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Powder Characterisation PDF
Powder Characterisation PDF
Particle
Smallest unit of a powder that cannot be
subdivided easily
P/M generally deals with particles larger
than smoke (0.01-1 m), but smaller
than sand (0.1-3 mm)
SEM is one of the best tools available to
study particle characteristics
a) tellurium, milled, acicular
b) iron alloy, argon atomized,
spherical with agglomerated
fines
c) tungsten, gas reduced, polygonal
aggregates
d) tin, air atomized, rounded &
ligamental
e) iron alloy, centrifugally atomized,
spherical
f) tin, splat quenched, flake
g) stainless steel, water atomized
rounded & irregular
h) palladium, electrolytic, sponge
i) nickel, carbonyl decomposition
porous
j) iron-based metallic glass,
crushed ribbon, angular plates
k) titanium, sodium reduced &
milled, irregular
l) niobium hydride, milled, angular
Powder characteristics
Particle size & distribution
Particle shape
Surface area
Interparticle friction
Flow & packing
Internal particle structure
Composition, homogeneity & contamination
Powder characteristics
o Properties of single particle
Size, shape, chemistry, microstructure,
density, hardness
Properties of bulk powder
Packing, flow, size distribution, surface
attributes
Powder sampling & dispersion
Collecting a representative sample is a
difficult task
Simple rules for avoiding sampling errors
Powder sample should be taken from a moving
stream
If, taken after shipping
More probability for segregation
Hence, it may not be a true representative sample
It is important to blend the lot before sampling
Sample should be taken from many points
Particle size
Consider a rounded, but
irregular shape particle
Dimensioning the
particle is quite difficult
Widely differing size
determinations are
possible
Depending on the size
parameter
For a cubic particle with a size of 1 m
as measured on each edge, find out
equivalent spherical diameter based on
projected area, surface area and
volume.
DA=1.13 m, DS=1.38 m and DV=1.24
m
Particle clustering
Most of the metal particles are cohesive
Not easily dispersed
Adsorbed moisture causes particle agglomeration
Agglomerate
A cluster of particles held together by weak forces
Can be dispersed easily
Eg. Dried mud
Aggregate
Cluster of crystals or particles held together by strong bonds
Cannot be dispersed easily
Particle clustering
Small particles
Large driving force for agglomeration
Significant problem in characterisation
Agglomerates of small particles are considered as large
particles
Improper characterisation can create
difficulties in processing
Proper dispersion is necessary
Surface active agents can be used
Powder dispersion
First step is to remove adsorbed moisture
Smaller particles (<100 m) exhibit sufficient capillary
forces
Agglomerate with water contents of 1%
Capillary force increases as the moisture content
decreases
Polar molecules are used as dispersants
Carbon chains with charged anionic or cationic terminal
groups
Hydroxyl, sulphite, sulphate, ammonium
Shear forces are effective in conjunction with the
dispersant
Ultrasonic agitation or intensive mixing
Particle size determination
Determination of the dimensions of a particle
Particle size depends on
Measurement technique
Specific parameter being measured
Particle shape
Different instruments will give different values
Because of the differences in the measured parameter
Most of the particle size analysers use only one
geometric parameter
Also assume spherical particle shape
Basis for analysis can be any one of the geometric
values
Surface area, projected area, maximum dimension,
minimum cross-sectional area, volume
Particle size
Spherical particle
Size can be defined by a
single parameter
The diameter
As the shape becomes
more complex
Single parameter may not be
enough
Flake-shaped particle
At least two parameters are
needed An illustration of the difficulty in measuring particle size.
Diameter & width The number of possible size parameters increases
as the particle shape becomes more complex.
Irregular shapes
Large number of parameters
Particle size
Rounded shape
Size can be described in terms of
Projected height, maximum length, horizontal width, equiv.
spherical volume, dia. of a sphere with an equiv. surface area
Irregular shaped particle
Difficult to define a single particle size
Size depends on the attribute measured
So, disagreement between different measurements
Usually a spherical particle shape is assumed
Size is given in terms of diameter
Parameters used for the determination of equivalent
spherical diameter
Surface area, volume, projected area, settling rate
Particle size measurement
techniques
Microscopy
Screening (Sieve analysis)
Sedimentation
Light scattering
Electrical zone sensing
X-ray diffraction
Microscopy
Widely used technique
Reasonably accurate
Size & shape can be observed
Microscopes
Optical, SEM or TEM
Instrument choice depends on particle size
Large depth of field in SEM is a distinct advantage
Analysing statistically significant quantities
Image analysers are used
Microscopes can generate image for analysis
Image analysers count length or area
Generate frequency distribution
Microscopy
A major problem
Obtaining well dispersed
sample
Frequently agglomeration
occurs
Difficult to distinguish the
actual particle size & shape Agglomerated tungsten powder, showing a common
difficulty in separating particles for size analysis by
One technique for microscopy techniques
a) SEM micrograph
dispersing sample b) TEM micrograph
Using 40% naphthalene &
60% camphor eutectic
Orientation independent
parameters are preferred
Equivalent spherical
projected diameter
Screening (Sieve analysis)
Common technique for rapidly analysing particle size
A square grid of evenly spaced wires creates mesh
Common convention for specifying mesh size
Number of wires per inch
200 mesh implies 200 wires per inch
Useful only to particles larger than 38 m
Electroformed meshes available down to 5 m
Screening is useful for obtaining a particular size powder
Termed as classification
Screening also provides a means for removing specific
size particles
Sieve analysis
Stack screens with decreasing
mesh openings
100 g of powder is loaded
Agitated for 15 min.
Amount of powder in each
screen is weighed
Powder passing through a mesh
is designated by –ve sign
Retained on a mesh is Sieve analysis relies on use of a stack of mesh
designated by +ve sign screens of progressively smaller opening sizes
for capture of particles based on the projected
Powder below 45 m is termed cross sectional size
as sub-sieve powder
Problems with screening
Permissible screen variation is 3-7%
Individual openings can be up to 50% larger
Overloading is a common problem
Blocks the mesh openings
Different screens & techniques
Defects in screens will allow oversized particles
Long screening duration may result in breakage of
particles
Too short duration may not be sufficient
8% error can be expected
Minimum error is 1%
Sedimentation
Applicable to smaller sizes
Applicable size range 0.02-100 m
Larger particle sizes need higher fluid viscosities
Particle settling in a fluid reach a terminal
velocity
Dependent on particle size & fluid viscosity
Particle size is estimated from the settling
velocity
Sedimentation
Uses a predetermined settling height
Fluid can be water or air
Air for smaller particles
Amount of powder settling at the bottom w.r.t.
time is measured
Particle size distribution is calculated
Largest particles settle fast
Smallest take considerable amount of time
Automatic instrumentation used
Light blocking, x-ray attenuation, weight or settled
cake height
Sedimentation
Different forces
acting on the settling
particles
Upward buoyancy &
viscous forces
Downward
gravitational force
At the terminal
velocity, the forces
are balanced
Sedimentation
g mD 3
Gravitational settling FG
6
force equals mass m density of particle
times acceleration
g f D 3
Buoyancy force is FB
determined by the 6
f density of fluid
volume of fluid
displaced Fv 3DV
Viscous drag force V terminal velocity, η fluid viscosity
depends on the gD 2 m f
viscosity of fluid V Stokes law
Combining equations 18
1
Experimentally, settling 18H 2
Particle size D
time t is measured for a
known settling height H
gt m f
Sedimentation - Limitations
Limited to narrow size range
Unreliable result with particles below 1 m
Slow settling & turbulence
Certain particles can be quite troublesome
Internal porosity decreases the powder density
Slow particle settling
Irregular particles
Settling depends on hydraulic diameter
May not take a straight trajectory
Prior information of particles are needed
Approximate particle size & density
Concentration should be kept below 1%
To avoid particle-particle interaction
Fluid & powder should not react chemically
Iron powder in water is not advised
Elutriation
A sedimentation technique
Where the fluid flow is in the opposite
direction to gravity
Provides a means of separating into
sized fractions
The greater the fluid flow rate
The larger the particle size carried away
Air classification
Another variation of
sedimentation
Separation of powders using
cyclone or spinning disk and
a cross-current air flow
Lighter or smaller particles
are deflected by air flow
To alter the particle size
separation
Control the disk rotational
speed & air flow velocity
Applicable size range
1-150 m
Streaming techniques
Particles are dispersed in a moving fluid
Size determination is based on a discontinuity in
the fluid stream
Most of the devices are highly automated
Expensive, but popular
Provide a large dynamic ratio (large/small)
Can be as large as 8000
A versatile streaming technique is based on
light scattering
Light scattering
Low angle Fraunhofer
light scattering using
monochromatic light
(laser)
Particle size affects the
intensity & angular extent
of scattering
Angle of scattering varies
inversely with diameter
Intensity of scattered
signal varies with d2
http://www.particletesting.com/docs/primer_particle_sizing_laser.pdf
Light scattering
Computer analysis of intensity versus angle data
Gives particle size distribution
Fraunhofer scattering applied to 1-200 m range
Smallest particles should be at least twice the
wavelength of laser
Particle shape is assumed to be spherical
Detecting agglomeration is difficult
Minimised by proper distribution
Widely used because of easy data collection
Mie scattering is applicable below 3 m
Detector is located at 90˚ w.r.t. incident beam
Both detectors can be incorporated into one
instrument
Expanded dynamic ratio
Electrical zone sensing
Electrical conductivity of a
fluid passing through a
small aperture in an
insulator is measured
Conductivity of fluid
changes when particles
are suspended
Depends on the size of
particles
Common technique for
measuring the size of
blood cells
Electrical zone sensing
An electrolyte flows
through a narrow aperture
in a nonconductive glass
tube
An electrical current is
maintained between the
electrodes inside & outside
of tube
Particles are dispersed in
the fluid
Cause a decrease in the
conductivity
Decrease is proportional to
particle size
Electrical zone sensing
Technique can be applied to several size ranges
Better calibration is needed
Selection of appropriate aperture diameter is important
1.6 times the largest particle size
Dynamic ratio is approx 300
Lower particle size up to 0.5 m
Particle settling problem is acute for high density
materials
Iron & Tungsten
For tungsten powder, limited to <6 m
Low powder concentration should be maintained
Better results are obtained for low density materials
Ceramics & polymers
Light blocking
Another variation of
streaming analysis
A light beam is interrupted
by the flow of dispersed
particles
Particle partially blocks the
light reaching the photocell
The amount of light blockage
is equated to an equivalent
circular cross-sectional area
Dynamic ratio is 45
Problems & limitations
similar to electrical zone
technique
X-ray techniques
Applied to size analysis of very small
crystallites
Diffraction line broadening
strain and small crystal size
Reason for broadening
The destructive interference from the crystal is not
complete at angles slightly different from the
Bragg condition
Due to insufficient number of diffracting planes
The width of the diffraction peak increases as
the thickness of the diffracting crystal
decreases
X-ray techniques
The most widely used
approach
the peak width at half of
the maximum intensity
Scherrer formula gives
the crystal size
The wider the diffraction
peak, the smaller the
particle size
0.9
D
B cos
X-ray techniques
For accurate size analysis
the effect of strain must be subtracted
broadening due to machine sources and
beam divergence must be subtracted
Peak broadening is best applied to
annealed or brittle materials
Milled metal powders usually exhibit non-
uniform strains
X-ray techniques
To isolate the broadening due to crystallite size
Mix a standard that produces a different diffraction pattern
Particle size broadening B is calculated from the total BT
using the difference of the squares
B2=BT2-Bs2
Bs is the peak broadening for the standard
The technique is best applied to crystallites in the
50 nm size range
Under careful experimental conditions
Can be used for crystallites up to 200 nm
This technique gives only a mean crystal size
No distribution or shape information.
Small angle X-ray scattering
The x-ray intensity versus angle is
measured within the 0 to 3˚ range
Can determine the size distribution
The intensity varies with the particle
volume.
most useful for particles below 50 nm
The technique assumes that the
particles are dispersed without
interparticle interference.
Comparison of Particle Size
Analysis Techniques
Analysis of particle size depends upon measuring the
response of a particle to some physical parameter
Spherical particle shape is assumed
Various size analysis techniques will give very
different results for the same powder
Automated instruments are relatively expensive
An accurate particle size analysis is possible using
simple instrumentation and basic physical principles
with a watch and water filled graduated cylinder
The selection of a technique
Depends on several factors including availability and
approximate particle size range
Particle size data
The distribution is given in terms of a
histogram or frequency plot
The amount of powder in each size
increment
The first task
Convert the data into incremental
percentages
Example particle size
distribution data
Mesh size Opening size Weight Interval Cumulative
(m) retained (g) percentage percentage
500 25 0 0 0
400 38 10.8 8.8 8.8
325 45 13.6 11.1 19.9
270 53 16.9 13.8 33.7
230 63 18.0 14.7 48.4
200 75 20.8 17.0 65.3
170 90 16.5 13.5 78.8
140 106 13.2 10.8 89.6
120 125 8.7 7.1 96.7
100 150 3.0 2.5 99.1
80 180 1.1 0.9 100
70 212 0 0 100
measurement tool 1 3
2
S
Does not access closed pores m 5 1 2
is porosity
m is theoretical density of material
Surface area as a shape index
Specific surface As D 2
area is area per unit D 3
V
mass (m2/g) 6
Area per unit weight is A / W
W mV
6
Area per unit weight is S
D m
Interparticle friction
Interparticle friction is another main concern
Powder flow & packing
Factors controlling friction between particles
Surface area, surface roughness, surface
chemistry
As the surface area increases, the amount of
friction increases
Less efficient flow & packing
Important parameter for
Die filling and compaction, packaging,
transportation, blending & mixing
Interparticle friction
Resistance to flow is
a main feature of
friction
Density or packing
properties decrease
Measures of
interparticle friction
Apparent density &
tap density The angle of repose can be determined from
the height and radius of a powder pile passed
The angle of repose through a funnel
Interparticle friction
Flow rate
Rate of powder flow
under gravity through a
small opening
Most sub-sieve
powders will not flow
Non-free flowing
Hall flow meter & Scott
volumeter measure flow
The basic components of Hall flow meter and
rate & apparent density Scott volumeter for measuring the flow &
packing of powders
Interparticle friction
The flow rate is usually expressed as the time
for 50 g of powder to flow through the Hall
flow meter
Short flow times indicate free flowing powders
long times indicate high interparticle friction
For easy determination of the apparent
density and flow time
Hall flow meter with a precision volume cup &
funnel
Interparticle friction
High packing densities are desired in most of the
applications
Improved packing densities
by selecting appropriate particle size, shape, and size distribution
Small particles will have more interparticle friction
So, lower number of nearest neighbours
the smaller the mean particle size, the lower the apparent density.
Tap to apparent densities ratio (Hausner ratio)
Gives a signature characteristic of the interparticle friction
For a spherical powder, slightly above unity.
More irregular particle shapes, higher Hausner ratio
undergo a larger density increase with vibration
True density of powder
Pycnometer is used
to assess the true
density of an
unknown powder
Powder mass
divided by the
A schematic diagram of the true volume
volume gives measurement for a loose powder using a
powder density pycnometer
1 s p
The typical error is P V V P V V V
2 s p c
1%
V p Vs Vc 1 P1 / P2
1
Compressibility
Measures the ability to densify a powder
under an applied load
Density measured after compaction
Green density
pressure, often near 400 MPa
Compression ratio
CR=VL/VC=g/a
A parameter used in tool design
Particle size, particle chemistry, lubrication
will determine the pressed density
Powder internal structure
Cross-sectional analysis
provides information on internal pores &
segregation
can be useful in detecting inclusions and oxides
Such microstructures
indicate subsequent
processing problems,
since internal pores are
difficult to eliminate
Powder internal structure
SEM analysis
Important microstructure information can be gained
Additionally, nucleation sites, contamination, cooling rate,
grain size, and segregation can be assessed
Material Tungsten
Designation -325 mesh
Metallic chemistry 99.99% W
Impurities (ppm) C (10), Cu (1), Fe (2), K (15),
Mg (4), Mo (10), N (100), Na
(6), O (740), Si (2)
Apparent density 4.37 g/cm3 (23%)
Tap density 8.05 g/cm3 (42%)
Flow time for 50 g Not free flowing
BET specific surface area 0.12 m2/g
Gas permeability surface area 0.028 m2/g
Particle size by sedimentation D10 = 3.0 m
D50 = 6.4 m
D90 = 12 m SEM micrograph of
tungsten powder
Particle size by electrical zone D10 = 3.5 m
sensing D50 = 6.2 m
D90 = 8.9 m
A spherical nickel powder is analyzed for particle size using sedimentation.
It is suspected that the particle size is 8 m. If the powder is dispersed in water
at the top of a settling column 100 mm high, then what is the expected settling
time? Nickel density is 8.9 g/cc, water viscosity is 10-3 kg/m/s. Also calculate the
time taken by a tungsten particle of size 2 m (Tungsten density is 19.3 g/cc).
1
18 H 2
Particle size D
gt m f
The specific surface area of nickel powder is 20 m2/g.
Find the diameter of particles.
For iron with an apparent density of 2.4 g/cc, a pressure of 770 MPa gives a
density of 7.0.8 g/cc. What is the fill height needed to form a compact of
height 1.5 cm?