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Introduction
Static light scattering
Measurement process
Important instrumental considerations
Applications
Introduction
Static light scattering (SLS) or more commonly known as laser
scattering/diffraction is used for the size determination of micron to
submicron particles. The laser diffraction technique for the
determination of particle size distribution is based on the
phenomenon that particles scatter light in all directions with an
intensity pattern that is dependent on particle size (and shape).
Introduction
Assumptions
Requirements
Characteristics
Particles suspended in a fluid
RI difference between particle and fluid
Large particle
Small/low angle scattering
Large signal/intensity
Small particle
Big/high angle scattering
Small signal/intensity
Scattering pattern
Characteristics
The figure below shows the effect of size on the scattering pattern
detected at different angles. Note that the scattering intensity at the
front of a particle (close to 0 degree) is always the highest and bigger
particle scatters more intensely as compared to a smaller one.
Characteristics
Characteristics
Why you need two light sources of different wavelengths?
Theory
Mie
Rigorous solution valid for all sizes of spherical particles
Requires optical propety (RI) to be known for both
sample and dispersant
Fraunhofer
Approximation for large particles (~> 50 micron) or
opaque particles
Optical property (RI) is not necessary
Limited to forward (low angle) scattering
Theory
Big particle
Theory
Small particle
Assumptions
All particles are spherical and optically homogeneous.
If particles are not spherical, then the scattering pattern obtained is
used to calculate the equivalent spherical diameter for the particles.
Requirements
1. Sample dispersion in a fluid (liquid or air) is necessary.
2. Sample cannot dissolve or react with the fluid it is dispersed in.
3. There must be a difference in refractive index of the sample and
the fluid.
4. Particle concentration cannot be too high (multiple scattering) or
low (low signal).
5. Refractive index of the sample and fluid should be known,
especially for small particles.
Requirements
Reflected
Refracted
Absorbed
and
Reradiated
Diffracted
Requirements
Requirements
Measurement process
Static/laser light scattering measurement process
Sample is dispersed in a fluid (liquid or air) in a cell
Monochromatic light source(s) illuminate(s) the cell
The light scattered by the particles, at various angles, is measured
by multi-element detectors
The scattering pattern is used to calculate the particle size
distribution
Measurement process
14
100
q(%)
60
40
20
0
0.010
0.100
1.000
10.00
Diameter(m)
100.0
1000
0
5000
Undersize(%)
80
10
2. Detection system
3. Sampling mechanism
4. Performance specifications
Images are obtained from the internet and are copyright of respective owners
90 o
270 o
180 o
Scattering patterns
for 0.05 and 0.07
micron particles with
650 nm laser and 405
nm LED
Applications
CMP slurry
Pigment ink
CMP slurry
http://www.horiba.com/semicondu
ctor/products/processes/semicond
uctor-process/cmp-process/
CMP slurry
http://www.horiba.com/scientific/products/particlecharacterization/applications/cmp/
CMP slurry
What is a CMP slurry?
CMP slurry is a special chemical formulation that has abrasive
particles with a specific (narrow) size range and pH value. The
abrasive particles can be silica, alumina, ceria, titania, diamond, etc.
A silica CMP slurry normally has a high pH value that has a certain
weight % of silica abrasives. The alkaline solution helps to soften/etch
the silicon wafer surface while the abrasive particles remove material
from the surface through mechanical action.
CMP slurry
An example of a silica CMP slurry
http://www.fujimico.com/catalog/Chemical%20Mechanical%20Planarization/33
CMP slurry
A certain CMP slurry particle size specification
CMP slurry
Particle size measurements needed by:
CMP slurry producers to control their product quality
End users to confirm specification before use and periodic check to
ensure consistent performance
CMP slurry
Silica CMP slurry
40
100
q (%)
60
20
40
10
0
0.010
20
0.100
1.000
Diameter (m)
0
10.00
Undersize (%)
80
30
CMP slurry
Diamond CMP slurry
45
100
40
q (%)
30
60
20
40
10
0
0.010
20
0.100
1.000
Diameter (m)
0
10.00
Undersize (%)
80
Pigment ink
What are pigments?
Industrially, a pigment is any finely divided
insoluble black, white or colored solid
material, a major function of which is to
improve the appearance of or give color to
the medium in which it is to be used.
Pigment ink
Types of pigments
Pigment ink
What are pigment inks?
Pigment inks are complex liquid dispersions of pigments, binding
agent and additives. A binding agent is normally a plastic resin.
Additives commonly consist of anti-foam, waxes, extenders, pHcontrollers and surfactants. Pigment inks can be solvent based or
aqueous based.
Pigment ink
Why do you need to know particle size and distribution for pigment inks?
Pigment ink
Particle size and distribution for pigment inks
Pigment ink
C I pigment blue 15
16
100
10
q (%)
60
40
5
20
0
0.010
0.100
Diameter (m)
0
1.000
Undersize (%)
80
Pigment ink
C I pigment blue 15:3
23
100
20
q (%)
15
60
10
40
5
0
0.010
20
0.100
Diameter (m)
0
1.000
Undersize (%)
80
Gracias
Tack
Danke
Cm n
Grazie
Obrigado