CERAMIC INDUSTRY- CH 552

Lesson – 3 (Powder Preparation)

Professor B. S. B. Karunaratne

Ceramic products that use naturally occurring rocks and minerals as a starting
material must undergo special processing in order to control purity, particle size,
particle size distribution, and heterogeneity. Chemically prepared powders also
are used as starting materials for some ceramic products in particular the
advanced ceramics.

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The three main steps involved in the fabrication
of a ceramic body / item

(a) Obtaining un-agglomerated fine powders with a uniform

size distribution.

(b) Shape forming by compaction to obtain crack free green

bodies.

(c) Sintering or firing to obtain a dense body.

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Step (i)-Preparation of Ceramic Powders
• The processing of raw ceramics into ceramic products requires the preparation of ceramic
powders.
• The application and quality of the product( Structural or functional) defines the type of
powder preparation required. Depending on the application, particle size can effect
densification, transport and mechanical properties. The range of particle sizes is broad,
from 100 µm down to several nanometers (nm).

• The raw materials for the powder preparation for traditional ceramics are generally natural
minerals such as Quartz, Zircon, clay. However, for advanced ceramics, much harder raw
materials such as silicon nitride, silicon carbide, alumina, etc. have to be powdered.

• Laser diffraction, dynamic light scattering and acoustic spectroscopy have all been
successfully utilized to characterize ceramic powders.

• The application spectrum of ceramics ranges from household items to heat resistance tiles
for space-shuttle.
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Characteristics of powders
• Chemical composition
• Phase composition
• Particle size
• Particle size distribution
• Particle shape
• Agglomeration
• Surface area
Depending on the method of production, powders
exhibit a diversity of shapes from spherical to
acicular. Particle shape is an important property,
because it influences the surface area of the
powder, its permeability and flow, its density after
compaction and the characteristic of the product
(e.g. Powder particles with sharp edges in a
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grinding wheel performs well).
5
• Products used in ceramic and abrasive applications(grinding wheels, papers,
etc.) are invariably produced from powders. Particle size, particle size
distribution, particle shape have profound effects on processing and
function of these products.
• These materials include most oxides and minerals from aluminum oxide to
zirconium oxide. Depending on the application, particle size can affect
densification, transport(diffusion) and mechanical properties. The range of
particle sizes is broad, from less than 100 nm to greater than 100 µm.
Electronic Ceramics
• Particle size analysis plays a crucial role in the manufacture of electronic
materials for dielectric applications.
• These materials include single-phase powders such as barium titanate as
well as formulations that contain many different oxide phases.
• In all cases, the particle size distribution has a great impact on their
processing and performance. 6
Ceramic powder processing
• Ceramic powder processing can be broadly divided into two main
categories- Chemical and Mechanical.
• In addition some miscellaneous methods are also available.

Chemical Methods
(a) Sol-gel method,
(b) Co-precipitation method
(c) Hydrothermal method
(d) Combustion method
(e) Freeze Drying, etc.
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Sol-gel Process
• Sol-gel Process is transition of
a solution or a sol to a rigid
porous mass or a gel through
destabilization, precipitation or
super-saturation.
• Sol is typically a one phase
solution of water, alcohol and
metal alkoxides. A sol can also
be a suspension or dispersion
e.g. Oxide or hydroxide.
• At the transition a clear sol can
become a rigid two phase gel
containing a solid network with
solvent filled pores.

Precursor: A substance that, following a reaction, becomes an intrinsic part of a product chemical.
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The material must be stable at room temperatures.
 Sol-Gel Method
Sol-gel is a generic term that includes a variety of techniques to achieve a high purity
composition with homogeneity at the molecular level. Preparing a powder by a sol-gel
approach involves the following steps.
1. Form a stable dispersion (sol-solution) from a suitable precursor (particle size about 1
m).
2. By changing concentration(evaporation of the liquid), aging, or addition of a suitable
electrolyte, include a polymer like 3D bonding to form a gel.
3. Evaporate the remaining liquid from the gel.
4. Increase the temperature to convert the dehydrated gel to the ceramic composition.
As shown in the figure above, films by spin coating or dip coatings or fine powered can be
produced. The rigidity of gel prevents migration or segregation of atoms during drying and
assures homogeneity at the molecular level. The resulting powder has high surface area (
about 500 m 2 per gram) and small particle size ( 20-50 nm).
Gel formation is known as gelation. This occurs through the growth and linkage together
polymeric units to form a continues network that extends through the liquid. The
parameters such as solution pH and temperature are important .
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Co-precipitation
• Co-precipitation is a simple, economical
and industrially viable technique that can
be used for the synthesis of
technologically important oxide
materials.
• The steps involved in the process are
shown schematically in the flow chart.
Using this process, it is possible to
prepare flowable powders without any
additional agglomeration steps.
• One can tailor the process to get nano or
micron size particles by adjusting the pH,
the precipitating agent, temperature and
solvents.
• This process has been successfully used
for the preparation of ceramic oxide Schematic diagram of co-precipitation method to synthesize
powders suitable for suspension plasma paramagnetic La Doped Mn-Zn Nano Ferrites a an example
spraying and powder plasma spraying.
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General steps for hydrothermal preparation.
• The hydrothermal method refers to the use of an aqueous solution
as a reaction system in a special closed reaction vessel (autoclave)
to create a high-temperature, high-pressure reaction environment
by heating the reaction system and pressurizing it (or the vapor
pressure generated by itself).
• The process dissolves and recrystallizes a substance that is poorly
soluble or insoluble under normal conditions . The general
preparation steps of the hydrothermal method are shown in the
flow chart.

Schematic of typical hydrothermal method equipment.

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Combustion method

Polymer precursor

Example: Preparation of Li1.2Mn0.4Co0.4O2 composite powder 12

 Freeze Drying
• Freeze drying (also known as cryochemical
processing) is a relatively new process.
• It has potential for producing uniform
particles and crystallites sizing of very pure
homogeneous powder.
• There are 4 steps in freeze drying.

1. A mixture of suitable salts containing the desired ratio metal ions is dissolved in distilled
water.
2. Spray freezing is the next step where the above solution is atomized, sprayed with a
nozzle, into a chamber with liquid nitrogen. The small droplets are then rapidly frozen with a
minimum of ice crystal growth.
3. The frozen material (granules) are then transferred to a freeze dryer where the ice is
removed by sublimation, i e never go through a liquid state that ensure homogeneity
preservation.
4. The resulting powder is then calcined at a temperature that decomposed crystallized
salts and convert them to fine crystallites of the desired oxide or compound. 13
Mechanical preparation methods: Crushing/Milling/Grinding

• Hammer milling, Jaw crushing, roll Hammer Milling

crushing, etc. are used to Break
ceramic ( non plastic) raw materials
into small particles.

• Cone crusher is suitable for silica,

flint talc, etc. Can be obtained even
smaller sizes than that from a jaw
crusher.

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 Mechanical preparation……

Jaw Crusher

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Mechanical preparation……

Roll Crushing

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Mechanical preparation……

Different types of ball mills:

attrition mill, horizontal mill,
planetary mill, and the 1D and
3D vibratory mills.

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Mechanical • Ball milling is one of the most widely used grinding
preparation…… method.

• A ball mill is a machine with a rotating hollow cylinder

partly filled with steel or ceramic balls (milling media).
Ball Milling • Depending on the powder amount and the powder
properties, different types of mills are used for dry and wet
grinding.

• A ball mill consists of a hollow cylindrical shell rotating

about its axis. Less wear takes place in rubber lined mills.
The length of the mill is approximately equal to its
diameter.

• The ball to powder ratio (BPR) is a processing parameter

and is typically about 45 % to 55% of the milling media
(balls).
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Mechanical preparation……

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Ball Milling
• Ball Mill grinds a material by rotating a cylinder with hard balls, causing them to fall back
into the cylinder and onto the material to be ground.
• The impact of balls is important for reduction in size of the particles. Ball milling is mostly
used for brittle materials. The diameter of the mill decides the speed of the mill.
Generally, the rotational speed does not exceed 20 RPM.
• Diameter of cylinder is inversely proportional to the rotational speed. The larger the
diameter, the slower the rotation.
• If the speed is too high, it begins to act like a centrifuge and the balls do not fall back, but
stay on the perimeter of the mill.
• The rate of milling is determined by the relative size of the initial powder, density and
relative hardness of the grinding media and the powder material.
• As mentioned, the milling can be conducted either dry or wet. Dry milling avoids re-
drying the milled powder and avoids reaction of the powder with the liquids used.
Further advantage is less media and lining wear than wet milling.
• In wet milling, some advantages are low energy requirement, less dust problem,
achieving higher rotational speeds, good homogeneity, smaller particles and narrow
particle size distribution than dry milling.
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Correct Rotational Speed – Revolutions Per Minute (RPM)

Slow RPM Correct RPM High RPM

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 Grinding Balls ( and Rods) or milling media

Zirconia Silicon Nitride Alumina Tungsten carbide

Steel balls Sialon short rods and balls Long rods Porcelain balls

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Laboratory ball mills

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 Outer cover Industrial ball mills

Mill liner

Schematic diagram of a ball mill. 24

 High-energy ball milling

High-energy ball milling is a ball milling process in which a powder

mixture placed in a ball mill is subjected to high-energy collisions from
the balls. 25
High Energy Ball Mill • The unique combination of high
friction and impact results in
extremely fine particles ( nm) within
the shortest amount of time.

• With cooling system with water, or

N2 the high energy input is
effectively used for the grinding
process without overheating the
sample.

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Attrition Mills • Attrition milling is similar to a ball mill, but
rather than the cylinder rotating, the very
small balls are agitated by a series of
stirring arms mounted to an axial shaft.
• The horizontal stirring arms provide
excellent grinding performance because it
applies a strong shearing and impact
energy to a material.
• It is suitable as a primary or secondary
grinding machine for materials with large
particle sizes, and it allows even particle
distribution.
• Attrition milling is quicker than ball milling.
This can be conducted dry, wet or with a
vacuum or in an inert gas atmosphere.
• Featuring a variety of safety devices, the
machine minimizes the risk of exposure of
the worker. 27
 Vibratory mill • Vibratory milling is substantially different from
ball milling or attrition milling. The energy for
milling is supplied through vibration rather than
tumbling.
Powder
Vibratory mill • Mill container is packed with milling media rods
material as shown in the figure.
Lid • The powder to be milled is pored into the
container and the lid is closed tightly.
• The powder can move in between the rods.
Vibration • The container is pleased secularly in the vibrating
machine and vibrate it at very high frequency for
Rods about 15-30 minutes.
• Dry or wet milling can be done.
• Vibrating cylindrical rods (milling media) provides
excellent grinding performance because it applies
a strong shearing and impact energy to the
powder particles of the material. 28
Planetary Ball Mills
• The planetary ball mill
performs mixing by continually
revolving the large plate and
rotating the containers
concurrently.

• Both the plate revolution

(centrifugal) speed and
container rotation (planetary)
speed are independently
adjustable.

• This unique mixing capability

allows the operator to design
precise solutions for mixing
various systems.

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 Changes in the material
trapped between colliding
balls in a ball mill.

High-energy ball milling is a mechanical

deformation process that is frequently used for
producing nanocrystalline metals or alloys in
powder form.
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Advantages and Disadvantages of Ceramic Powder Production by Ball
milling
Disadvantages
Advantages • Irregular particles
• Inexpensive • Introduction of defects
• Large scale process • Introduction of impurities from balls and
• Old well-established process milling additives
• Down to 2 –20 nm possible

Contamination is a major problem in ball milling.

Contamination can be controlled by careful
selection of the mill lining and the milling media
(balls). Polyurethane and various types of rubber Mill lining
are excellent wear resistance lining materials. Very
hard grinding media can reduce contamination.
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Miscellaneous methods
• Spray drying is a well-known method of particle
Spray drying production which consists on the transformation of
a fluid material (slurry) into dried particles.

• Slurry preparation is most frequently done in a ball

mill.

• The process may be described by three major

phases atomization, droplet-to-particle conversion
and particle collection as shown.

• Atomized droplets are ejected into a drying gas

chamber where the moisture vaporization occurs,
resulting in the formation of dry particles.

• Finally, using an appropriate device, the dried

particles are separated from the drying medium,
being then collected in a tank. 32
 Miscellaneous methods: Spray pyrolysis
• In spray pyrolysis, the drying process is the same as that in spray drying. However, in spray pyrolysis, after
drying the particles undergo a chemical reaction, and one or more elements, which are usually in gas form,
separate from the original material.
• In conventional spray pyrolysis owing to the high temperature of the surrounding gas, the solute is
decomposed to form final solid particles. Spray drying (SD) is similar to spray pyrolysis, except that there is
no chemical decomposition in SD and usually the process temperature is lower.
• Advanced ceramic powders are prepared by spray pyrolysis. This method enables the production of high-
purity, sub-micron sized particles with a homogeneous chemical composition.

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 Particle Size Analysis
Why we measure particle size and particle size distribution???

• Particle size is the most important parameter in the production

of ceramic products. The particle size must be optimized to ensure that the
desired physical / mechanical properties are achieved.

• Particle size can affect

• Final formulation: performance, appearance, stability.
• “Processability” of the powder. Maintenance of the desired particle size
distribution requires control of the dispersion stability of the ceramic slip.

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 Methods for determining particle size
• Microscopy
• Sieving
• Sedimentation techniques
• Optical and electrical sensing zone method
• Laser light scattering techniques
• Surface area measurement techniques

Choosing a method for particle sizing

• Nature of the material to be sized, e.g. estimated particle size and particle size
range solubility, ease of handling, toxicity, flowability, intended use
• Cost: capital cost and running cost
• Specifications, requirements
• Time restrictions, labour, etc.
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Microscopy
Optical microscopy (1-150 µm)
Being able to examine each particle individually has led
to microscopy being considered as an absolute
measurement of particle size.

• Can distinguish aggregates from single particles

• When coupled to image analysis computers each field Optical microscope image of a
can be examined, and a distribution obtained. representative sample of
alumina powder
• Most severe limitation of optical microscopy is the depth
of focus being about 10 µm at x100 and only 0.5 µm at
x1000.

• With small particles, diffraction effects increase

causing blurring at the edges - determination of particles
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< 3µm is less and less certain.
For submicron particles it is necessary to use either
• TEM (Transmission Electron Microscopy) or
• SEM (Scanning Electron Microscopy).
TEM and SEM (1 nm - 5µm)

TEM image of synthesized glass-ceramic powders.

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SEM image of alumina particles.
 Types of Diameters
• Feret's diameter (F)
• This is the distance between two tangents on
opposite sides of the particle, parallel to some fixed
direction.

• Martin's diameter (M)

The length of the line which bisects the particle
image. The lines may be drawn in any direction
which must be maintained constant for all image
measurements.

• Projected area diameter (da or dp)

This is the diameter of a circle having the same
area as the particle viewed normally to the plane
surface on which the particle is at rest in a stable
position.

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 Types of Diameters
Others:
• Longest dimension:
A measured diameter equal to the
maximum value of Feret's diameter.
• Perimeter diameter:
The diameter of a circle having the same
circumference as the perimeter of the
particle.
• Maximum chord:
A diameter equal to the maximum length
of a line parallel to some fixed direction
and limited by the contour of the particle.
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Manual Optical Microscopy
Advantages
• Relatively inexpensive
• Each particle individually examined - detect aggregates, 2D shape,
colour, etc.
• Permanent record - photograph
• Small sample sizes required
Disadvantages
• Time consuming - high operator fatigue - few particles examined
• Very low output
• No information on 3D shape
• Certain amount of subjectivity associated with sizing - operator bias
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Transmission and Scanning Electron Microscopy
Advantages
• Particles are individually examined
• Visual means to see sub-micron specimens
• Particle shape can be measured

Disadvantages
• Very expensive
• Time consuming sample preparation
• Materials such as emulsions difficult/impossible to prepare
• Low output - Not for routine use

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Automatic and Image Analysis Microscopes
Advantages
• Faster and less operator fatigue than manual
• No operator bias

Disadvantages
• Can be very expensive
• No human judgement retained e.g. to separate out aggregates,
select or reject particles etc. (unlike semi-automatic)

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 Sieve methods
• Equivalent diameter:
• Sieve diameter, ds (the particle dimension that passes through a
square aperture (length = x)).

• In practice sieves can be obtained

for size analysis over a large range
from 5 µm.

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 Sieve analysis
• Sieve analysis is performed using a stack of sieves where each lower
sieve has a smaller aperture size than that of the sieve above it.
• Sieves can be referred to either by their aperture size or by their mesh
size (or sieve number).
• The mesh size is the number of wires per linear inch.
• For example a 16- mesh screen has 16 equally spaced openings per
linear inch.

• Approx. size range : 5 µm - ~ 3 mm and types

• Standard woven wire sieves
• Electroformed micromesh sieves at the lower end or range (< 20µm)
• Punch plate sieves at the upper range.
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Sieve types

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Standard mesh sizes
Particle Size ASTM
US Standerd Sieve
Inches Microns (mesh size )

0.0059 149 100

0.0049 125 120

0.0041 105 140

0.0035 88 170

0.0029 74 200

0.0025 63 230

0.0021 53 270 Question: If the particle size

0.0017 44 325 is 44 µm, what is the mesh
0.0015 38 400
sizes?
0.0010 25 500
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0.0008 20 635
Raw and processed ceramic powders are often supplied according to
mesh size.
• Example: 1. What is a -325 mesh powder?
2. What is a -120 mesh + 200 powder?

• A -325 mesh powder has all passed through 325 mesh screen and
should contain no particle larger than 44 µm.

• A -120 mesh + 200 powder has particles less than 125 µm and
larger than 74 µm.

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48
 Sieve analysis- Procedure
1. Weigh the powder sample to be used, sieves and receiving
pans separately.

2. Stack sieves in order from smallest to largest, starting at

the bottom, with the pan below the smallest sieve.

3. Add the powder sample to the top sieve.

4. Tighten the equipment to ensure that the sieve stack is held

firmly in the shaker assembly.

5. Set the sieve shaker to vibrate for 15 minutes. A shorter

time may be required for brittle materials.

6 Weigh the mass of powder particles in each sieve.

49
Weight of the powder particles stopped W5 W4 W3 W2 W1
by each sieve

50
 Sieve Analysis -test
• This is a procedure used to assess the particle size distribution of a
powder material by allowing the powder to pass through a series of
sieves of progressively smaller mesh size and weighing the amount of
material that is stopped by each sieve as a fraction of the whole weight
(W5+ W4+ W3+ W2+ W1)= W

• fraction retained by each sieve- (W1)/W, (W2)/W, (W3)/W, (W4)/W and

(W5)/W

Cumulative weight fractions by each sieve

(W1) / (W5+ W4+ W3+ W2+ W1),
(W2+ W1) /(W5+ W4+ W3+ W2+ W1),
(W3+ W2+ W1) /(W5+ W4+ W3+ W2+ W1)
(W4+ W3+ W2+ W1) /(W5+ W4+ W3+ W2+ W1),
(W5+ W4+ W3+ W2+ W1)/(W5+ W4+ W3+ W2+ W1) =1 or 100%
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EXAMPLE
Total amount of powder = 1000 (g)

52
• You must plot the cumulative % (or weight fractions) of all the particles in the
bed which have a diameter less than the maximum diameter for each size range.
• In each size range of particles there exists a maximum diameter. What fraction of
the bed has a particle size less than or equal to that diameter?
• The plot should look like the plot below. You must plot the data correctly, or your
entire sieve analysis will be incorrect.

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Other possible distributions can be plotted

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55
 Test for particle size analysis or sieve analysis of aggregates are done to
determine its particle size distribution, fineness modulus, effective size and
uniformity coefficient.
• Sieving may be performed wet or dry; by machine
or by hand, for a fixed time or until powder passes
through the sieve at a constant low rate

Advantages Disadvantages
• Easy to perform • Known problems of reproducibility
• Wide size range • Wear/damage in use or cleaning
• Inexpensive • Irregular/agglomerated particles
• Rod-like particles : overestimate of under-size
• Labour intensive
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 Sedimentation techniques
• Methods depend on the fact that the terminal velocity of a particle in a fluid
increases with size. Recall Stokes law.
• Stokes's Law :  
 s   f gd sph 2

18
18 x
d sph 
 
s   f g t

• Stokes's diameter (dst) is defined as the diameter of the sphere dsph that
would settle at the same rate as the particle.
• s and f are density of solid particle and density of the fluid respectively.
• x/t is the terminal velocity.
57
 Andreasen Pipette method
• Size distribution is determined by allowing a
homogeneous suspension to settle in a cylinder and
taking samples from the settling suspension at a fixed
horizontal level at intervals of time.
• To collect samples a special type of pipette
(Andreasen) having 3 direction cock, is used.
• A syphon tube is immersed into the water to depth of h
below the suspension level.
• The terminal velocity v is calculated from Stokes law
for different sizes of particles, for example 35, 25, 15
and 10 µm.
• Each sample will contain a representative sample of
the suspension, with the exception of particles greater
than a critical size, all of which will have settled below
the level of the sampling point.
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 Andresen Pipette method continued
• The time required for a 10 µm particle to settle from the suspension level to the
bottom of the syphon tube distance h is calculated from v (t = h/v). Similarly, find t
for other particle sizes.
• The suspension is gently stirred to disperse the particles through the whole
volume of water and then allowed to stand for the calculated time.

• The concentration of solid in a sample taken at time t is determined by

centrifugation of the sample followed by drying and weighing or simply by drying
and weighing.

• This concentration expressed as a percentage of the initial concentration gives the

percentage (w/w) of particles whose falling velocities are equal to or less than h/t.
Substitution in the equation above gives the corresponding Stokes' diameter.

• We can represent the findings as a cumulative weight distribution similar to that

expressed in sieve analysis. 59
Advantages
• Equipment required can be relatively simple and inexpensive.
• Can measure a wide range of sizes with considerable accuracy and reproducibility.

Disadvantages
• Sedimentation analyses must be carried out at concentrations which are sufficiently low for
interactive effects between particles to be negligible so that their terminal falling velocities
can be taken as equal to those of isolated particles.

• Large particles create turbulence, are slowed and are recorded undersize.

• Careful temperature control is necessary to suppress convection currents.

• The lower limit of particle size is set by the increasing importance of Brownian motion for
progressively smaller particles.

• Particle re-aggregation during extended measurements.

• Particles have to be completely insoluble in the suspending liquid.

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Laser light diffraction techniques
• This uses the technique of laser diffraction to
measure the particle size and particle size
distribution of materials. It does this by
measuring the intensity of light scattered as a
laser beam passes through a dispersed
particulate sample.
• The angles of diffraction are, in the simplest
case inversely related to the particle size.
• The particles pass through an expanded and
collimated laser beam in front of a lens in
whose focal plane is positioned a
photosensitive detector consisting of a series
of concentric rings.
• Distribution of scattered intensity is analysed
by computer to yield the particle size
distribution.
• Particle size range 20 nm – 2000 µm can be
measured. 61
Advantages:
• Non-intrusive : uses a low power laser beam
• Fast : typically < 3 minutes to take a measurement and analyse.
• Precise and wide range - up to 64 size bands can be displayed covering a
range of up to 1000,000:1 in size.
• Absolute measurement, no calibration is required. The instrument is based on
fundamental physical properties.
• Simple to use.
• Highly versatile.

Disadvantages:
• Expensive.
• Volume measurement all other outputs are numerical transformations of this
basic output form, assuming spherical particles.
• Must be a difference in refractive indices between particles and suspending
medium.
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 Electrical sensing zone method
– Coulter Counter
• Instrument measures the particle volume
which can be expressed as dv : the diameter of
a sphere that has the same volume as the
particle.
• The number and size of particles suspended in
an electrolyte is determined by causing them
to pass through an orifice an either side of
which is immersed an electrode.
• The changes in electric impedance (resistance)
as particles pass through the orifice generate
voltage pulses whose amplitude are
proportional to the volumes of the particles.
• Coulter counters have a wide variety of
applications including blood cells, paint,
ceramics, glass, molten metals and food
manufacturing.
• Volume distribution 63
Optical sensing zone method
• Obscuration of light source relates to particle size
(area)
• Advantage of not requiring medium to be an
electrolyte
• It can also be used to obtain an overall size
distribution, when operated with proper technique.
• The sample must be in a dilute form for analysis. The
technology works by passing a dilute stream of
particles in a liquid suspension between a light
source and a detector.
• The light source in this case is a laser diode, which illuminates the individual particles in
the stream and results in a shadow or blockage of light on the detector.

• This light blockage is termed obscuration. The detector measures this reduction in light
intensity and using a calibration curve, processes the signal to determine the size of the
particle. 64
 Photon Correlation Spectroscopy (PCS) or dynamic light scattering
Intensity
• Large particles move more slowly than small particles,
so that the rate of fluctuation of the light scattered
from them is also slower. time
• PCS uses the rate of change of these light fluctuations
to determine the size distribution of the particles
scattering light. (SPAD -single photon avalanche diode)
• Comparison of a "snap-shot" of each speckle pattern
with another taken at a very short time later
(microseconds). A laser scattered by a sample is analyzed.

• The time dependent change in position of the speckles relates to the change of position of
the particles and hence particle size.
• The dynamic light signal is sampled and correlated with itself at different time intervals
using a digital correlator and associated computer software.
• The relationship of the auto-correlation function obtained to time intervals is processed to
provide estimates of the particle size distribution.
• The Particle size range :1 nm to 5 µm can be measured.
65
Photon Correlation Spectroscopy (PCS) or dynamic light scattering
Advantages:
• Non-intrusive
• Fast
• Nanometre size range

Disadvantages:
• Sample prep critical
• Vibration, temperature fluctuations can
interfere with analysis
• Restricted to solid in liquid or liquid in
liquid samples
• Expensive
• Need to know R.I. values and viscosity

66
 Surface area of Powders
The specific surface area of a powder
• Best described as the external surface
area of a solid object including surface
attributable to pores.
BET-Method
BET stands for Brunauer, Emmett and
Teller
This is the most common method used to
describe specific surface area.
Concept: : Determine the quantity of gas
adsorbed on a clean powder particle
surface to form a mono-layer. 67
 BET-Method
1. Desorb the dry powder under vacuum and weigh it.
2. Pass Nitrogen gas under known pressure and weigh it.
3. Find the mass Wm of Nitrogen required to form a monolayer.

• Total Surface area (St) can then be derived at a given pressure,

N = Avogadro's number (6.023x1023)

M = Molecular weight of Adsorbate (Nitrogen)
Acs = Adsorbate cross sectional area (16.2 Å2 for Nitrogen)

• Specific Surface Area (S) is then determined by total Surface area by sample
weight (w) .

• BET method is a cheap, fast and reliable. 68

It is important to note that different techniques determine an effective diameter of a
powder particle depending on the nature of the detecting method. Typical size
parameters are, for example, breadth, length and diameter of equivalent circle.

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