Powder Characterizations

Characterizations
Physical
Characteristics
Chemical
Composition
Phase
Composition
Surface
Characteristics
1. Particle size and
distribution
2. Particle shape
3. Degree of
agglomeration
4. Surface area
5. Density and
porosity
6. Flow properties
and granulation
1. Major elements
2. Minor elements
3. Trace elements
(AAS, AES, XRF)
Crystal structure and
phase
composition
1. Surface structure
(LEED, STM, AFM)
2. Surface
composition
(AES, XPS, ESCA,
SIMS)

Physical Characterizations of Powder
Types of Particles
Primary particle
Smallest unit in
the powder with
a clearly defined
surface/isolated
porosity
Agglomerates
Cluster of
primary particles
held together by
surface force
Types: Soft and
Hard
Particles
Small units that
move as a
separate entity
(Coarse particle
1-100 m)
Granules
Large
agglomerates
(Dimension 100-
1000 m)
Physical Characterizations of Powder
Types of Particles
Flocs
Cluster of
particles in a
liquid
suspension
Colloids
Finely divided
phase in a fluid
(Brownian
motion, negligible
sedimentation
under normal
gravity (1 nm 1
m)
Aggregates
Coarse
constituent in a
mixture (pebbles
in concrete)
(> 1 mm)
Definition of Particle Size
Stokes diameter Diameter of the sphere calculated from
Stokes law
Projected area diameter projected area of the particle under
microscope
Ferets diameter/Martins diameter Linear dimension
measured parallel to some fixed direction
(Attached sheet)
Physical Characterizations of Powder
Methods for Measurement of Particle Sizes
Method Range (m)
Microscopy
Optical > 1
SEM > 0.1
TEM > 0.001
Sieving 20 10,000
Sedimentation 0.1 100
Coulter counter 0.5 400
Light Scattering
Scattering intensity 0.1 1000
Brownian motion 0.005 1
X-ray line broadening < 0.1
Physical Characterizations of Powder
Martins Diameter (X
M
) - length of a line that
bisects the area of the particle image

Ferets Diameter (X
F
) - distance between two
tangents on opposite sides of the particle,
parallel to some fixed direction

Projected Area Diameter (X
PA
) - diameter of a
circle having the same area as the two-
dimensional image of the particle

Perimeter Diameter (X
C
) - diameter of the circle
having the same circumference as the perimeter
of the particle

The longest dimension is equal to the maximum
value of Ferets diameter


Measurement of Particle Size by Microscopy
Physical Characterizations of Powder
Methods for Measurement of Particle Sizes
Method Range (m)
Microscopy
Optical > 1
SEM > 0.1
TEM > 0.001
Sieving 20 10,000
Sedimentation 0.1 100
Coulter counter 0.5 400
Light Scattering
Scattering intensity 0.1 1000
Brownian motion 0.005 1
X-ray line broadening < 0.1
Physical Characterizations of Powder
Measurement of Particle Size and Size Distribution by Sieving
Mesh size = the number of wires per
linear inch of the sieve screen, which is
the same as the number of square
apertures per inch.

If mesh number = M, aperture width = a,
wire diameter = w, and the open area =
A, then:





w a
M
+
=
1
w
M
a =
1
2
2
2
) (
) (
Ma
w a
a
A =
+
=
Problem: Find out the wire diameter
and open area of a 400 mesh sieve
with an aperture of 38 m?
Physical Characterizations of Powder
Methods for Measurement of Particle Sizes
Method Range (m)
Microscopy
Optical > 1
SEM > 0.1
TEM > 0.001
Sieving 20 10,000
Sedimentation 0.1 100
Coulter counter 0.5 400
Light Scattering
Scattering intensity 0.1 1000
Brownian motion 0.005 1
X-ray line broadening < 0.1
Physical Characterizations of Powder
Measurement of Particle Size and Size Distribution by Sedimentation
Stokess Law,
av F tq 6 =
F = Frictional force
acting on the particle,
q= Liquid viscosity,
a = particle radius
v = terminal velocity
Stokess Equation,
( )
2 / 1
18
(

=
g d d
v
x
L s
q
x = diameter of the
particle with sphere
shape,
d
s
= particle density
d
L
= liquid density
For non spherical particle,
Limitations
1. Holds good for laminar (non-turbulent) flow
2. No inter-particle collision
3. No interactions between the particles
STK
x x =
Laminar to turbulent flow occurs at some critical velocity,
2 . 0 ~ = =
x d
N
v
L
R
c
q
2 . 0 <
q
x vd
L
2 . 0 >
q
x vd
L
N
R
= Reynolds Number
Laminar Flow
Turbulent Flow
The particle size distribution is determined by measuring
the change in concentration (or density) of the suspension as a function
of time, height along the suspension, or both.

A light beam or an x-ray beam is projected at a known height through a
glass cell containing the suspension.

The intensity of the transmitted beam is measured by a photocell or an
x-ray detector located at the opposite side.
The intensity I of the transmitted beam will increase as,
) exp(
0
KACy I I =
I
0
= Intensity of the incident beam
K = Extinction coefficient
A = Projected area per unit mass of the
particle
C = Concentration by mass of the particle
y = Optical path length through the
suspension
The particle size distribution [e.g., the cumulative mass percent finer
(CMPF) versus the Stokes diameter] is deconvoluted from the measured intensity
ratio, I/Io, coupled with Stokes Eq.
Physical Characterizations of Powder
Methods for Measurement of Particle Sizes
Method Range (m)
Microscopy
Optical > 1
SEM > 0.1
TEM > 0.001
Sieving 20 10,000
Sedimentation 0.1 100
Coulter counter 0.5 400
Light Scattering
Scattering intensity 0.1 1000
Brownian motion 0.005 1
X-ray line broadening < 0.1
Physical Characterizations of Powder
Measurement of Particle Size and Size Distribution by Coulter Counter
As a particle passes through the orifice,
it displaces an equivalent volume of the
electrolyte and causes a change in the
electrical resistance, the magnitude of which
is proportional to the volume of the particle.

The changes in resistance are converted to
voltage pulses, which are amplified, sized,
and counted to produce data for the particle
size distribution of
the suspended particles.

Since the number and volume of the
particles are measured in this technique, the
particle size distribution will consist of the
CNPF (or CNPL) versus the volume diameter
x
V
Disadvantage
Blocking of the orifice by bigger particle