Mechanical stirrer (the mixture is stirred constantly)
Reflux condenser (needed to prevent the solution from
evaporating)
Constant temperature bath (the rate of hydrolysis
depends on temperature)

Lecture 5 Powder Processing

 Chemical Method- Solgel Process1

Lecture 5 Powder Processing

 Chemical Method- Solgel Process1

Lecture 5 Powder Processing

 SOL-GEL PROCESS
pH<2.5 acid, pH>2.5, basic

Lecture 5 Powder Processing

 Drying and Firing
Weak skeleton of amorphous material. Alcohol and water, which must be removed.
Shrinkage during this step is usually large

During firing, further changes occur as the gel densifies. The driving forces for
these changes are as follows:
Reduction of the surface area provides a driving force for densification.
The free energy, ΔGf, of the polymerization reaction and this acts as a driving
force for increasing the amount of cross-linking.

Lecture 5 Powder Processing

 Factors controlling sol-gel process
Rates of hydrolysis and condensation (relative differences in the rates can

be used to modify the microstructure of the powder)

Type of alkoxide (mixing of the alkoxides in the solution is achieved at a

molecular level giving the powders a high degree of chemical homogeneity)

Amount of water added (affects the degree of polymerization of the gel)

Solution pH (rates of hydrolysis and condensation can be changed by the

addition of acids or bases, respectively)

Lecture 5 Powder Processing

 Powders by Precipitation

Lecture 5 Powder Processing

 Powders by Precipitation

Lecture 5 Powder Processing

 Pechini Method

Lecture 5 Powder Processing

 Chemical Method for non oxides
Si3N4 production (morphology)

SiCl4 + 2NH3 → 3Si(NH)2 + 12 HCl

3Si(NH)2 → Si3N4 + 2NH3

SiC production (dechlorination)

SiCl4 + CCl4 + 8Na → “SiC” + 8NaCl

Lecture 5 Powder Processing

 Vapor Method

Lecture 5 Powder Processing

 DEFINING THICK FILMS
THICK FILMS: 10-25 µm The ways thick and thin films are produced
THIN FILM: <500 nm are significantly different

TAPE CASTING

To produce ceramic
flat sheets with
maximum thickness
upto 1 mm

Lecture 6 Thick Film Processing

 TAPE CASTING

CONTROLLING PARAMETERS

AMOUNT OF BINDER TO HOLD SHAPE SOLVENT CONTROL FOR UNIFORM SPREADING

PLASTICIZER TO ROLL THE GREEN BODY DISPERSANT TO AVOID SETTLING

Lecture 6 Thick Film Processing

 DIP COATING

THICKNESS DEPENDS ON the viscosity, η, of the solution and the speed, v, with
which the object is withdrawn from the solution

Lecture 6 Thick Film Processing

 SPIN COATING

STATIC FORM
SPREADING OF COATING
AND THEN ROTATION

DYNAMIC FORM
SIMULTANEOUS
SPREADING AND ROTATION

THICKNESS DEPENDS ON THE ANGULAR VELOCITY OF THE COATER AND VISCOSITY OF THE COATING

Lecture 6 Thick Film Processing

 THERMAL SPRAYING MAIN USE: WEAR RESISTANT AND
THERMAL BARRIER

THIS PROCESS USES

OXYACETYLENE FLAME TO MELT OR
SOFTEN THE POWDER TO BE
DEPOSITED

TEMPERATURE IN THE RANGE OF

10,000 K

Lecture 6 Thick Film Processing

 PLASMA SPRAYING
NO FLAMES HERE, RATHER
ARC IS CREATED BETWEEN
A COPPER ANODE AND
TUNGSTEN CATHODE

THE ARC IONIZES THE

INCOMING GAS AT AROUND
28,000 K

Lecture 6 Thick Film Processing

 PLASMA SPRAYING

THERMAL
BARRIER
COATING

Lecture 6 Thick Film Processing

 ELECTROPHORETIC DEPOSITION
MOVEMENT OF CHARGED PARTICLES THROUGH A
LIQUID UNDER THE INFLUENCE OF AN EXTERNAL
ELECTRIC FIELD

Large particle ……. Small particle

mobility is proportional to κ.

Lecture 6 Thick Film Processing

 ELECTROPHORETIC DEPOSITION
RESPONSE TO INCREASING pH OF THE SOLUTION

MOVEMENT OF PARTICLE

ACIDIC
BASIC

Zero Mobility

Lecture 6 Thick Film Processing