3.

Powder characterization
 Powder and powder morphology: definitions
Powder: Dispersed system
Collectiv made of particles with different form and size

Powder particle
(Primary particle)
Grain •Single crystalline/polycryst./amorphous
(Crystal) •Single/multi-phased
•massive/hollow

Sekundärteilchen

Agglomerate Aggregate
•Soft/weak bonding between prim. part. •hard
•Intentially/unintentially •unintentially
•Spherical/irregular •irregular
Powder particle shape

Thümmler, S. 67, Fig. 3.2

Adhesion force between primary particles in agglomerates

Solid state bridges made of crystallized salts or sintering contacts

Immobile liquid bridges made of viscous binders or adsorbed layers
Mobile liquid bridges (capillary forces)
Van der Waals and electrostatic forces
Mechanical anchorage
 Powder characteristics

•Particle size
Particle size distribution
Particle form (variation with particle size and topologie)
Specific surface
Surface topography
Friction between particles (powder flow ability)
Packing density (apparent density, tab density)
Particle microstructure (single/polycrystalline, single/multi-phase, porous)
Chemical composition (concentration gradient, segregation)
Contaminations
Surface layers (hydrolysis, oxidation)
 Features of particle size

•Particle diameter
•Projected image of the particles
•Particle surface
•Particle volume
•Particle mass
•Settling velocity of the particles in a stationary fluid
•Manipulation of electrical fields by particles
 Description of the particle size
Size parameter
Maximum cord length (M)
Projected Area (A)
Volume (V)
Surface area (O)

Equivalent spherical diameter d

dA = (4A/)1/2
dV = (6V/)1/3
dO = (O/)1/2

dA (Projected area diameter) Diameter of a circle with equal projected area

d v (Volume diameter) Diameter of a ball with equal volume

d O (Surface diameter) Diameter of a ball with equal surface

d sv (Surface-volume diameter) Diameter of a ball with equal surface/volume ratio

d F (Free falling diameter) Diameter of a ball with equal density and falling velocity

d St (Stokes diameter) Diameter of a ball with equal density and falling velocity in a fluid
with a Reynolds number smaller than 0.25

d S (Sieve diameter) Smallest square opening the particle can pass through
 Sieve analysis
Vibrating sieving machine

Coarse

Particle number of a fraction

N = 6w/(mD3)
Fine w: Mass of the fraction
m: Theoretical density
D: Particle diameter

Starting Final
 Sieve analysis

Opening size Size class Fraction Passed Retained

Particle size amount amount

Iron powder formed by atomization < 400 m

 Particle size distribution

Frequency distribution Cummulative distribution

(Histogram)
[%] [%]
100 100

50

0 0
xmin xi-1 xi xmax xmax
xmin x50
Particle size Particle size
[m] [m]

Fraction within a size class i Quantity proportion (xmin ....xi)

f ( xi )  F ( xi ) 
Class width ( xi  xi 1 ) Total quantity (xmin .... xmax)
Probability grid
 Distribution function in the logarithmic probability grid

Passed amount in %

1: Fe powder obtained by atomization Particle size in µm

2: Cu powder obtained by atomization
 RRSB distribution

F(x)

x x`
Typical distribution functions
 Methods for the determination of the particle size
Method Size range [m]

Particle separation (Cassification)

Sieve analysis:
Wire mesh 32 -
Electroform 5 - 100
Counterflow classifiers:
Gravitational field 5 - 60
Centrifugal field 1 - 60
Sedimentation
Gravitational:
Pipette method
Sedimentation balance 1 - 60
Photosedimentometer
Centrifugal:
Centrifugation 0,05 - 10

Counting methods
Electrical zone sensing/light blocking 0,4 – 1200/1 - 600
Light microscopy 1 - 100
Electron microscopy 0,004 - 1

Scattering and diffraction

Light scattering 0,1 - 200 (projected area-weighted)
Small angle x-ray diffraction <0,05
Broadening of x-ray reflexes (wide- <0,2 (volume-weighted)
angle diffraction)

Specific surface area

BET <20
Subsieve Sizer
Counterflow classifier
Gravitational field

d < dT

d = dT

d > dT

Air in
 Sedimentation analysis
Pipette method

18h
d
( T   M ) gt

h d: Particle diameter
: Fluid viscosity
T: Particle density
M: Density of the fluid
g: acceleration (gravity)
h/t=v: Fall velocity
Sedimentation analysis
Sedimentation balance
 Coulter Counter
(Electrolytic cell)
Counting by disturbance of an electrical field

Powder particle

Electrolyte

 Particles are suspended in an electrolyte

 Suspension flows through aperture
 Particle in the aperture influence the electrical resistivity of the cell
 Counting of signals
 Electrical Resistivity is proportional to the particle volume
 Light blocking
Optical counting
Suspension
flow

Particle

Photo cell

Light source
(Laser)

Collimator

Window

Particles flow individually (diluted suspensions !) an illuminated sensing zone

Particles interrupt the light beam
Counting of the interruptions
Particle size can be derived from the weakening of the light intensity