Chap 2-Ceramic Technology

16-Jan-24
Course instructor: HUỲNH NGỌC MINH
CONTENT
1. Traditional ceramics and advanced ceramics
2. Ceramic fabrication process
3. Raw materials used in traditional ceramics
4. Powder preparation
5. Forming methods (shaping)
6. Drying behaviors
7. Firing & Sintering
8. Glaze and decoration application techniques
9. Introduction some advanced ceramics
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Learning outcomes
2.1 Traditional ceramics and advanced ceramics
2.1.1 Briefly define “traditional ceramic” and
“advanced ceramic”
2.2 Note some types of traditional ceramics and, for
each, its distinctive feature(s).
2.2 Ceramic fabrication process
2.2.1 Briefly describe /diagram the ceramic
fabrication process
2.2.2 Understand the purpose of each stage in the
ceramic production process
Learning outcomes
2.3 Raw materials used in traditional ceramics
2.3.1 Know three main raw materials used in
traditional ceramic (clay, silica, feldspar)
2.3.2 Describe the role of each of three main raw
materials on traditional ceramic fabrication (forming and
firing).
2.3.3 Cite the two desirable characteristics of clay
minerals relative to fabrication processes.
2.4 Powder preparation
2.4.1 Note the goal of the powder preparation.
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Learning outcomes
2.5 Forming methods (shaping)
2.5.1 Name and briefly describe forming methods
that are used to fabricate ceramic products.
2.5.2 Cite the criteria for the forming method
selection.
2.6 Drying behaviors
2.6.1 Define “drying”
2.6.2 Briefly describe processes that occur during
the drying green ceramics.
2.6.3 Cite (3) factors that influence the rate of
drying, and explain how.
Learning outcomes
2.7 Firing & Sintering
2.7.1 Define “sintering”, “firing” in ceramic process
2.7.2 Briefly describe/diagram the sintering process

of powder particle aggregates.
2.7.3 Know various stages of firing and various

factors related to firing operation of ceramic products
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Learning outcomes
2.8 Glaze and decoration application techniques
2.8.1 Understand the role of ceramic coating
2.8.2 Note the desirable properties of glaze
2.8.3 Know various glaze coating methods
2.8.4 Note three conventional pigments used in

ceramic materials
2.9 Introduction some advanced ceramics

2.9.1 Note some types of advanced ceramics and,
for each, its distinctive feature(s). 7
1.4. TYPES AND APPLICATIONS OF CERAMICS

Applications of ceramics
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FUNCTIONAL CLASSIFICATION OF CERAMICS
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TYPES OF CERAMIC MATERIAL
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2.1.1. TRADITIONAL CERAMICS

OR CLASSICAL CERAMICS
Vật liệu gốm
Ceramic materials
Gốm sứ VL chịu lửa VL mài Thủy tinh Xi măng Ceramic tiên

Clay products Refractories Abrasives Glasses Cements tiến
Advanced
Thủy tinh ceramics
Gốm kết cấu, gốm
xây dựng Glasses
Structural clay
products Gốm thủy
tinh
Glass-
Gốm sứ dân dụng Ceramics
Whitewares
Based on mineral silicates, silica, and mineral oxides found in nature

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Clay products (Các sp gốm từ đất sét)
-earthenware e.g. plant pot -porcelain e.g. table wares
(dirty red brown, very cheap, plate, souvenirs
opaque) (clean, light, translucency)
-stoneware e.g. coffee mug, -bone china e.g. table wares,

plate, bowl souvenirs
(very clean, very expensive,
(cheap, heavy, opaque) very good translucency,
light, mostly ivory colour)
earthenware stoneware porcelain bone china

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History
 Clay has been used by humans as long ago as
37,000-12,000 BC (Ice Age!)
 Clay was first fired by humans in what is now East
Asia, and by 6,000-4,000 BC, firing clay had become
widespread. Cultures on almost every continent now
have long-standing ceramic traditions.
 Fired clay enabled humans to store grain and led to
a more settled, agricultural existence.
 Glazes were first developed in 4,000 BC in
Egypt/Mesopotamia. Glazes developed not only for
decorative purposes, but they also made containers
strong and waterproof.
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Earthenware (đồ đất nung)
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Earthenware (Structural Clay Products)
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Earthenware (Decorative ceramics)
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 Firing temperature: 1000-1180 ̊ C. Low fired!
 Rather porous, lighter feel
 Found around the world
 Can be grey, white, red, orange, buff, yellow and/or
brown
 Red clay contains iron oxide, which gives it its color
and keeps the firing temperature low.
 Often used to make flower pots, bricks, tiles, etc.
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Stoneware (Đồ sành)
 Firing temperature:
1200-1300 ̊C. High
fired!
 Hard, dense clay body
which has a water
absorption rate of 3%
or less when fully fired
 Colors can be off-white,
tan, grey and/or brown
 Often used for “art
pottery”: jugs, mugs,
plates, bowls, etc.
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Porcelain (Sứ)
 Firing temperature: 1240-1350oC. High Fired!
 Translucent, waterproof and “rings like a bell” when
fully vitrified.
 Dense, smooth clay body
 Once a luxury item that drove global trade in the 17th
century, it’s now readily available and used to make
dishes, plates, mugs, bowls, statue, etc.
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Porcelain (Sứ)
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Sanitary-ware (Gốm / sứ vệ sinh)
Ceramic wash basins

Toilets
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Decorative ceramics (Gốm trang trí)
.
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2.1.2. ADVANCED CERAMICS

(GỐM TIÊN TIẾN)
Advanced ceramic materials have been developed
over the past half century.
 Structural: Wear parts, bioceramics, cutting tools,
engine components, armor.
 Electrical: Capacitors, insulators, integrated circuit
packages, piezoelectrics, magnets and
superconductors
 Coatings: Engine components, cutting tools, and
industrial wear parts
 Chemical and environmental: Sensors, filters,
membranes, catalysts, and catalyst supports.
…
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 SENSOR
 THERMAL PROTECTION SYSTEM Ceramic knife
 BIOCERAMICS
 MAGNETIC MATERIALS
 ELECTRONIC MATERIALS
Electronic materials
Biomaterials Magnetic materials 28
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“FINE CERAMICS (Gốm tinh / mịn)
The picture “Fine
ceramic tree” shows
relationships between
advanced ceramic
materials and
properties.
In Japan, the
expression “Fine
ceramic” is similar to
advanced ceramics
and used rather than
advanced ceramics.
Published by Japan Fine Ceramics Association

(JFCA), 2012. 29
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Electrical ceramics (Gốm điện)
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Chemical ceramics (Gốm bền hóa)
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Ceramics used in textile machines (Gốm máy dệt)
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Abrasives (vật liệu mài)
 Natural (garnet, diamond, etc.)

 Synthetic abrasives (silicon carbide, diamond, fused
alumina, etc.) are used for grinding, cutting,
polishing, lapping, or pressure blasting of materials.
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Cutting tools (dụng cụ cắt)
• Tools:
-- for grinding glass, tungsten,
carbide, ceramics
-- for cutting Si wafers
-- for oil drilling
• Materials: oil drill bits blades
-- manufactured single crystal Single crystal
diamonds
or polycrystalline diamonds
in a metal or resin matrix.
-Diamond simulants: cubic zirconia, polycrystalline

silicon carbide… diamonds in a resin
matrix.
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Refractories (vật liệu chịu lửa)
 Refractories are used for furnaces and ovens in the
manufacturing plant for iron and steel, non-ferrous
metals, glass, cements, ceramics, energy
conversion, petroleum, and chemical industries.
 They are usually composed of alumina

(Tmelt=2050°C) and silica along with other oxides:
MgO (Tmelt =2850°C), Fe2O3, TiO2, etc., and have
intrinsic porosity typically greater than 10% by
volume.
 Specialized refractories: BeO, ZrO2, mullite, SiC, and

graphite with low porosity are also used.
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Refractories (vật liệu chịu lửa)
W. D. Kingery, H. K. Bowen, and D. R. Uhlmann, Introduction to Ceramics, 2nd edition. John Wiley & Sons36
Copyright © 1976 by, New York.
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Typical steps of ceramics processing

Raw Sources: nature (minerals), synthesis
materials
• Milling / Blending / Spray drying
Powder • Powder characterization: composition,
preparation microscopy, partical size and distribution,
XRD, surface area …
Forming / • Slip casting
Casting
• Plastic forming
• Powder pressing / compaction /
Drying • Liquid (water) is removed
• Shrinkage
Green body
Firing • Calcination
• Sintering
Secondary • Grinding / Cutting / Polishing

processing • Glazing (coating) / Final sintering
Final
sintered
ceramic Strength, durability, density and desired
product properties are enhaned
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Examples of ceramic tiles

There are two basic types of tiles: glazed or unglazed
– Glazed tiles have a vitreous coat applied on top of the body, which provides
additional wear resistance. For decoration (digital or trad.) glazed tiles are required.
– Unglazed tiles undergo a single firing and are not decorated
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© 2014 Durst Phototechnik AG - www.durst-online.com - Norbert von Aufschnaiter
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Different techniques for processing of

not use clays or natural
advanced ceramics minerals because of impurities
©2003 Brooks/Cole, a division of Thomson Learning, Inc. 41
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Making powder-metallurgy parts

(ceramic technology)
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COMPARISON OF CONVENTIONAL CERAMICS

WITH ENGINEERING CERAMICS
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Mechanical properties of selected

advanced ceramics
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materials
Casting
• Plastic forming
• Shrinkage
Green body
• Sintering

Final
sintered
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2.3. RAW MATERIALS USED IN TRADITIONAL CERAMIC
 Mineral silicates (khoáng silicate), such as clays (đất

sét) of various compositions, feldspar (tràng thạch)
and silica (SiO2), such as quartz (vd: cát thạch anh),
are among the most abundant substances in nature
and constitute the principal raw materials for
traditional ceramics.
 Another important raw material for traditional
ceramics is alumina (Al2O3).
 These solid crystalline compounds have been
formed and mixed in the earth’s crust over billions of
years by complex geological processes.
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Clay Products
Clay (50%)
Plasticity → formability
Must
be clean and
pure enough for Silica
Feldspar (Flux) products (quartz sand / flint)
(25%) (25%)
Reduction for vitrification Increasing strength
temperature
Additives may be added
for improving particular properties
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Clay as a Ceramic Raw Material
 Clays consist of fine particles of hydrous aluminum
phyllosilicate (sheet silicate) minerals.
 Most common clays are based on the mineral:
smectite (Ca,Na,K)(Al,Mg,Fe,Zn)2(Si,Al)4O10(OH)2.nH2O,
kaolinite (Al2Si2O5(OH)4).
 When mixed with water, clay becomes a plastic
substance that is formable and moldable.
 When heated to a sufficiently elevated temperature
(firing), clay fuses into a dense, strong material.
Thus, clay can be shaped while wet and soft, and
then fired to obtain the final hard product.
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Hydroplasticity of Clay (tính dẻo khi trộn nước)
Shear
• Clay is inexpensive
• When water is added to clay charge
-- water molecules fit in between neutral
layered sheets
-- reduces degree of van der
Waals bonding weak van der Waals
-- when external forces applied – bonding
clay particles free to move past one
another – becomes hydroplastic
4+
charge Si
• Structure of Al
3+
neutral
Clay mineral OH
-
2-
O
Shear
W. D. Callister and D. G. Rethwisch, Materials Science and Engineering: An Introduction, 9th ed. 51
John Wiley & Sons, Inc., 2013.
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Cấu trúc của nhóm khoáng smectite (tính dẻo)
Nguồn: R. H. A. Ras, Y. Umemura, C. T. Johnston, A. Yamagishi, and R. A. Schoonheydt,

“Ultrathin hybrid films of clay minerals,” Phys. Chem. Chem. Phys., vol. 9, no. 8, pp. 918–932,
Feb. 2007
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Silica SiO2 (quartz sand / flint) (cát thạch anh)
 as a filler material:
 being inexpensive,
 relatively hard,
 and chemically unreactive.
 It has a melting temperature ( ~1730oC) well above
the normal firing temperature (1000 – 1350 oC).
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Feldspars (tràng thạch)
 The feldspars are some of the more common fluxing
agents;
 They are a group of aluminosilicate materials that
contain K+, Na+, and Ca2+ ions (alkalis).
 A flux forms a glass that has a relatively low melting
point.
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Compositions for Typical Traditional Ceramics
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Porcelain tile compositions
for trational processing cycles
(1200-1220oC and cycles of 30-50 hrs)
for fast cycles (1200-1230oC and cycles of 50-70 mins)
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SACMI IMOLA s.c. a r.l. - 2005 - Applied ceramic technology- Volume 2
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materials
Casting
• Plastic forming
• Shrinkage
Green body
• Sintering

Final
sintered
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2.4. POWDER PREPARATION

Common methods for Ceramics
M. N. Rahaman, Ceramic Processing

and Sintering. CRC Press, 2003,pp 53 59
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 Particles and other ingredients (binders and

lubricants) are ground and blend wet or dry.
 This is followed by screening or sizing to yield a
powdered product having the desired range of
particle sizes and homogeneity.
 For multicomponent systems, powders must be
thoroughly mixed with water and perhaps other
ingredients to give flow characteristics that are
compatible with the particular forming technique.
M. N. Rahaman, Ceramic Processing and Sintering. CRC Press, 2003,pp 52 60
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by mechanical methods
 The process in which small particles are produced by
reducing the size of larger ones by mechanical
forces is usually referred to as comminution. It
involves operations such as crushing, grinding, and
milling.
 For traditional, clay-based ceramics, machines such
as jaw, gyratory, and cone crushers are used for
coarse size reduction of the mined raw material, to
produce particles in the size range of 0.1–1 mm.
 For the production of fine powders: high-
compression roller mills, jet mills (also referred to as
fluid energy mills), and ball mills.
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by mechanical methods
 In the milling process, the particles experience mechanical
stresses at their contact points due to compression, impact,
or shear with the mill medium or with other particles.
 The mechanical stresses lead to elastic and inelastic
deformation and, if the stress exceeds the ultimate strength
of the particle, to fracture of the particles.
 The mechanical energy supplied to the particle is used
not only to create new surfaces but also to produce other
physical changes in the particle (e.g., inelastic deformation,
increase in temperature, and lattice rearrangements within
the particle). Changes in the chemical properties (especially
the surface properties) can also occur, especially after
prolonged milling or under very vigorous milling conditions.
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Schematic of crushing and milling equipment
Source: From Principles of

Ceramics Processing,
Second Edition, by J.S.
Reed, p. 314, Figs. 17-1 and
17-2. Copyright © 1995 John
Wiley & Sons, Inc. Reprinted
by permission. Ball mill
grinding: Source: From
Modern Ceramic
Engineering, by D.W.
Richerson, p. 387, Fig. 9-3.
Copyright © 1992 Marcel
Dekker, Inc.) 63
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Jaw crusher
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Ball mill
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Ball mill
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materials
Casting
• Plastic forming
• Shrinkage
Green body
• Sintering

Final
sintered
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2.5. FORMING METHODS

Particulate
forming
Powder Hydroplastic Slip

pressing forming casting
%H2O 0- 10 15-20 20- 30
Extrusion
Throwing
Jiggering
Uniaxial
Isostatic
Hot
Green product
Drying
Firing
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Processes for shaping ceramics
❖Criteria for the selection:
• The shape and
characteristics of the
product.
• Technical properties of
batches.
• Capacity and costs, and
consumer tastes.
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Processes for shaping ceramics
Uniaxial pressing (ép 1 phía) Isostatic pressing (ép đẳng tĩnh)
Jiggering
Slip
(dao gạt)
Extrusion casting
(ép đùn) (đổ rót)
©2003 Brooks/Cole, a division of Thomson Learning, Inc. Thomson Learning is a trademark used herein under license.
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2.5.1. SLIP CASTING

(Tạo hình đổ rót)
• A slip (hồ) is a suspension (huyền phù) of clay and/or other
nonplastic materials in water.
• When poured into a porous mold (commonly made of plaster of
Paris (thạch cao)), water from the slip is absorbed into the mold,
leaving behind a solid layer on the mold wall.
• The thickness of pieces depends on the time.
• Slip casting operation

pour slip absorb water pour slip drain “green
into mold into mold into mold mold ceramic” Adapted from Fig.
“green 13.12, Callister &
ceramic” Rethwisch 8e. (Fig.
13.12 is from W.D.
Kingery, Introduction
to Ceramics, John
Wiley and Sons,
Inc., 1960.)
solid component hollow component
• The cast pieces then are dried and fired 73
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2.5.1. SLIP CASTING

(Source: From Modern Ceramic Engineering, by

D.W. Richerson, p. 462, Fig. 10-34)
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2.5.1. SLIP CASTING

 Advantages:
 Large parts, complex shapes;
 low equipment cost.
 Limitations:
 Low production rate;
 limited dimensional accuracy.
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2.5.2. PLASTIC FORMING

Wheel throwing (Vuốt / xoay tay)
A manual plastic forming method on the pottery wheel,
The moisture content is 23-27%.
Wheel throwing requires skill and experience.
Less used in industry, popular in fine arts and crafts.
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Molding (In / Ép dẻo trong khuôn)
 Often used to shape large-size products such as
flower pots, jars.
 The plastic soil is cut into thin sheets with the
required thickness. Then apply to the surface of the
mold, rubbing evenly.
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Jiggering (Tạo hình dẻo bằng dao gạt)
 Advantages:
• High production rate with automation;
• low tooling cost.
• Limitations:
• Limited to axisymmetric parts;
• Limited dimensional accuracy.
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Extrusion (Tạo hình dẻo bằng pp ép đùn)
 Usually for forming tile and brick products
1 1-thân máy
2 4
3
2-trục vít
3-đầu nén
4- đầu tạo hình
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 Dies for tile and brick products:
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Advantages:
• Hollow shapes and small diameters;
• high production rate.
Limitations:
• Parts have constant cross section;
• limited thickness.
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2.5.3. POWDER PRESSING / COMPRESSION /

COMPACTION (Phương pháp nén / ép bột)
 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
 Biaxial compression - compacted in double
directions
 Isostatic (hydrostatic) compression - pressure
applied by fluid - powder in rubber envelope
 Hot pressing - pressure + heat

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2.5.3. POWDER PRESSING / COMPRESSION /

COMPACTION (Phương pháp nén / ép bột)
 Advantages:
 Close tolerances;
 High production rate with automation.
 Limitations:
 Density variation in parts with high length-to-diameter
ratios;
 Dies require high abrasive-wear resistance;
 Equipment can be costly.
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2.5.3. POWDER PRESSING

(Phương pháp nén / ép bột)
Uniaxial pressing Biaxial pressing

(Ép 1 phía) (Ép 2 phía)
Hot pressing Isostatic pressing Hot isostatic pressing

(Ép nóng) (Ép đẳng tĩnh) (Ép nóng đẳng tĩnh) 89
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Uniaxial vs. biaxial powder compaction
Oberacker, Rainer. “1. Powder Compaction by Dry Pressing.” (2012).
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Cold isostatic pressing
The powder is enclosed in a Schematic diagram of cold
flexible container (rubber). isostatic pressing, as
Pressure is applied isostatically applied to forming a tube.
•Pressure: 400MPa ( up to 1000MPa)
to the assembly inside a high-
pressure chamber.
Source: R.M. German, Powder Metallurgy Science.

Princeton, NJ; Metal Powder Industries Federation, 1984. 94
94

Cold isostatic pressing
 Advantages:
• Uniform density distribution.
• Limitations:
• Equipment can be costly.
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Pressing machines
Máy ép thủ công Máy ép gạch tự động

(A cold isostatic pressing machine)
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Hot isostatic pressing
compaction +
sintering
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 Advantages:
• Strong, high-density parts.
• Uniform density distribution.
• Limitations:
• Protective atmospheres required;
• die life can be short.
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Figure 11.12 Schematic illustration of hot isostatic pressing.

The pressure and temperature variation vs. time are shown in the diagram.
Source: R.M. German, Powder Metallurgy Science, Princeton, NJ; Metal Powder Industries
Federation, 1984.
•Common condition: 100MPa at 1100oC: 100% density, good metallurgical

bonding, good mechanical properties
•Relatively expensive → superalloy components
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Characteristics of Ceramic forming Process
Process Advantages Limitations
Slip casting Large parts, complex shapes; low Low production rate; limited dimensional
equipment cost. accuracy.
Extrusion Hollow shapes and small Parts have constant cross section; limited
diameters; high production rate. thickness.
Dry pressing Close tolerances; high production Density variation in parts with high
rate with automation. length-to-diameter ratios; dies require
high abrasive-wear resistance; equipment
can be costly.
Wet pressing Complex shapes; high production Part size limited; limited dimensional
rate. accuracy; tooling costs can be high.
Hot pressing Strong, high-density parts. Protective atmospheres required; die life
can be short.
Isostatic Uniform density distribution. Equipment can be costly.
pressing
Jiggering High production rate with Limited to axisymmetric parts; limited
automation; low tooling cost. dimensional accuracy.
Injection Complex shapes; high production Tooling can be costly.
molding rate.
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materials
Casting
• Plastic forming
• Shrinkage
Green body
• Sintering

Final
sintered
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2.6. DRYING
 Drying: as water is removed - interparticle spacings
decrease – shrinkage
wet body partially dry completely dry

 The most common effect of drying (by hot air convection)
can be described by the sequence:
 Transfer of heat from air to piece
 Transformation of water from liquid to vapour
 Removal of vapour from surface of piece
 Transport of liquid water from piece interior to surface
 Drying too fast causes sample to warp or crack due to
non-uniform shrinkage 103
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2.6. DRYING
©2003 Brooks/Cole, a division of Thomson Learning, Inc. Thomson Learning is a trademark used herein under license.
Dimensional changes stop

after the interparticle water
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is gone.
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2.6. DRYING
Natural drying
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2.6. DRYING
Sacmi horizontal drier for ceramic tile
Hot air from the cooling area of the kiln can be used to
lower specific temperature consumption.
https://www.sacmi.it/SacmiCorporate/media/ceramics/Catalogues/HORIZONTAL-DRYERS-Sacmi-
Forni-(EN-IT-ES).pdf 107
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2.6. DRYING
Sacmi chamber drier for sanitaryware
https://www.sacmi.com/de-de/ceramics/sanitaryware/Drying 108
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2.6. DRYING
Kỹ thuật sấy ẩm sứ vệ sinh
Löôïng nöôùc Löôïng nöôùc Löôïng nöôùc
A A A
Tâm mẫu
bề mặt
B B B
Thôøi gian Thôøi gian Thôøi gian
a Sấy ở nhiệt độ thấp b) Sấy ở nhiệt độ thấp c) Sấy ở nhiệt độ tăng

và độ ẩm không khí cao và độ ẩm không khí thấp và độ ẩm không khí cao
Khi chênh lệch độ ẩm bề mặt và độ ẩm tại tâm mẫu là nhỏ nhất: quá trình
sấy nhanh nhất.
Các sp sứ vệ sinh có hình dạng phức tạp thường được sấy theo
phương pháp sấy ẩm:
1. Mẫu được làm nóng nhanh trong môi trường ẩm, chưa xảy ra quá
trình sấy: tạo cân bằng độ ẩm trong mẫu và môi trường, đồng thời làm
giảm độ nhớt của nước.
2. Giảm độ ẩm môi trường: quá trình sấy xảy ra, nước có thể bay hơi
đồng đều với tốc độ lớn nhất mà không làm nứt vỡ sp. 109
109
110
110
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materials
Casting
• Plastic forming
• Shrinkage
Green body
• Sintering

Final
sintered
111
111
2.7.1. SINTERING (quá trình kết khối)

Definitions
Sintering: is a processing technique used to
produce density-controlled materials and
components from metal or/and ceramic powders
by applying thermal energy.
(Sintering: removal of pores between particles
accompanied by shrinkage (densification) and
grain growth)
Basically, sintering processes can be divided into
two types:
 Solid state sintering
 Liquid phase sintering
Suk-Joong L. Kang, Sintering: Densification, Grain Growth and Microstructure. Butterworth-Heinemann, 2004
112
112
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2.7.1. SINTERING
Types of sintering (các dạng kết khối)
 Sintering: removal of pores between particles
accompanied by shrinkage (densification) and
grain growth.
Types of sintering
Solid-state sintering (SSS)
only in high-purity compounds
Liquid phase sintering (LPS)
<20% liquid; impurities or specific
additives
Viscous glass sintering or viscous
flow (VGS)
Densification of glass powders
Viscous composite sintering or
vitrification (VCS) >20% liquid:
whitewares, porcelains. cement
(GLASS)
113
113
2.7.1. SINTERING
Stages of sintering (các giai đoạn kết khối)
-- Powder particles coalesce and reduction of pore size
Aluminum oxide powder:

-- sintered at 1700ºC
for 6 minutes.
15 m
W. D. Callister and D. G. Rethwisch, Materials Science and Engineering: An Introduction, 9th ed. 115
John Wiley & Sons, Inc., 2013.
115
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2.7.1. SINTERING
Material transport mechanisms during sintering
Suk-Joong L. Kang, Sintering: Densification, Grain Growth and Microstructure. Butterworth-

117
Heinemann, 2004
117
2.7.1. SINTERING
Driving force (Động lực)
 Driving force for sintering: is the reduction in surface
free energy of the consolidated mass of particles. High
energy solid-gas surfaces are replaced by low energy
solid-solid interfaces (grain boundaries).
 At microscopic level, the driving force is related to the
difference in surface curvature and consequently of
partial pressure and chemical potential between different
parts of the system.
Neck formation Pore removal

and shrinkage
Effect of particle size: the smaller the particles, the higher the radius of curvature and the
chemical potential → higher sintering rate.
118
118
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Hình biểu diễn sự phân bố lỗ trống và các nguyên

tử ở trạng thái hơi ở bề mặt cong của hạt
Suk-Joong L Kang (2005), Sintering, p17
119
2.7.1. SINTERING
Characteristics of Sintered Ceramics
 Typically, ceramics with a small grain size are stronger
than coarse-grained ceramics. Finer grain sizes help
reduce stresses that develop at grain boundaries due to
anisotropic expansion and contraction.
 Apparent porosity - The percentage of a ceramic body
that is composed of interconnected porosity.
 True porosity - The percentage of a ceramic body that is
composed of both closed and interconnected porosity.
 Bulk density - The mass of a ceramic body per unit
volume, including closed and interconnected porosity.
 Apparent density
 True density
 Specific density 120
120
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2.7.1. SINTERING
SEM of sintered Al2O3 specimens
Which specimen is good?
121
2.7.1. SINTERING
Comparison of solid-phase sintering and
liquid-phase sintering
Flux lowers
sintering temperature
M. N. Rahaman, Ceramic Processing and Sintering. CRC Press, 2003. (p622)
122
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2.7.1. SINTERING
Density change of porcelain during sintering
©2003 Brooks/Cole, a division of Thomson Learning, Inc.

During firing, clay and other fluxing materials react with coarser
particles to produce a glassy bond and reduce porosity.
The density is further increased and the mechanical strength is
enhanced. 123
123
2.7.1. SINTERING
SEM of of a fired porcelain specimen
Glassy (rim) phase Glassy (rim) phase
(vòng nhẫn silic) (vòng nhẫn silic) Quartz grain
Pore
Pore
Vitrification (quá
trình thủy tinh
Quartz grain hóa): liquid glass
forms from clay
and flux – flows
between SiO2
Crack in particles.
quartz grain
Pore
Mullite needles
[3 main raw materials: clay, feldspar, sand (SiO2 quartz)]
W. D. Callister and D. G. Rethwisch, Materials Science and Engineering: An Introduction, 9th Edition. 2013.124
124
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2.7.1. SINTERING
Sintering aims (mục đích kết khối)
 Sintering aims, in general, to produce sintered parts
with consistent and, if possible, designed microstructure
through control of sintering variables.
 Microstructural control means the control of grain size,

sintered density, and size and distribution of other phases
including pores.
 In most cases, the final goal of microstructural control is

to prepare a fully dense body with a fine grain structure.
Suk-Joong L. Kang, Sintering: Densification, Grain Growth and Microstructure. Butterworth-Heinemann, 2004
125
125
2.7.2 FIRING (NUNG)
 After drying, the green ceramic is placed in the kilns

when they are cold and is then heated up on a
predetermined time-temperature schedule to a
selected maximum temperature. The firing
temperature (900-1400ºC…) depends on the
composition and desired properties of the finished
piece.
 This temperature is usually held for a certain period
(up to 3 hours) called the soak.
 After the soak, the heat source can be reduced or
shut off, and the ware allowed to cool in the furnace
until it is cool enough to be removed.
126
126
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2.7.2 FIRING (NUNG)

A typical firing curve of traditional ceramic
S. Ferrer, A. Mezquita, M. P. Gomez-Tena, C. Machi, and E. Monfort, “Estimation of the heat of reaction
in traditional ceramic compositions,” Applied Clay Science, vol. 108, pp. 28–39, May 2015, doi:
127
10.1016/j.clay.2015.02.019.
127
2.7.2 FIRING (NUNG)

Firing conditions (các điều kiện nung)
 The maximum rate of temperature change that
ceramic ware can withstand depends on the shape
of the ware and the mechanical strength of the body.
 Fast firing:
 Tile: tfiring ≥ 30 minutes, and tfiring = 45 minutes is
common.
 Tableware (the shapes are diverse and sometimes
more fragile): six hours.
 Sanitary ware (larger shapes): 12 to 15 hours.
 A single-fire process is lower in cost.
 A two-fire process is easier to control for consistent
high-quality ware free of defects.
128
128
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2.7.2 FIRING (NUNG)

Ex: Porcelain
 Production:
- mixture of 3 materials
- forming by hand
(spinning slice) or by
machines (pressure)
- first firing (850 – 950 °C), cool down (slow)
- second firing (1300 – 1410 °C)
- glaze applied
- painting + glaze
- third firing (780 – 1410 °C, depending on
glaze)
129
129
2.7.2 FIRING (NUNG) 1

Kiln (lò)
 A structure built to fire raw
materials at high temperatures.
 An oven or furnace that is used
for hardening, burning, or drying
something (such as pottery) 2
3 4 5
130
130
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2.7.2 FIRING (NUNG)

Kiln (lò)
 The kilns used for firing ceramics come in two basic
types:
 Intermittent or periodic kilns,
 continuous or tunnel kilns.
 Kilns can be electric, gas, oil, coal or wood / rice
hush-fired.
131
131
2.7.2 FIRING (NUNG)

Intermittent or periodic kilns (lò gián đoạn)
Shuttle kiln
(NABERTHERM NW 660/H) 132
132
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2.7.2 FIRING (NUNG)

Continuous kiln (Lò liên tục)
133
133
2.7.2 FIRING (NUNG)

Tunel kiln (lò đường hầm)
Roller kiln
(Lò tunel con lăn) Lò tunel xe goòng
134
134
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2.7.2 FIRING (NUNG)

Roller kiln (the cross-section) (lò con lăn)
2 3
5
3
4 1
2
SACMI IMOLA s.c. a r.l. - 2005 - Applied ceramic technology- Volume 2

135
135
2.7.2 FIRING (NUNG)

Methods of loading the material in the kiln
❖ Xếp trực tiếp vật liệu ❖ Dùng giá, khung, ❖ Xếp trong bao nung
nung vào lò tấm kê, cột chống (hộp)
136
136
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2.7.2 FIRING (NUNG)

Advantage of kilns
Intermittent kilns Continuous kilns
 Lower capital cost  Lower fuel consumption
 Take up much less floor  lower maintenance costs
space  In the well-designed
 Flexibility: in operating, in conditions, the quality of
scheduling ware will generally be
somewhat better.
137
137
138
138
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materials
Casting • Plastic forming
• Shrinkage
Green body • Glazing (coating)
• Sintering
Final
sintered
139
139
2.8.1. CERAMIC GLAZE (MEN GỐM)

140
Overview
 Glazes are the ceramic coatings done on ceramics,
and enamels are done on metals.
 In a given application, a ceramic coating may render
the substrate (or the body) impervious, mechanically
stronger, more resistant to abrasion and scratching,
chemically more inert, more readily cleanable, and
aesthetically pleasing.
 Glazes and enamels are formed by melting and
solidification. The composition of these coatings is
similar to that of glass.
 Almost all vitreous coatings are expected to be
homogeneous, smooth, and hard.
140
140
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141
Overview
 These coatings are usuaIly silicate glasses that may
or may not include dispersed crystals or bubbles.
 As a glaze is fired, its structure changes
continuously:
 Materials initially present decompose and fuse.
 Bubbles are formed and rise to the surface, and
reactions take place with the body under the glaze.
 The interface between the glaze and body is rough
because of the differences in solubility in the body
constituents.
141
141

142
Glaze classification
1. According to phase composition:
 Vitreous glaze (1 pha thủy tinh)
 Crystalline glaze (Men có pha tinh thể kết tinh từ pha thủy tinh)
2. According to chemical composition:
 Lead / leadless glaze,…
3. According to manufacturing method:
 Raw glaze (Men sống hoặc men nguyên liệu)
 Fritted glaze (Men chín hoặc men frit)
 Self-forming glaze (Men tự tạo)
4. According to visual perception:
 Gloss glaze (men bóng), matte glaze (men mờ)
 Transparent glaze (trong), translucent glaze (trong mờ), opaque
glaze (đục)
 …
142
142
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143
Types of glaze
Reticulation glaze Cluster glaze

Glossy glaze
Matte glaze Crystalline glaze Ceramic enamel

143
143

Properties of glaze
 Liquid state (at high temperature)

 Viscosity,
 Surface tension
 Solid state:
 Adherence, thermal expansion
 Hardness
 Chemical durability, optical properties…
144
144
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145
Properties of glaze
The surface tension (Sức căng bề mặt)
 The surface tension of the melting glaze depends on
the composition and temperature.
 When the temperature increases, the surface
tension decreases very quickly.
 When softening or completely melting, the change
rate of surface tension will decrease.
 The coating must have a low surface tension, so it
will spread uniformly over the substrate, and not
crawl away from edges and holes.
145
145

146
Properties of glaze
Thermal expansion (giãn nở nhiệt)
 On cooling the fired ware, the whole coated substrate
contracts.
 If the coefficients of thermal expansion (CTE) of coating
and substrate (body) are not close enough, stresses and
strains lead to spalling or crazing. The thermal expansions
should be close, but not identical.
 Ceramic coatings are much stronger in compression than
in tension. Therefore, the coating is intentionally put in
compression by putting it on a substrate that has a
somewhat higher coefficient of expansion. During cooling,
the coating shrinks less and is put in compression.
R. A. Eppler and D. R. Eppler, Glazes and Glass Coatings. American Ceramic Society, 2000. 146
146
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149
Some glaze defects
Crazing (Rạn men) Peeling /Shivering Crawling (men bị co)

CTE of glaze is too (bong men) high index of surface tension
high CTE of glaze is too low in the melting glaze.
“It is especially true in the ceramics world that one person’s fault is another
person’s fancy–especially when it comes to glaze defects. Many ceramic artists
deliberately create faults in their glaze surfaces to achieve a particular aesthetic.”
https://ceramicartsnetwork.org/daily/ceramic-glaze-recipes/glaze-chemistry/how-to-fix-five-common-
149
ceramic-glaze-defects/
149
2.8.1. GLAZE (MEN)

155
The interface between the glaze and body
0,1 – 0,2 mm
Glaze (men)
Interface (bm chung

/lớp trung gian)
Fired body (xương gốm)
Green body (Unfired body: “mộc”) 155
155
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2.8.1. GLAZE (MEN)

The intermediate layer (engobe) for fast-fired tiles
157
 Với các sản phẩm ốp lát,
theo công nghệ nung nhanh
một lần: đường ranh giới
giữa xương-men thể hiện rõ
nét, không thấy những dấu
hiệu của phản ứng.
 Do lớp trung gian khó hình
thành, vì vậy thường phải
dùng lớp men lót (engobe)
tạo lớp thành phần biến đổi Đồng thời, engobe là lớp nền
trung gian nhằm tăng độ che phủ phần xương “xấu”,
bền liên kết cho xương và giúp các lớp men trang trí
men. phía trên dễ dàng hơn
157
157

158
Porcelain enamels (men tráng kim loại)
 Porcelain enamels on metal are similar to glazes in
that they are basically a silicate glass coating.
 They are normally fired for shorter periods and at
lower temperatures, and a wide range of defects is
common.
 A ground coat containing nickel or cobalt oxide or a
nickel dip (of the metal in a nickel sulfate solution) is
frequently used to improve adherence (to cause
galvanic corrosion of the base metal; certain grains
corrode more rapidly than others, providing a rough
interface and improved adherence).
158
158
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159
Porcelain enamels (men tráng kim loại)
 An enamel coating is commonly made of a bilayer.
 Recently, single-layer enameling has become more
popular, because of the decreased number of
applications and firings required during fabrication.
Therefore, single-layer enamels must be defect-free in
order to provide chemical durability and adhesion
strength at the same time.
J. Cha, J. Kim, J. Shin, and B. Ryu,

“Effect of Nano-NiO Additive on
Adhesion Strength and Bubble Structure
of Vitreous Enamels,” J. Korean Phys.
Soc., vol. 72, no. 7, pp. 770–774, Apr.
2018,
159
159
2.8.2. COLOR OF GLAZE

163
Scattering is caused by light

falling on small particles with
refractive indices different
from that of the surrounding
material, as, for example,
small particles of a pigment
dispersed in a glaze.
163
163
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conventional pigment
(absorption pigment) metal effect pigment
natural pearl pearl luster pigment
F. Shi, Ceramic Coatings: Applications in Engineering. BoD – Books on Demand, 2012, pp. 238. 165
165

Conventional pigments (absorption pigments)
Three methods to obtain color in a vitreous matrix:
1. Certain transition metal ions can be added directly
to the coating formulation (become part of the
glassy coating).
2. Induce the precipitation of a crystal (widely used for
opacification / white color).
3. Disperse in that matrix an insoluble crystal or
crystals that are colored (most commonly used due
to the greater stability).
166
166
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168
168

170
Một số tinh thể thường làm chất mang màu:
 Spinel type 1 (MgO.Al2O3)
 Spinel type 2 (2ZnO.TiO2)
 Zircon (ZrO2.SiO2)
 Baddleyite (ZrO2)
 Granate (2CaO.Al2O3.3SiO2)
 Corundum (Al2O3)
 Willemite (2ZnO.SiO2)
 Perovskite (CaO.TiO2)
 Mulite (3Al2O3.2SiO2)
 Olivine (CoO.SiO2).
170
170
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171
CIE L*a*b* color space
Diagram showing colors obtained from

the major traditional ceramic pigments.
R. A. Eppler and D. R. Eppler, Glazes and Glass

Coatings. American Ceramic Society, 2000, pp. 278.
171
171

Inorganic effect pigments
172
F. Shi, Ceramic Coatings: Applications in Engineering. BoD – Books on Demand, 2012, pp. 239.
172
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2.8.3. APPLICATION TECHNIQUES
173
173

Waterfall / bell / curtain (xối)
Waterfall
Units
(Bell units)
174
174
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Dipping (nhúng)
175
175

Dipping (nhúng)
Automatic glazing systems for ceramic tableware
https://www.sacmi.it/en-US/ceramics/tableware/Glazing
176
176
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Painting (quét / vẽ)
177
177

Spraying (phun)
178
178
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Silk-screen printing
Screen printing machine of SACMI
http://www.sacmiiberica.com/en-
US/Products/Ceramics/3rd-firing/Screen-
printing/Screen-printing-
machines.aspx?idC=62394&LN=en-US 179
179

Digital printing
DHD digital printer of SACMI
http://www.sacminanhai.com/en-US/Products/Ceramics---Tiles/Group-Production-for-China/Wet-
Decoration-and-Glazing/COLORA-HD-Digital-Printer.aspx?idc=65442&ln=en-US 180
180
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Ex:
How Staub Ceramic Cookware is Made
 https://www.youtube.com/watch?v=lbYEE0OqCGs
181
181
182
182
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2.9. INTRODUCTION SOME ADVANCED CERAMICS

Bioceramics
 Biomaterials are employed in components
implanted into the human body to replace diseased
or damaged body parts.
 These materials must not produce toxic
substances and must be compatible with body
tissues (i.e., must not cause adverse biological
reactions).
 All of materials — metals, ceramics, polymers,
composites, and semiconductors — may be used as
biomaterials.
W. D. Callister and D. G. Rethwisch, Materials Science and Engineering: An Introduction,

9th Edition: Ninth Edition. 2013, pp 12. 183
183

Bioceramics
• Apatite hydroxide
Ca10(PO4)6(OH)2, alumina
(Al2O3) and zirconia (ZrO2),
these products take the
HIP JOINT advantage of the new
ceramic's strength and
capability with the human
body.
Acrylic teeth Porcelain teeth
Glass ceramics
Porcelain and metals crowns and bridges
184
crowns and bridges
184
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Sensors
• Ex: Oxygen sensor: ZrO2 Ca2+
• Principle: Make diffusion of ions
fast for rapid response.
• Approach: A Ca2+ impurity
Add Ca impurity to: removes a Zr 4+ and aO2 - ion.
--increase O2- vacancies
--increase O2- diffusion
sensor
• Operation:
gas with an reference
--voltage difference unknown, higher gas at fixed
produced when oxygen content O2-
oxygen content
diffus
O2- ions diffuse ion
between external
and references + -
voltage difference produced!
gases.
185
185

Space Shuttle Ceramic Tiles
• Silica-based insulation material
and similar materials were used
to manufacture heat-resistant
tiles and other coverings to
protect the Orbiter's airframe.
• After the Orbiter has landed and

been taken indoors for inspection,
any damaged tiles are removed and
replaced for the next flight.
“Space Shuttle Tiles.”

https://depts.washington.edu/matseed/mse_resources/Webpage/Space%20Shuttle%20Tiles/Space 186
%20Shuttle%20Tiles.htm (accessed Apr. 07, 2020).
186
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Ceramics for automobile engines
 Advantages: • Disadvantages:
 Operate at high – Ceramic materials are
temperatures – high brittle
efficiencies – Difficult to remove
 Low frictional losses internal voids (that
 Operate without a cooling weaken structures)
system – Ceramic parts are
 Lower weights than difficult to form and
current engines machine
• Potential candidate materials: Si3N4, SiC, & ZrO2

• Possible engine parts: engine block & piston coatings
189
189

Ex:
Sử dụng ceramic trong các động cơ kiểu pittông có khả năng
cải thiện các tính chất và giảm giá thành
Thành phần Zirconia được

sử dụng làm xi lanh nhiên
liệu của động cơ
Cummins
Si3N4 cam roller followers are
used in Detroit Diesel
Corporation (DDC)
engines
Si3N4 valves are being
developed for
reciprocating
190
190
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Ex:
Xi lanh nhiên liệu chiu áp suất cao bằng Zirconia ceramics
trong động cơ diesel làm giảm tổn thất và tăng độ tin cậy
• Excellent wear and

corrosion
resistance keeps
injectors from
sticking
• Injectors operate at
20,000-35,000 psi –
thus very tight
tolerances required
to accurately meter
fuel
191
191

Ex:
Light-weight valves are being developed for NG recips

to improve corrosion resistance at high temperatures
and reduce emissions
Reduced mass of
TiAl Si3N4
Si3N4 valves
Valves Valves
are more responsive
to engine control
Exhaust Intake
Original Steel Valves

192
192
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Ex:
Si3N4 bearings are used in DE applications from 100 kW
microturbines to 1.5 MW wind turbines
Longer life
Lower friction
70% stiffer
60% lighter
2” diameter ball bearings
193
193

Ex:
Si3N4 components are being developed to increase turbine inlet
temperatures and to increase efficiency to near 40%
Si3N4 turbine rotors and vane

194
194
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Ceramic armor (Vỏ giáp)
 Ceramic armor systems are Ceramic-
Outer hard Discontinuous
used to protect military skin
personnel and equipment. Projectile
 Advantage: low density of the Personnel

ceramic can lead to weight- and
Equipment
efficient armor systems.
 Typical ceramic materials used Inner
ductile
skin
in armor systems include
alumina Al2O3, boron carbide, Ceramic Armor System
silicon carbide, and titanium
•The ceramic material is discontinuous
diboride. and is sandwiched between a more
ductile outer and inner skin.
D. B. Rahbek and B. B. Johnsen,
“Dynamic behaviour of ceramic armour systems,”
•The outer skin must be hard enough to
Norwegian Defence Research Establishment (FFI), shatter the projectile.
2015. 195
195
CLIP: ceramic manufacturing process

 Đồ gốm truyền thống (4 ph 52 s)
https://youtu.be/LOPLebrAMYo
 Sơ lược quy trình sản xuất gốm y sinh (Advanced
ceramics của BIOLOX) (7 ph 30 s)
https://youtu.be/DXnlbpaRk4s
 Giới thiệu các sản phẩm gốm kỹ thuật (Advanced
Engineering Ceramics của International Syalons) (2
ph 20 s)
https://youtu.be/zhJhj8J4m9I
196
196
82
16-Jan-24
CLIP: ceramic manufacturing process

 Table wares (China)
https://www.youtube.com/watch?v=7CDxt028co0
 How TILES are Made
https://www.youtube.com/watch?v=8hw4SrG0Zuc&fea
ture=share&fbclid=IwAR0q51awTe-
wryO7wfjqLwBucplpoTJU_8bjbnjH7vn4OGRT6rBwRI
OJlO GOOD
https://www.youtube.com/watch?v=bk24Y83LBrY
197
197
Silicate glasses
Nhớ xem các clip về quy trình

sản xuất được giới thiệu !
THANK YOU 198
198
83

Chap 2-Ceramic Technology

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Chap 2-Ceramic Technology

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16-Jan-24

Course instructor: HUỲNH NGỌC MINH

2.7.2 Briefly describe/diagram the sintering process

2.7.3 Know various stages of firing and various

2.8.2 Note the desirable properties of glaze

2.8.3 Know various glaze coating methods

2.8.4 Note three conventional pigments used in

2.9 Introduction some advanced ceramics

1.4. TYPES AND APPLICATIONS OF CERAMICS

FUNCTIONAL CLASSIFICATION OF CERAMICS

TYPES OF CERAMIC MATERIAL

2.1.1. TRADITIONAL CERAMICS

Gốm sứ VL chịu lửa VL mài Thủy tinh Xi măng Ceramic tiên

Based on mineral silicates, silica, and mineral oxides found in nature

2.1.1. TRADITIONAL CERAMICS

-stoneware e.g. coffee mug, -bone china e.g. table wares,

earthenware stoneware porcelain bone china

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

2.1.1. TRADITIONAL CERAMICS

Ceramic wash basins

2.1.1. TRADITIONAL CERAMICS

2.1.2. ADVANCED CERAMICS

2.1.2. ADVANCED CERAMICS

Biomaterials Magnetic materials 28

2.1.2. ADVANCED CERAMICS

Published by Japan Fine Ceramics Association

2.1.2. ADVANCED CERAMICS

2.1.2. ADVANCED CERAMICS

2.1.2. ADVANCED CERAMICS

2.1.2. ADVANCED CERAMICS

 Natural (garnet, diamond, etc.)

2.1.2. ADVANCED CERAMICS

-Diamond simulants: cubic zirconia, polycrystalline

2.1.2. ADVANCED CERAMICS

 They are usually composed of alumina

 Specialized refractories: BeO, ZrO2, mullite, SiC, and

2.1.2. ADVANCED CERAMICS

Typical steps of ceramics processing

Secondary • Grinding / Cutting / Polishing

Examples of ceramic tiles

Different techniques for processing of

©2003 Brooks/Cole, a division of Thomson Learning, Inc. 41

Making powder-metallurgy parts

COMPARISON OF CONVENTIONAL CERAMICS

Mechanical properties of selected

Typical steps of ceramics processing

Secondary • Grinding / Cutting / Polishing

2.3. RAW MATERIALS USED IN TRADITIONAL CERAMIC

 Mineral silicates (khoáng silicate), such as clays (đất

2.3. RAW MATERIALS USED IN TRADITIONAL CERAMIC

2.3. RAW MATERIALS USED IN TRADITIONAL CERAMIC

2.3. RAW MATERIALS USED IN TRADITIONAL CERAMIC

Cấu trúc của nhóm khoáng smectite (tính dẻo)

Nguồn: R. H. A. Ras, Y. Umemura, C. T. Johnston, A. Yamagishi, and R. A. Schoonheydt,

2.3. RAW MATERIALS USED IN TRADITIONAL CERAMIC

2.3. RAW MATERIALS USED IN TRADITIONAL CERAMIC