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Powder Characterization

This document discusses techniques for characterizing powders, specifically particle size analysis. It describes several common techniques: microscopy, screening, and sedimentation. Microscopy can be used to directly measure particle sizes above 1 μm by imaging particles and counting dimensions. Screening involves separating particles into fractions based on their ability to pass through screens of decreasing mesh size, useful for particles above 38 μm. Sedimentation relies on particles settling at different rates depending on size in a fluid, applicable in the 0.05 to 60 μm range. The document emphasizes the importance of particle size for powder properties and processing and notes challenges in analysis.

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0% found this document useful (0 votes)
200 views21 pages

Powder Characterization

This document discusses techniques for characterizing powders, specifically particle size analysis. It describes several common techniques: microscopy, screening, and sedimentation. Microscopy can be used to directly measure particle sizes above 1 μm by imaging particles and counting dimensions. Screening involves separating particles into fractions based on their ability to pass through screens of decreasing mesh size, useful for particles above 38 μm. Sedimentation relies on particles settling at different rates depending on size in a fluid, applicable in the 0.05 to 60 μm range. The document emphasizes the importance of particle size for powder properties and processing and notes challenges in analysis.

Uploaded by

ecternal
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PPTX, PDF, TXT or read online on Scribd
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to introduce the techniques and measures available for describing

powders.
The influence of the powder characteristics on processing and
properties will be demonstrated in subsequent chapters.
1.POWDER SAMPLING
A typical production lot may be several
tons in size; a sample of this lot will
probably be on the order of a
kilogram.
Many of the modern analytical
instruments require sample sizes of a
gram or less for particle size analysis.
Assuming a spherical shape, the
particle population in one gram
depends on the size and material
density ( theoretical density).
2. PARTICLE SIZE
The size of a particle depends on :
a.The measurement technique
b. specific parameter being measured
c. particle shape.

Particle size analysis can be achieved by several techniques, which
usually do not give equivalent determinations due to differences in
the measured parameters.
The basis for analysis can be any of the obvious geometric values,
such as surface area, projected area, maximum dimension,
minimum cross sectional area, or volume.

Particle size is probably one of the most important powder
characteristics to the powder metallurgist. Size data are most useful
when presented within the context of the measurement basis and
the assumed particle shape.
A particle size analysis should convey information on the particle
size distribution, particle shape, and state the basis for measuring
particle size. The desire is to use a particle dimension most
characteristic of the powder.

l. Microscopy
The procedure is covered in American Society for Testing Materials
specification E20 (ASTM E20).
Although the technique is reasonably accurate, the tedium of sizing
statistically significant quantities of particles has led to use of
automatic image analyzers.
The image for analysis is generated by optical, scanning electron or
transmission electron microscopes.
The instrument choice depends on the particle size.
By microscopic counting of diameter, length, height or area, a
frequency distribution can be generated.
Counting two or more small particles as a large particle will cause a
skewing of the distribution towards the coarse sizes.

2. Screening
The most common technique for rapidly analyzing particle size is
based on screening.
A square grid of evenly spaced wires creates a mesh.
Mesh sizes can not go to very small opening sizes; thus, the
screening technique is usually applied only to particles larger than
38 m.
There are electroformed meshes available down to 5 m, but
agglomeration and particle adhesion to the mesh generally make the
electroformed screens of little practical use.
A listing of mesh sizes and opening sizes for the U. S. Standard
series of screens appears in Table l.2.3 (ASTM E11).
TABLE Standard Sieve Sizes (U. S. Standard. ASTM E119 )

Mesh Size Opening in m
Permissible Variation +,-
m
Maximum Individual Opening in
m
18
20
25
30
1000
850
710
600
40
35
30
25
1135
970
815
695
35 500 20 585
40 425 19 502
45 355 16 425
50 300 14 363
60 250 12 306
70 212 10 263
80 180 9 227
100 150 8 192
120 125 7 163
140 106 6 141
170 90 5 122
200 75 5 103
230
270
325
400
63
53
45
38
4
4
3
3
89
76
66
57
The powder is loaded onto the top screen and the screen stack is
vibrated for a period of 20 to 30 minutes.
For particle size analysis, a sample size of 200 g is usually sufficient
when using 20 cm diameter screens. After vibration, the amount of
powder in each size interval is weighed and the interval percent
calculated for each size fraction (ASTM B214)
3. Sedimentation
Particle size analysis by sedimentation is most applicable to the finer
particle sizes.
Particles settling in a fluid (liquid or gas), reach a terminal velocity
dependent on both the particle size and the fluid viscosity.
On this basis, particle size can be estimated from the settling
velocity. Depending on the particle density and shape,
sedimentation techniques are most applicable to particles in the
0.05 to 60 m range.

F
G
=
F
G
=
( ) g
D
m

t
6
3

D is the particle diameter,
g is the acceleration (gravity)

m
is the particle density
The buoyancy force is determined by the volume of fluid displaced
by the particle,
F
B
=


( ) g
D
t

t
6
3
Finally, the viscous drag force Fv is given as.
F
V
=

DVU t 3
U is the fluid viscosity.
For a sedimentation experiment,
the velocity is calculated from the
height and time.
Combining equations gives.
V =
( )
( ) U
gD
t m
18
2
For the terminal velocity, which is known as STOKES LAW. It is
experimentally most convenient to work with a known settling
height H while measuring the time for settling.

D =

( ) ( )
2 / 1
18
(

t m
gt
HU














Figure 1.2.1 The force balance leading to a constant settling velocity for a spherical
particle in a viscous fluid.

Internal porosity in the powder decreases the mass, thereby causing
slower particle settling.
There are mathematical limits to Stokes law. The derivation
assumes that viscosity controls settling.
Accordingly, at Reynolds numbers R in the range of 0.2 to l.2 the
assumption of viscosity controlled settling break down.
At high settling velocities the sedimentation model is invalid if the
calculated Reynolds number is large, where gives the Reynolds
number in terms of the settling parameters. Finally, the fluid and
powder can not react chemically.
In spite of these several difficulties, sedimentation techniques are in
use for several powder systems such as the refractory metals.
Automatic instrumentation for performing sedimentation based
analyses use light blocking, x-ray attenuation, weight or settled
cake height to determine the size distribution.
4. Light Scattering
5. Electrical Conductivity
6. Light Blocking
7. X-Ray Techniques


PROBLEMS IN PARTICLE SIZE ANALYSIS
For sieves, this is generally above 38 m
optical microscopy is restricted to particles above l m
In contrast, techniques such as sedimentation are only applicable to
a narrow size range because of limitations in the applicable physics.
PARTICLE SHAPE

The shape of a particle is a distributed parameter, which can
influence packing, flow, and compressibility of a powder.
Particle shape provides information on the powder fabrication route
and helps explain many processing characterictics.
Because of the difficulty in quantifying particle shape, qualitative
descriptors are used.
Figure 1.2.2 gives a collection of particle shapes and shows the
appropriate qualitative descriptors.
Figure 1.2.2 A collection of possible particle shapes and qualitative descriptors.

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