TEKNOLOGI KERAMIK

ENMT6000025

FABRICATION TECHNIQUES OF
CERAMICS
Teaching team:
Prof. Dr. Ir. Akhmad Herman Yuwono, M.Phil.Eng.
Dr. Sotya Astutingingsih, M.Eng

DEPT. of METALLURGY & MATERIALS ENGINEERING

FAC. of ENGINEERING UNIVERSITAS INDONESIA
 ISSUE TO ADDRESS...
2

How is processing of ceramics different than for

metals?
Ceramic fabrication techniques:
Glass forming: pressing, blowing, fiber drawing).
Particulate forming: hydroplastic forming, slip
casting, powder pressing, tape casting
Cementation
Processing of Ceramics

Two distinct classes of processing ceramics:

Glasses are manufactured by means of molten material
via viscous flow
Crystalline ceramics are manufactured by pressing
moist aggregates or powder into shape
The material is then bonded together using one of
several mechanisms
Chemical reaction
Vitrification
Sintering
 Ceramic Fabrication Methods (i)
4

GLASS PARTICULATE CEMENTATION

FORMING FORMING

Blowing of Glass Bottles: Pressing: plates, cheap glasses

Pressing -- glass formed by application of
Gob
operation
pressure
Parison
-- mold is steel with graphite
mold lining
Fiber drawing:
Compressed
air

Suspended
parison

Finishing
mold wind up
Adapted from Fig. 13.8, Callister & Rethwisch 8e. (Fig. 13.8 is adapted from C.J.
Phillips, Glass: The Miracle Maker, Pittman Publishing Ltd., London.)
 Sheet Glass Forming
5

Sheet forming continuous casting

sheets are formed by floating the molten glass on a pool of molten tin

Adapted from Fig. 13.9,

Callister & Rethwisch 8e.
Sheet Glass Forming

Sheet forming continuous draw

originally sheet glass was made by floating glass on a
pool of mercury or tin

Adapted from Fig. 13.9, Callister 7e.

Modern Plate/Sheet Glass making:

Image from Prof. JS Colton, Ga. Institute of Technology

 Glass Structure
8

Basic Unit: Glass is noncrystalline (amorphous)

Fused silica is SiO2 to which no
4- impurities have been added
Si0 4 tetrahedron
Other common glasses contain
Si 4+ impurity ions such as Na+, Ca2+,
Al3+, and B3+
O2-

Quartz is crystalline
SiO2: Na +
Si 4+
O2-

(soda glass)
Adapted from Fig. 12.11,
Callister & Rethwisch 8e.
 Glass Properties
9

Specific volume (1/r) vs Temperature (T):

Crystalline materials:
Specific volume -- crystallize at melting temp, Tm
-- have abrupt change in spec.
Supercooled Liquid vol. at Tm
Liquid (disordered)

Glass Glasses:
(amorphous solid)
-- do not crystallize
Crystalline -- change in slope in spec. vol. curve at
(i.e., ordered) solid glass transition temperature, Tg
Tg Tm T -- transparent - no grain boundaries to
scatter light
Adapted from Fig. 13.6,
Callister & Rethwisch 8e.
 Glass Properties: Viscosity
10

Viscosity, h:
-- relates shear stress () and velocity gradient (dv/dy):

dy dv
glass dv h
dy dv / dy

velocity gradient

h has units of (Pa-s)

 Log Glass Viscosity vs. Temperature
11

Viscosity decreases with T soda-lime glass: 70% SiO2

balance Na2O (soda) & CaO (lime)
borosilicate (Pyrex):
13% B2O3, 3.5% Na2O, 2.5% Al2O3
Vycor: 96% SiO2, 4% B2O3
fused silica: > 99.5 wt% SiO2
Viscosity [Pa-s]

10 14 strain point
annealing point
10 10

10 6 Working range:
glass-forming carried out
10 2 Adapted from Fig. 13.7, Callister & Rethwisch
Tmelt 8e. (Fig. 13.7 is from E.B. Shand,
1 Engineering Glass, Modern Materials, Vol. 6,
200 600 1000 1400 1800 T(C) Academic Press, New York, 1968, p. 262.)
 Heat Treating Glass
12

Annealing:
-- removes internal stresses caused by uneven cooling.
Tempering:
-- puts surface of glass part into compression
-- suppresses growth of cracks from surface scratches.
-- sequence:

before cooling initial cooling at room temp.

cooler compression
hot hot tension
cooler compression

-- Result: surface crack growth is suppressed.

 Ceramic Fabrication Methods (iia)
13

GLASS PARTICULATE CEMENTATION

FORMING FORMING

Hydroplastic forming:
Mill (grind) and screen constituents: desired particle size
Extrude this mass (e.g., into a brick)

Ao
container die holder
force Adapted from
ram billet extrusion Ad Fig. 12.8(c),
Callister &
container die Rethwisch 8e.

Dry and fire the formed piece

 Typical Porcelain Composition
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(50%) 1. Clay
(25%) 2. Filler e.g. quartz (finely ground)
(25%) 3. Fluxing agent (Feldspar)
-- aluminosilicates plus K+, Na+, Ca+
-- upon firing - forms low-melting-temp. glass
 Hydroplasticity of Clay
15
Shear
Clay is inexpensive
When water is added to clay
-- water molecules fit in between charge
layered sheets neutral
-- reduces degree of van der Waals
bonding
-- when external forces applied clay
weak van
particles free to move past one
another becomes hydroplastic der Waals
bonding
4+
charge Si
Structure of Kaolinite Clay: 3+
neutral Al
-
Adapted from Fig. 12.14, Callister &
OH
2-
Rethwisch 8e. (Fig. 12.14 is adapted from O
W.E. Hauth, "Crystal Chemistry of
Ceramics", American Ceramic Society
Bulletin, Vol. 30 (4), 1951, p. 140.) Shear
 Drying and Firing
16

Drying: as water is removed - interparticle spacings decrease

shrinkage .
Adapted from Fig.
13.13, Callister &
Rethwisch 8e. (Fig.
13.13 is from W.D.
Kingery, Introduction
to Ceramics, John
Wiley and Sons,
Inc., 1960.)
wet body partially dry completely dry
Drying too fast causes sample to warp or crack due to non-uniform shrinkage
Firing: micrograph of porcelain Si02 particle
-- heat treatment between (quartz)
900-1400C glass formed
-- vitrification: liquid glass forms around
from clay and flux flows the particle

between SiO2 particles. (Flux

lowers melting temperature). 70mm
 Ceramic Fabrication Methods (iib)
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GLASS PARTICULATE CEMENTATION

FORMING FORMING

Powder Pressing: used for both clay and non-clay compositions.

Powder (plus binder) compacted by pressure in a mold

-- Uniaxial compression - compacted in single direction
-- Isostatic (hydrostatic) compression - pressure applied by fluid - powder in
rubber envelope
-- Hot pressing - pressure + heat ( porosity reduced)
 Sintering
18

Sintering occurs during firing of a piece that has been powder pressed
-- powder particles coalesce and reduction of pore size

Adapted from Fig. 13.16,

Callister & Rethwisch 8e.
Aluminum oxide powder:
-- sintered at 1700C
Adapted from Fig. 13.17, Callister
for 6 minutes. & Rethwisch 8e. (Fig. 13.17 is from
W.D. Kingery, H.K. Bowen, and
D.R. Uhlmann, Introduction to
Ceramics, 2nd ed., John Wiley and
Sons, Inc., 1976, p. 483.)

15 mm
 Tape Casting
19

Thin sheets of green ceramic cast as flexible tape

Used for integrated circuits and capacitors
Slip = suspended ceramic particles + organic liquid
(contains binders, plasticizers)

Fig. 13.18, Callister &

Rethwisch 8e.
 Ceramic Fabrication Methods (iii)
20

GLASS PARTICULATE CEMENTATION

FORMING FORMING
Hardening of a paste paste formed by mixing cement material with
water
Formation of rigid structures having varied and complex shapes
Hardening process hydration (complex chemical reactions involving
water and cement particles)

Portland cement production of:

-- mix clay and lime-bearing minerals
-- calcined (heat to 1400C)
-- grind into fine powder
 Sol-Gel Processing
Sol-gel processing is a wet chemical route for
synthesis of colloidal dispersions of inorganic and
organic-inorganic hybrid materials, particularly
oxides and oxide-based hybrid.
This method can be used to prepare powders, fibers,
thin films, and monolith.
The advantages include low processing temperature
and molecular level homogenity.

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 Sol-Gel Processing

Typical sol-gel processing consists of hydrolysis and

condensation of precursors.
Hydrolysis:

M(OEt)4 + xH2O M(OEt)4-x(OH)x + xEtOH

Condensation:

M(OEt)4-x(OH)x +M(OEt)4-x(OH)x
(OEt)4-x(OH)x-1MOM(OEt)4-x(OH)x-1 + H2O

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 Sol-Gel Processing
The evolution of a system from a colloidal suspension (the sol)
into a solid/semi-solid (the gel) phase
Hydrolysis Formation of a colloidal suspension (Sol)

M OR + HOH M OH + ROH

Gelation of the sol to form a network (Gel)

Condensation

M OH + M OH M O M + HOH Water liberation

OH M O M + ROH Alcohol liberation

M + M OR
 Sol-Gel Processing

Advantages:
Simpler composition control
High reactivity
Lower synthesis temperature 300oC
Disadvantages:
Influence by: alkalinity, reagents, concentration,
nature of precursors and mineralizer
Spray technique may induce crack
SOL-GEL PROCESSING

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 Sol-Gel Processing
THE EFFECT OF PH ON THE SOL-GEL STRUCTURE
 Sol-Gel Processing
THE EFFECT OF PH ON THE SOL-GEL STRUCTURE
Sol-Gel Processing