Kwame Nkrumah University of

Science & Technology, Kumasi, Ghana

MSE 351
Engineering Ceramics I

Anthony Andrews (PhD)

Associate Professor
Department of Materials Engineering
Faculty of Mechanical and Chemical Engineering
College of Engineering
Website: www.anthonydrews.wordpress.com
Online Lectures: classroom.knust.edu.gh

Teaching Assistant: Miss Freda Quaye

1
 Kwame Nkrumah University of
Science & Technology, Kumasi, Ghana

UNIT 3

CERAMIC SYNTHESIS – Part 2

2
 Content

• Ceramic types and processing routes

• Characteristics and properties of ceramic powders

• Ceramic powder processing

• Ceramic shaping methods

• Sintering and densification

www.knust.edu.gh

3
 Learning Outcome

1. Identify the various ceramic powder synthesis processes

2. List the properties of ideal ceramic powders

3. Identify the various forming processes

4. Understand sintering and grain growth

www.knust.edu.gh

4
 Shaping Processing

• Hot pressing
• Isostatic pressing
• Slip casting
• Extrusion
• Injection moulding

www.knust.edu.gh

5
Traditional Ceramic Processing

www.knust.edu.gh

6
 Shaping Processes
• Slip casting
– The clay-water mixture is a slurry

• Plastic forming methods

– The clay is plastic

• Semi-dry pressing
– The clay is moist but has low plasticity

• Dry pressing
– The clay is basically dry (less than 5% water) and has no
plasticity
www.knust.edu.gh

7
Effect of Water Content in Shaping
Processes

www.knust.edu.gh

8
 Slip Casting
• Slip, is poured into porous plaster of paris mold

• Water from the mix is absorbed into the plaster to form a firm layer
of clay at the mold surface

• Slip composition is 25% to 40% water

• Two principal variations:

– Drain casting
– Solid casting

www.knust.edu.gh

9
Drain Casting

www.knust.edu.gh

10
 Dry Pressing

• Process sequence similar to semi-dry pressing

• Dies made of hardened tool steel or cemented carbide

• No drying shrinkage occurs

• Products: bathroom tile, electrical insulators, refractory brick, and

other simple geometries

www.knust.edu.gh

11
Dry Pressing

www.knust.edu.gh

12
 Sintering - Definition
• Sintering is the thermal treatment for bonding particles into a
coherent solid structure via mass transport events that often occur
on the atomic scale

• Density is a measure of the degree of sintering

• Theoretical density
• Measured density (% theoretical density)

• Green density
• Green strength Prior to sintering
• Green porosity

• Fractional porosity + fractional density = 1 (for SSS)

www.knust.edu.gh

13
 Sintering - Definition
• Powders are collections of particles with a range of sizes and
shapes
• Packing of monosize particles in a container = 60% density
• Vibration effect = 64% density

• Higher densities achieved by changing particle shape, PSD, or

application of pressure
• Compacts – green bodies prior to sintering (add binder or
lubricant)

• Shrinkage vs swelling

• Mixed powders of different compositions are common basis for

sintering
• Example: WC-Co; Fe-8Ni
www.knust.edu.gh

14
 Experimental aspects of sintering
Parameters used to regulate sintering and control the development
of the microstructure

• Composition of the starting system

• chemical composition of the starting powders
• size and shape of the particles
• compactness rate of the pressed powder

• Sintering conditions
• treatment temperature
• treatment duration
• treatment atmosphere
• pressure during the heat treatment (for pressure sintering).

www.knust.edu.gh

15
 Sintering Definition
• Sintering is defined as a thermal treatment of a powder or
powder compact at an elevated temperature below the melting
temperature
• The goal of sintering is to increase powder compact strength

General fabrication pattern of sintered pattern

www.knust.edu.gh

16
 Types of Sintering
• Solid phase sintering – only solid phases are present

• Liquid phase sintering – liquid phases are also present

• Reactive phase sintering – different phases are present which

react to produce new phases

www.knust.edu.gh

17
Schematics of the two sintering
processes

www.knust.edu.gh

18
Stages in Sintering

a) Green body, loose powder

b) Initial stage: increase of the
interparticle contact area from 0 to 0.2
grain diameter (neck formation),
increase of the density from 60 to 65%
c) Intermediate state: further increase
of the contact area, stage characterized
by continuous pore channels along
three grain edges (pore closure),
increase of the density from 65 to 90%
d) Final stage: Elimination of the pore
channel along three grain edges (grain
growth), increase of the density to 95
to 99%

www.knust.edu.gh

19
Simplest temperature protocol

www.knust.edu.gh

20
To develop analytical models for sintering,
the two-particle approximation is used

www.knust.edu.gh

21
Mass transport at green compact
contact area

www.knust.edu.gh

22
Densification During Firing

www.knust.edu.gh

23
 Dimensional changes during
densification
• Shrinkage is expressed relative to some fixed starting
point.

• Linear firing shrinkage versus volumetric shrinkage

• Isotropic dimensional change – percent linear shrinkage

is the same in all directions

www.knust.edu.gh

24
 Dimensional changes during
densification
• During sintering the bulk density of the part should
approach the theoretical density of the material

• Bulk density = mass of part / geometric volume of part

• Density of sintered parts are expressed as percent of

theoretical densities
𝜌𝐵𝑢𝑙𝑘
𝜌 % = × 100
𝜌𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙

www.knust.edu.gh

25
 Important outcome of sintering

• Volumetric shrinkage
In most cases
• Densification
• Reduction of pore volume and size
• Significant enhancement of mechanical strength
• Grain coarsening (if not controlled)

www.knust.edu.gh

26
Typical Shrinkage Behaviour

www.knust.edu.gh

27
Grain size versus density variation

www.knust.edu.gh

28
Grain size versus pore size variation

www.knust.edu.gh

29
 Uniaxial Pressing
• Can be done cold or hot.
• Done to achieve desired features in the green compact.
– Eg. Uniformity, lack of defects, high green density and high green strength

• Hot pressing is similar to dry pressing

– Except it is carried out at elevated temperatures so sintering of
the product is accomplished simultaneously with pressing
– Higher densities and finer grain size are obtained
• Die life is reduced by the hot abrasive particles against the
die surfaces

www.knust.edu.gh

30
 Uniaxial Pressing – Wall Effect

“diabolo” effect in
single effect pressing

Pressure profiles within a compressed piece starting from a non-granulated

powder
www.knust.edu.gh

31
 Isostatic Pressing
• Uses hydrostatic pressure to compact the ceramic
powders from all directions

• Avoids the problem of non-uniform density in the final

product that is often observed in conventional uniaxial
pressing

• Die wall friction is significantly reduced or eliminated

entirely

www.knust.edu.gh

32
 Isostatic Pressing

Principles of isostatic pressing: a) wet mold, b) dry mold

www.knust.edu.gh

33
Typical temperature profile for sintering
of the nanoscale silver pastes

www.knust.edu.gh

34
www.knust.edu.gh

35
Effect of Sintering Temperature on Hardness of WC- 20
Wt.% (Fe,Co) Cemented Carbides

www.knust.edu.gh

36
 Secondary Operations

• Secondary operations are necessary to:

• Achieve the required dimensional accuracy

• Surface finish
• Specific geometrical features

• Since ceramics generally have high hardness, the conventional

machining processes used for finishing metals cannot be used
for ceramics

www.knust.edu.gh

37
 Secondary Operations

• The selection of the process depends on the properties of the

ceramics such as:

• Brittle
• High hardness
• High melting point
• Electrical conductivity
• Thermal conductivity

www.knust.edu.gh

38
 Secondary Operations

• Operations used are:

• Ultrasonic machining
• Abrasive water jet machining
• Laser beam machining
• Lapping
• Grinding

www.knust.edu.gh

39
 Ceramic Coatings
• Ceramic coatings are used to improve the resistance to
indentation, wear and erosion

• Improve the resistance to corrosion

• Used to improve the aesthetic aspects by imparting special

surface texture, finish and colour

• Coating extends the useful life of many components

www.knust.edu.gh

40
 Chemical Vapor Deposition (CVD)

• CVD is used to grow a thin layer of a ceramic material on the

surface of the substrate

• A solid material is deposited from a vapor by a chemical reaction

occurring on normally heated surface of the substrate

• The solid material is obtained as a coating

• High temperature process

www.knust.edu.gh

41
 Chemical Vapor Deposition (CVD)

• Experimental conditions:

• Substrate material
• Substrate temperature
• Composition of the reacting gas mixture

• Typical application: coating of cutting tools with TiN

www.knust.edu.gh

42