Ceramic Powders: Production and Characterization

MM 362
Ceramics and Glasses

Spring Semester 2020, FMCE, GIKI
Lecture 10-15
Instructor:
Muzammil Irshad
Lecturer
1
Ceramic Powders
Why Conventional processing routes of

synthesizing materials do not work for ceramics ?
 High melting points and extreme brittleness.
 Extremely poor ductility and malleability

restricts their formability via processes such as
rolling, low-temperature extrusion, and bending.
 Ceramics processing requires sintering to

achieve full (or controlled) densification without
reaching the melting point of the ceramics.
 A combination of heat and pressure can be

adopted for successful compaction of ceramics.
2
Ceramic Powders
Why we need powders for ceramics ?
 It is a near-net shape forming process

 Close tolerances and good surface finish
 Material wastage is low
 Powders have a high surface energy and curved surface, which is a driving force for
sintering ceramic materials.
 Ceramic powders usually incorporate additives as sintering aids and to inhibit grain
Why starting powder is critically important for the fabrication of ceramics ?

 For improved thermo-mechanical properties
 Reliability as well as reproducible behaviour.
 Strength and fracture toughness strongly dependent on the particle size
 Chemistry of the starting powder
 Sintering parameters
Why fine and spherical particles are preferred in processing of ceramic powders ?
Irregular particles heavy plastic deformation, interlocking and local welding.
Any other reason ?? (better packing, density).
3
Ceramic Powders
 Ceramic powders are generally in the size range 0.5 - 5.0 μm Natural
materials such as clays are mixed mineral powders of this size with water
 Traditional ceramics are made from treated mixtures of clays!

 Engineering ceramic powders are synthesized.
 SiC and Si3N4 are made by reaction e.g. the reduction of sand by coke.
 Many methods are available for the preparation of ceramic powders.

These can be divided into just three basic types:
 Mechanical (series of processes e.g. milling)
 Chemical (exceptional control over particle morphology and Purity )
 Vapor phase (expensive, but offer many advantages)
4
Ceramic Powders
TYPES OF POWDERS
Particles is a general term applied to both primary particles and agglomerates.
Primary particles: smallest clearly identifiable unit in the powder (cannot easily
be broken down into smaller units).
Agglomerates are clusters of bonded primary particles.
Granules are large agglomerates, usually 0.1–1 mm in diameter.
Flocs are clusters of particles in a liquid suspension held together

electrostatically.
Colloids are very fine particles (they can be as small as 1 nm in diameter) held in
fluid suspension (settle very slowly)
Aggregates are coarse constituents, >1 mm, in a Mixture (e.g. addition of gravel
to cement).
5
Ceramic Powders: Powder production (Mechanical methods)
Mechanical Milling:
 It is often necessary to eliminate aggregates and to reduce the

particle size.
 Compound formation during firing and densification during

sintering require diffusion between neighbouring particles.
 Diffusional processes are proportional to the square of the

particle size.
 The minimum particle size possible by ball milling is ∼0.1 μm.

Desirable powder characteristics
Milling media
6
Ceramic Powders: Powder production (Mechanical methods)
Spray Drying:
 Spray drying is an example of powder production

from solution.
 Fine droplets produced by an atomizer are sprayed

into a drying chamber and the powder is collected
The variables in spray drying are:
 Droplet size
 Solution concentration and composition
 Temperature and flow pattern of the air in the drying

chamber
 Chamber design
7
Ceramic Powders: Powder production (chemical methods)
Powders by sol-gel processing:
 The method is used for the

production of metal oxides.
 Hydrolysis of metal salts or

metal oxides with subsequent
coagulation of the product colloids.
 The hydrolysis of metal

alkoxides dissolved in alcohol
leads to condensation reactions.
 Disadvanatage is undesired
atoms, molecules, ions, etc
deteriorates the electrical as well as
optical properties.
 Condensation is a reaction in which two molecules combine to form a larger molecule, producing a
small molecule such as H2O as a by-product, and reverse of that reaction is hydrolysis.
8
Typical reactions in sol-gel processing:
General Reaction:
M(OEt)4 + 2 H2O → MO2 + 4 HOEt
9
Nanopowders by vapor-phase reactions:
 Relatively expensive but they have benefits:
 High purity
 Discrete and nonaggregated particles
 Nanoparticles with narrow size distributions
 Versatility in producing powders of oxides and Nonoxides
 Material is evaporated from the two sources and condenses in the gas phase.
 The condensate is transported by convection to the liquid nitrogen cold finger.
 The clusters are scraped from the cold finger and collected via a funnel.
10
With this technique ceramic powders with very small

particle size have been produced, e.g., TiO2 powders
with an average particle size of 10–15 nm.
Shape, size and the distribution is mainly controlled by

the rate of evaporation (heating rate/temperature), rate
of condensation (cooling rate) and the gas flow.
11
Mechanochemical method:
It refers to the formation of the final product directly during milling

(high-energy milling, used to increase the reactivity of powders)
12
Ceramic Powders: Characterization
 The choice of technique depends on several factors, such as

applicable particle size range, sample size required, and the
analysis time.
Optical microscopy
 Scanning Electron microscope (also TEM)
 Characterization by Light scattering
 X-ray diffraction
The choice of technique depends on several factors:
 Measuring surface area (The bet method)  Type of material
 Amount of material
(Brunauer, Emmett, and Teller (BET) to estimate the particle size  Possible impurities
relies on determining the surface area of the powder)  Amount of impurities
 Availability and cost of instrument
13
Techniques to determining particle Composition and purity
XRF
XRF analyzers determine the chemistry of a sample by measuring
the fluorescent (or secondary) X-ray emitted from a sample when it
is excited by a primary X-ray source.
XRD
used for phase identification of a crystalline material and can
provide information on unit cell dimensions.
NMR
 Nuclear magnetic resonance spectroscopy, most commonly
known as NMR spectroscopy or magnetic resonance spectroscopy,
is a spectroscopic technique to observe local magnetic fields around
atomic nuclei.
 NMR can quantitatively analyze mixtures containing known
compounds.
14
Ceramic Shaping and Forming
Shaping and Forming
 Many shaping methods are used for ceramic products and these
can be grouped into three basic categories:
 Powder compaction: dry pressing, hot pressing, cold isostatic

pressing, etc. (Powder compaction is simply the pressing of a free
flowing powder).
 Casting: using a mold with the ceramic as, or containing, a liquid

or slurry poured into a porous mold.
 Plastic forming: extrusion, injection molding, etc. using pressure

to shape the green ceramic
 Plastic forming consists of mixing the ceramic powder with a
large volume fraction of a liquid to produce a mass that is
deformable (plastic) under pressure.
15
Ceramic Shaping and Forming
Shaping and Forming
 Binder is a component that is added to hold the powder together

while we shape the body (vinyl alcohol, ethylene glycol).
 Slurry is a suspension of ceramic particles in a liquid (As the

amount of water is decreased it becomes more solid.)
 Plasticizer is the component of a binder that keeps it soft or pliable;

it improves the rheological properties.
 Green is a ceramic before it is fired. Brown, white, or gray potter’s

clays are well known green ceramics.
 A transition state between the loose powder and the high-density
sintered product.
 Slip is the liquid-like coating used to form the glaze when fired.
16
Ceramic Powders: Powder production, chemical method
Sol-gel processing:
sol-gel process consists of two steps:
 Formation of sol. and Then the transform of this sol into a

gel.
 Colloidal particles or molecules are suspended in a liquid

or solution, a “sol.”
 The sol is mixed with another liquid, which causes

formation of a continuous three dimensional network, a “gel.”
 Interaction of alkoxides with water yields precipitates of

hydroxides, hydrates, and oxides.
 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.
17
Ceramic Powders: Powder production, chemical method
 Most alkoxides are either liquids or volatile solids

(Sensitive to moisture)
 Metal alkoxides undergo hydrolysis, meaning they react

with Water.
 The hydroxy metal alkoxide product can react by a further

condensation reaction to form polymerizable species
Examples of Metal Alkoxide
18
 Schematic showing condensation reactions in (a) single metal alkoxide solutions and (b) mixed metal alkoxide solutions.
 The sol-gel process can be used to make single or multicomponent oxides. (One component system 43 vol%
Si(OC2H5)4, 43 vol% C2H5OH, and 14 vol% H2O.)
19
Ceramic Powders: Powder production (chemical method)
Drying and Firing
 After gelation, the gel usually consists of a weak skeleton of amorphous material containing an
interconnected network of small liquid-filled pores.
 In most cases we obtain either an aerogel or a xerogel

 Aerogels are highly porous nanostructured materials
 A xerogel is a dry gel.
20
Ceramic Powders: Powder production
Ceramic fibers and whiskers
 Ceramic fibers and whiskers are used in the fabrication of

Composites.
 There are four general methods to produce ceramic fibers:
 From slurry
 By sol-gel processing
 By chemical vapor deposition
 From polymer precursors
What are whiskers and why they have high strength?
 Whiskers are small single crystals a few tens of micrometers

in length with a diameter typically <1μm.
 Absence of crystalline imperfections such as dislocations.
21
Ceramic Powders and Fibre Production
Whiskers from rice hulls:

Ceramic Fibers and whiskers by vapor-phase reactions:
 The rice hulls are heated in an oxygen-free
 Chemical vapor deposition (CVD) often involves atmosphere at 700C.
decomposition of a volatile gas to produce a nonvolatile solid.
 volatile constituents are driven off.
 SiC can be formed by decomposing methyltrichlorosilane,
CH3SiCl3.
 Further heated in an inert or reducing atmosphere
(flowing N2 or NH3 gas) at 1,500–1,600ºC for about 1
h to form SiC.
What is the disadvantage of whiskers over particles?

 In typical CVD, the wafer (substrate) is exposed to one or  Homogeneous dispersion is difficult
more volatile precursors to produce the desired deposit.  whiskers tend to form entwined agglomerates
 Even if well dispersed, some orientation of the
whiskers occurs leading to anisotropic properties.
22
Ceramic Powders: Powder production (Chemical method)
Ceramic Coatings and Films by Sol-gel method:
 Ceramic coatings can be prepared using a sol-gel

process involving metal alkoxides.
 Dipping
 Spinning Applications of Sol-Gel Films and Coatings
 Spraying
 Spinning is widely used for applying sol-gel coatings,

and one particular application is to produce thin coatings
of PZT for microelectromechanical systems (MEMS).
 Sol-gel forms a hard, dense surface that gives a high-

gloss, glass-like finish devoid of surface irregularities.
(Glasses can be synthesized using the sol-gel process.)

23
Ceramic Powders: Powder production (Chemical method)
Ceramic Coatings and Films by Sol-gel method:

 Study of PDMS (polydimethylsiloxane)
sol-gel coated channels.
 In aerospace for the corrosion protection
of Alloys.
 Viscosity controls thickness and uniformity.

 Solvent added to reduce the viscosity.
24
Ceramic Powders: Powder production (synthesis of TiO2 powder), Case study from literature
 In the synthesis of TiO2 particles,Titanium tetra isopropoxidewas used as a precursor

 Mixed with ethanol and deionized water mixture
 Stirred for half an hour
 10ml of deionized water was added to the above mixture
 Stirred for 2 hours at room temperature.
 Finally the solution was dried at temperature and the powder was heated at 120ºC for 1 hour.
 Used in sensor, solar

cells,Biomedical applications.
25
Ceramic Powders: Powder Production
Spray Drying process for powder production:
 Spray-drying is a process by which a fluid feed material is

transformed into a dry powder by spraying the feed into a hot medium.
 The feed materials are either water-based suspensions with air as

drying gas or organic solvent-based suspensions (usually ethanol) with
nitrogen as drying gas.
 Factors to influence the characteristics of spray-dried powders:
 Suspension composition
 Feeding rate
 Drying temperature
 Atomising pressure.
SMD is Sauter median diameter, C a constant whose value depends
on nozzle design ρ,µ,σ, U and m are density, viscosity, surface
tension, velocity and flow rate of the liquid (L) or air (A),
respectively.
26
Spray Drying process for

powder production:
Droplet Air mixing

classifications:
What causes the slurry to

take the shape of small
granules?
Surface tension causes the

airborne slurry to take shape
of small, nearly spherical  Surface tension is the elastic tendency of a fluid surface which makes it acquire the least surface
particles as it dries. area possible.
 It is the attractive force exerted upon the surface molecules of a liquid by the molecules beneath
that tends to draw the surface molecules into the bulk of the liquid
27
A simple mechanism to describe the spray-drying process of ceramics with four steps
(1) droplet formation, (2) evaporation and ballooning, (3) explosion (4) particle formation.
 Preparation of Ce–ZrO2
ceramics powders e.g 6 mol%
CeO2–94 mol% ZrO2 (6Ce–
ZrO2) spray dried and calcined at
500°C.
28
Nanopowders by vapor-phase reactions:  PVD is a process which produces coatings of pure

metals, metallic alloys and ceramics, It involves
 CVD is a process where gaseous precursors react to physically depositing atoms, ions or molecules of a
form a solid coating on a heated substrate. coating species on to a substrate.
Magnetron Sputtering is a Plasma Vapor Deposition (PVD) process in which a plasma is created
and positively charged ions from the plasma are accelerated by an electrical field.
29
 Plasma reactor can also be used to produce ceramic

nanoparticles.
 The gaseous reactants are introduced into an argon

plasma.
 Reactants decomposed into free atoms, ions, and

electrons.
 Quenching of these highly excited species results in

the formation of ultrafine powders with sizes typically
<20 nm.
30
Ceramic Powders: Powder Production (Case Study)
Synthesis of TaC nanopowders by injecting liquid

precursor into RF induction plasma:
 Direct introduction of liquid mist into thermal

plasma e.g. tantalum ethoxide Ta(OC2H5)5.
 Liquid precursor was atomized to generate micron-

sized mist droplets, and the mist was introduced into
plasma.
 Atomized precursor evaporated quickly in the high

temperature plasma flame, and nanoparticles were
formed as temperature decreased.
 yielded average particle sizes as small as 8 nm.
 Synthesized powders were collected in air at the

reactor wall and filter
31
Composite nanoparticles:
 Particles of this type, consisting of a metal-oxide

core and a polymerizable organic shell.
 Synthesized in a microwave plasma reactor by gas

phase synthesis.
 This concept allows the design of new functional

materials with novel or modified magnetic, optical,
electronic or biological properties.
 The components are introduced as gases into

the system just in front of the plasma zone.
 The chemical reaction in the gas-phase and the

nucleation and growth of nanoparticles occurs.
32
Ceramic Powders by precipitation method:
 To cause precipitation, it is necessary to produce a

supersaturated solution.
 At a supersaturation a large number of nuclei form

suddenly.
 Precipitation of mixed oxides is possible.
 The powders produced are not as uniform as those

from the sol–gel process: they often contain hard
agglomerates.
10 Ca(OH)2 + 6 H3PO4 = Ca10(PO4)6(OH)2 + 18 H2O
What is calcination, pyrolysis and rheology ?
33
Direct recation method to synthesise ceramics: Roasting
34
Mechanochemical synthesis using high-energy milling:
 Mechanochemical methods deal with chemical

transformations induced by mechanical energy, such as
compression, shear, or friction (mechanically induced
chemical reaction)
 This process, termed mechanical alloying (formation of

the final product directly during milling)
 Solid state reaction: Chemical process in which one or

more solid reaction products are formed with diffusion of
elementary particles.
 Refinement and desire phase formation are two main

stages in HEBM.
 Critical size is required for mechanical activation and to initiate the reaction
 Mechanical treatment form new surfaces and defects which enhance the reactivity
35
Mechanochemical synthesis of perovskite (e.g. BaTiO3):
Barium Titanate:
Other examples of piezoceramics i.e. PZT, PLZT etc.
36
Dielectric VS Sintering Temperature
Mechanochemical synthesis of PMN–PT ceramics (Lead magnesium
niobate -lead titanate )
 Commercial PbO, MgO, TiO2 and Nb2O5 powders were used as the
starting materials.
 The mixture of the starting oxides, without any additives, was placed in
the vial with the ball-to-powder weight ratio of 20:1.
 The milling speed was set at 200 rpm and milling time was 20 h.
PMN-0.1PT sintered at 1100C for 1hr
 Applications in multilayer capacitors and sensor applications
 Pizoelectric properties are much higher that PZT
 Also can be used as Ferroelectric material
 0.65PMN–0.35PT has a better higher dielectric constant

 Pb(Mg1/3Nb2/3)O3 and 0.65Pb(Mg1/3Nb2/3)O3–0.35PbTiO3
PMN-0.35PT sintered at 1100C for 1hr
37
Synthesis of BF–PT perovskite powders:
 0.7BiFeO3–0.3PbTiO3 (BF–PT) powders were synthesized from a

mixture of the oxides Bi2O3, Fe2O3, PbO and TiO2
 100 g mixed oxides were ball milled for 4 h with stabilized zirconia
balls in alcohol then the mixture was dried and sieved.
 Powders milled for 8 h were calcined from 500 °C to 750 °C to

analyze the structure change with the calcined temperature rising.
Synthesis of KNbO3: (lead free perovskite)

From a equimolar powder mixture of K2CO3 and Nb2O5.
Synthesis of ZrTiO4 by solid state reaction

From equimolar mixture of TiO2 and ZrO2
(Dielectric resonator antenna, DRA, Moisture sensor, temperature
sensor)
38
 Some of the important parameters that have an effect on the

final powder product.
 Type of mill
 Ball-to-powder weight ratio
 Milling container
 Extent of filing the vial
 Milling speed
 Milling atmosphere
 Milling time
 Process control agent
 Type, size of the grinding medium
 Temperature of milling.
39
What is Critical speed:

Speed at which the centrifugal forces
equal to gravitational forces.
40
Effect of speed above CR speed:

Above a critical speed, the balls will be pinned to the inner walls of the vial and do not fall down to exert any
impact force. Maximum speed should be just below critical value (max speed is 55-75% of CR speed).
Disadvantage of maximum speed:

limitation to the maximum speed is that at high speeds ,the temperature of the vial may reach a high value.
Effect of temperature:
Increased temperature accelerates the transformation process and results in the decomposition of supersaturated
solid solutions or other metastable phases formed during milling also amorphisation, (benefit is better diffusion)
Why sometimes annealing is required after milling?

To remove residual stresses, and to improve crystallinity e.g. Annealing of ZrTiO4 at temperature 1100°C, results
in completely crystalline ZrTiO4.
41
What is the effect of Ball to powder ration?
Process can be faster, but a high amount of impurities would introduced due to the wearing of the milling media.
 The rate of amorphization and contamination depend on the ball to powder weight ratio.
 The higher the BPR, the shorter is the time
 Number of collisions per unit time increases and consequently more energy is transferred to the powder particles
Generally about 50% of the vial space is left empty.

What you are expecting if BPR is too high ? (contamination, vial and ball wearing)
Why we need to stop mill on intervals? (1. To cool down system, 2. for sampling for analysis e.g. phase analysis)
42
What is the effect of particle size, distribution on microstructure , sintering and properties
Improved diffusion coefficient, point defect concentration, grain size reduction, distribution of boundary
phases, transport processes at grain boundaries, microstructure uniformity.
What is the effect of wide particle size distribution ?
Microstructure become non uniform. [ https://digitalfire.com/4sight/glossary/glossary_rheology.html ]
43
 The choice of technique depends on several factors, such as

applicable particle size range, sample size required, and the
analysis time.
 Characterization techniques
Optical microscopy The choice of technique depends on several factors:

 Type of material
 Scanning Electron microscope (also TEM)  Amount of material
 Possible impurities
 Characterization by Light scattering  Amount of impurities
 Availability and cost of instrument
 X-ray diffraction, XRF
 Measuring surface area (The bet method)
(Brunauer, Emmett, and Teller (BET) to estimate the particle size

relies on determining the surface area of the powder)
44
Ceramic Powders: Characterization:
Characterizing powders by Sieving:
 Oldest method for determining particle size distribution
 Sorting method and not measuring
 Sieving is the oldest method for determining particle size

distribution (suited for size >56 µm).
45
Characterizing powders by Laser Diffraction

Spectrometry (LDS) :
 Particles pass through a laser beam and the light

scattered by them is collected over a range of angles in the
forward direction.
 The angles of diffraction are, in the simplest case

inversely related to the particle size.
 Distribution of scattered intensity is analysed by

computer to yield the particle size distribution.
 LD is about the relationship between particle size, angle,

and intensity of scattered light.
46
Characterizing powders by light scattering:
 light strikes a particle

 Transmitted
 Absorbed
 Scattered
 Smaller particles scatter a small amount of light through a large

angle.
 Large particles scatter a greater amount of light but through a
smaller angle
 For He-Ne laser with λ = 0.63 µm size range is 2–100 µm
 Light scattering occurs at the edge of an object.
 A SLIT and PARTICLE of the same size produce the same

diffraction pattern. Show schematically.  Small particle  Large Particle
High Scatter Angle Small Scatter Angle
47 Small Signal High Signal
Characterizing powders by Differential Centrifugal Sedimentation (DCS)
 Particle size determined through Stokes Law by measuring the time

required by particles to settle a known distance in a fluid of known viscosity
and density.
 Very small particles (<0.1 μm) do not settle down by gravity unless
extremely dense, so they are not measured by gravitational sedimentation.
 Stokes law accurately measures the diameter of spherical particles based on V is particle settling velocity,
the arrival time at the detector. D is the particle diameter (m),
ρP the particle density (kg/m3),
ρF the fluid density (kg/m3),
 Particles suspended in the fluid, sediment at rates that depend on the G the gravitational acceleration (m/sec2)
following factors: η the fluid viscosity (Pa-s)
1. Gravitational field strength
2. Difference in density
3. Fluid viscosity
4. Particle size
48
Characterizing powders by Brunauer, Emmett, and Teller (BET)
 BET (Brunauer, Emmett and Teller) the specific surface area of a

sample is measured, including the pore size distribution.
Adsorption of gases onto a particle surface at low temperature
P = gas pressure
Po = saturation vapor pressure for adsorbate at the adsorption
temperature
Va = adsorbate volume at relative pressure P/Po
Vm = adsorbate volume per unit mass of solid for monolayer coverage
C = BET constant
 This information is used to predict the dissolution rate, as this

rate is proportional to the specific surface area.
49
Characterizing powders by Differential Scanning Calorimetry (DSC):
 DSC analysis measures the amount of energy absorbed or released by a
sample when it is heated or cooled.
 DSC enables the measurements of the transition such as the glass

transition, melting, and crystallization.
 An empty reference pan sits on a symmetric platform with its own

underlying chromel wafer and chromel-alumel thermocouple. Heat flow is
measured by comparing the difference in temperature across the sample
and the reference chromel wafers.
 Pans of Al, Cu, Au, Pt, alumina, and graphite are available to avoid
reactions with samples and with regard to the temperature range of the
measurement.
 Atmospheres: nitrogen, air, oxygen, argon, vacuum, controlled mixed

gases.
50
Characterizing powders by XRF:
 XRF analyzers determine the chemistry of a sample by

measuring the fluorescent (or secondary) X-ray emitted
from a sample when it is excited by a primary X-ray source.
 Moseley's law is an empirical law concerning the

characteristic x-rays that are emitted by atoms.
 Moseley was able to show that the square root of the

frequency v of a spectral line of the characteristic radiation
of an element is a linear function of its atomic number.
 Powders and pellets, powdered samples are often pressed

where R is the Rydberg constant (R
into pellets, suspensions may also be analysed. =1.0973731568508 ×107per meter), Sn is the
screening constant for the repulsion correction
Partcile size by XRD, (Scherrer equation) due to other electrons, and n is the principal
quantum number.
51
Energy dispersive spectroscopy (EDS or EDX) (used in
conjunction with SEM to determine the chemistry of a sample )
 The surface is exposed to incident electrons that excite the
inner shell electrons in the surface atoms to higher energy
states.
 The energy of the emitted x-ray is characteristic of the atoms

on the surface.
 The emission of x-rays in EDS is more pronounced for the

heavier elements than the lighter elements.
 Practically limited to detection of elements heavier than

beryllium
 Used to analyze surface regions, typically 1 μm across., The

electron beam typically penetrates to a depth of 5 μm
52

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MM 362

Ceramics and Glasses

Why Conventional processing routes of

 High melting points and extreme brittleness.

 Extremely poor ductility and malleability

 Ceramics processing requires sintering to

 A combination of heat and pressure can be

 It is a near-net shape forming process

Why starting powder is critically important for the fabrication of ceramics ?

 Traditional ceramics are made from treated mixtures of clays!

 Many methods are available for the preparation of ceramic powders.

 Mechanical (series of processes e.g. milling)

 Chemical (exceptional control over particle morphology and Purity )

 Vapor phase (expensive, but offer many advantages)

Agglomerates are clusters of bonded primary particles.

Granules are large agglomerates, usually 0.1–1 mm in diameter.

Flocs are clusters of particles in a liquid suspension held together

 It is often necessary to eliminate aggregates and to reduce the

 Compound formation during firing and densification during

 Diffusional processes are proportional to the square of the

 The minimum particle size possible by ball milling is ∼0.1 μm.

 Spray drying is an example of powder production

 Fine droplets produced by an atomizer are sprayed

The variables in spray drying are:

 Solution concentration and composition

 Temperature and flow pattern of the air in the drying

 The method is used for the

 Hydrolysis of metal salts or

 The hydrolysis of metal

 Relatively expensive but they have benefits:

 Discrete and nonaggregated particles

 Nanoparticles with narrow size distributions

 Versatility in producing powders of oxides and Nonoxides

 The condensate is transported by convection to the liquid nitrogen cold finger.

With this technique ceramic powders with very small

Shape, size and the distribution is mainly controlled by

It refers to the formation of the final product directly during milling

 The choice of technique depends on several factors, such as

 Scanning Electron microscope (also TEM)

 Characterization by Light scattering

 Powder compaction: dry pressing, hot pressing, cold isostatic

 Casting: using a mold with the ceramic as, or containing, a liquid

 Plastic forming: extrusion, injection molding, etc. using pressure

Shaping and Forming

 Binder is a component that is added to hold the powder together

 Slurry is a suspension of ceramic particles in a liquid (As the

 Plasticizer is the component of a binder that keeps it soft or pliable;

 Green is a ceramic before it is fired. Brown, white, or gray potter’s

 Formation of sol. and Then the transform of this sol into a

 Colloidal particles or molecules are suspended in a liquid

 The sol is mixed with another liquid, which causes

 Interaction of alkoxides with water yields precipitates of

 Alkoxides have the general formula M(OR)z where M is

 Most alkoxides are either liquids or volatile solids

 Metal alkoxides undergo hydrolysis, meaning they react

 The hydroxy metal alkoxide product can react by a further

Examples of Metal Alkoxide

Drying and Firing

 In most cases we obtain either an aerogel or a xerogel

 Ceramic fibers and whiskers are used in the fabrication of

 There are four general methods to produce ceramic fibers:

What are whiskers and why they have high strength?