Class 03

MTE 449 Powder Metallurgy
Chapter 2
Powder Characterization Techniques
Nagy El-Kaddah
Powder sampling
¾ Obtaining a representative sample is critical to
ensure measurement of real particle characteristics.
¾ Particles in produced powders tend to separate
during shipment and to agglomerate during storage.
¾ To obtain representative samples and minimize
sampling errors
¾ Samples must not be taken from the top or bottom of
the powder container.
¾ Samples should be taken from several locations and
mixed together
¾ Deagglomerate the particles by
¾ Drying the powder to remove adsorbed moisture
¾ Adding dispersants (organics with charged
anionic or cationic terminal groups)
¾ Mechanical stirring or ultrasonic agitation
¾ Samples should be taking from a moving stream of
particles
¾ Riffling is the most reliable practice for powder
sampling
Particle Size Measurement Techniques
¾ Microscopy
¾ It is a direct method to measure both particle size and particle shape
¾ Optical microscopes permit measurement of particles larger than 1 μm
¾ SEM extends the range down to 0.01 μm, shows surface topography and
permits compositional analysis.
¾ Measurement of characteristic dimensions of imaged particles is now
performed using an image analyzer attached to the microscope
¾ This technique is not suitable to measure particle size distribution.
¾ Sieving
¾ It is the oldest method, and reasonably accurate for particles larger than
38 μm
¾ This technique involves passing the materials successively over a series
of screens having progressively smaller openings
¾ The particles retained on a screen have a size between apertures (clear
space between individual wires) of that screen and the one above it.
¾ It gives particle size distribution in coarse size intervals
¾ The accuracy of this method is about 8%
Particle Size Measurement Techniques (cont.)
¾ Sedimentation
¾ It is based on measuring selling velocity of the particle and determining particle
size from Stokes equation for terminal velocity of a falling sphere
g D2 (ρm − ρ f )
V=
18 η
¾ This technique basically involve measuring time (t) for a particle to move a distance
H in a tube filled with a liquid of a viscosity η to determine particle velocity.
V=H/t
¾ The settling time in modern equipment is measured from the turbidity of the fluid at
distance H using a light source, slit and photodetector.
¾ From the measured time, the particle size is calculated using the following equation
1/ 2
⎛ 18 η H ⎞
D=⎜ ⎟
⎜ g (ρ − ρ ) t ⎟
⎝ m f ⎠
¾ Because stokes equation is only valid at low Re (<2), this technique is used for
particles smaller than 60 μm.
¾ To avoid the interaction between particles, which is known to affect settling
velocity, this technique uses very dilute suspensions of particles, and as a result it
is limit to particles with narrow size distribution.
¾ Light Scattering
¾ It is based on measuring the intensity and
the angle of a scattered light from the
particle.
¾ The intensity varies with the square of
particle diameter, while the angle varies
inversely proportional with the diameter
¾ These two characteristics permits accurate
determination of particle size in the range
between 1 and 200 μm.
¾ The analyzer consists of a container
placed in the gap between a laser and a
detector. A continues stream of a fluid
with dispersed particles enters at top and
exit the bottom of the container, and the
signal from the detector is analyzed using
a computer.
¾ The streaming feature of this technique
permits measurement of particle size
distribution.
¾ Electrical Zone Sensing
¾ It is based on measuring the changes in the
resistance of the fluid due to the flow of
particles through a small aperture
¾ The change of the resistance is proportional to
square of particle diameter.
¾ The apparatus consists of a tube with small
hole placed in tank filled with suspended
particles. Electric current passes through the
fluid via two electrodes, one in the take and the
other in tube. The flow through the aperture is
driven by a pump.
¾ It is used for particles between 0.5 and 100 μm
and measure particle size distribution.
¾ Other Techniques
¾ Light blocking
¾ X-Ray Line Broadening
Surface Area Measurement Techniques
¾ Gas Adsorption BET Method
¾ It is based on adsorption of a monolayer of gas molecules
on the surface of the particle at very low temperatures
¾ At saturation, the surface area is equal to mass of adsorbed
gas (wm) and the amount of adsorbed gas prior to saturation
(w) depends on the gas pressure (P)
1
=
1
+
(C − 1)Po
w(Po / P − 1) wmC wmC P
¾ The approach to determine wm and hence specific surface area S is to measure w at
different pressures and plot 1/w(P/Po-1) vs. P/Po to obtain the slop (s) and intercept (i)
for computing wm and S 1 w N Ao
wm = S= m
0.3
s+i W MW
0.25 Tantalum Powder
0.2
P/P o
0.15
0.1
Slope = 0.0004
Intercept = 0.0193
0.05 Surface area = 399 m 2 /kg
0
0 200 400 600 800
1/w(P/P o-1)
Surface Area Measurement Techniques (cont.)
¾ Gas Permeability Surface Area Analysis

¾ It is less accurate that BET method but very practical
¾ It exploit dependence of permeability of a gas flowing through a
porous column on bed on the surface area
¾ From measurement of the flow through a cylinder of packed powder,
we determine permeability (α) of the packed powder using Darcy’s
equation
Q = ΔP α A/ L η
¾ Based on Kozeny-Carman analysis the surface area of the compact is
1/ 2
1 ⎡ ε3 ⎤
S=
ρ m ⎢⎣ 5 α (1 − ε ) 2 ⎥⎦
where ε is the porosity of compact, which can easily be measured

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MTE 449 Powder Metallurgy

¾ Gas Permeability Surface Area Analysis

where ε is the porosity of compact, which can easily be measured

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