Powder Characterizations

Knowledge of the powder characteristics serves key purposes:

 Quality control of the starting material

 Ability to control the microstructure/final properties of the fabricated material

 Process automation

Powder Characteristics that Have a Significant Influence on Processing

 Property Method
Particle size and size distribution Sieve analysis, permeability, sedimentation, electrical
zone sensing, light obscuration, light scattering,
microscopy, surface area
Particle shape (external) SEM, shape parameters, morphological analysis,
fractals
Particle shape (external and internal) Stereology, mercury porosimetry, gas adsorption

Particle density Pycnometry, mercury porosimetry

Specific surface area Gas adsorption, permeametry
Surface chemistry X-ray photoelectron spectroscopy, Auger, SIMS, ion
scattering spectroscopy
Inclusions Acid insolubility test
Phase analysis Metallography, stereology, electron miscoscopy,
EDAX, XRD
Extent of mixing/segregation Macro-region: Variability Co-eff. (chem. Analysis),
Micro-region: Variability Co-eff. (2nd phase >5%),
Homogeneity Co-eff. (2nd phase <5%), by
Metallography
 Powder sampling

The following issues need to be addressed when

developing, or adapting, a sampling procedure:

i)the quantity of powder from which the samples are to be

obtained,
ii)the amount of sample required
iii)the powder characteristics including flow behavior, particle
shape, tendency to segregate and surface chemistry, and
iv)mechanical strength
 COMPARISON OF SAMPLING DEVICES
Device Advantages Disadvantages

Cone & Good for powders with poor flow Very operator-dependent
Quartering characteristics

Scoop Sampling Reliable for homogeneous and non- Particle segregation and non-
flowing powders flowing powders
Table Sampling Able to separate large quantity of Very dependent upon initial
material feed
Chute Splitting Can reduce powder sample Operator bias by 50% in one
pass
Spin Riffling Reliable for free-flowing powder Not efficient at handling large
samples samples of powder

Static sampling: (i) scooping, (ii) thieving

and (iii) cone & quartering.

Dynamic sampling: (i) table sampling,

(ii) chute splitting, and (iii) spin riffling.
Cone & Quartering

Chute Splitting
Particle Size and Shapes
 Class Method Size range
(m)
Sieving Mechanical/ultrasonic agitation 44-800
and screens/sieves
Microscopy Micromesh screens 5-50
Visible light 0.2-100
Electron microscopy 0.001-5
Sedimentation Gravitational 1-250
Centrifugal 0.05-60
Turbidimetry Turbidimetry 0.05-500
(light intensity attenuation)
Elutriation Elutriation 5-50
Electrolytic resistivity Coulter counter 0.5-800
(zone sensing)
Permeability Fisher subsieve sizer 0.2-50
Surface area Adsorption of gas phase 0.01-200.01-50
Adsorption of liquid phase
 Size and Morphology
Measurement of particle size

• Reduce to known geometry

– Volume
• Cubes
• Spheres
• Ellipsoids
– Area
• Circles
• Squares
• Ellipses
– Lengths
• Characteristic lengths
A= Projected area • Feret and Martin diameters
P=Perimeter • Relate to the geometry
d=equivalent diameter
– Fit into the geometry
S=surface area
– Have equal Volume or Area
V=volume
– Have equal properties
 Size and Morphology
Descriptors based on diameters of circles

dcirc= Diameter of circumscribed

minimum circle

dinsc= Diameter of inscribes maximum

circle

deq= Diameter of the circle having same

area as projection area of particle

Shape descriptor: Circularity

deq/dcirc
Feret diameter: mean value of the distance between pairs of parallel
lines tangent to the two-dimensional outline of a particle shape;
note that the maximum value of the Feret diameter is frequently
quoted as the Feret diameter without qualification.

Geometric average diameter: Geometric average of the chord

lengths of the particle surface along the three orthogonal principal
axes of that surface, which approximates the equivalent spherical
diameter

Martin diameter: Mean chord length of the two-dimensional

outline of a particle shape.
 Size and Morphology
Feret and Martin diameter
• The Feret diameter the distance
between two tangents to the
contour of the particle in a well
DFeret defined orientation.
• The Martin diameter, is the length
of a line that divide the area of the
DMartin particle into two equal halves.
• Normally measured
– Mean= the mean over several
orientations
– Y=largest
– X=smallest
– Elongation= Y/X
 Size and Morphology
More descriptors according to the same principles

Name Definition Formula

Volume Diameter of a sphere having the
diameter same volume as the particle V d 3

6
Surface Diameter of a sphere having the
diameter same surface as the particle S  d 2
Surface Diameter of a sphere having the
volume same surface to volume ratio as 
the dsv  dv3 /6d 2s
diameter particle
Projected Diameter of the circle having the

area same area as the projection area of A d 2

diameter particle 4

Perimeter Diameter of the circle having the
diameter same perimeter as the projection P  d
peramiter of particle

 Size and Morphology
Diameter Defined from equal properties
Drag diameter
• Diameter of a sphere having the same resistance to motion as the particle in a
fluid of the same viscosity and the same speed
Free-falling diameter
• Diameter of a sphere having the same density and the same free-falling speed
as the particle in a fluid of the same density and viscosity
Stoke diameter
• The free falling diameter of a particle in the laminar flow region
Aerodynamic diameter
• the diameter of a sphere of unit density (1 g/cm 3) that has the same
gravitational settling velocity as the particle in question.
Equivalent light-scattering diameter
• Diameter of the sphere giving the same intensity of light scattering as that of
a particle, obtained by the light-scattering method
Sieve diameter
• The diameter of the smallest grid in a sieve that the particle will pass
 Size and Morphology
Stoke diameter

• For small particles <0.5m

msolvent*g Brownian motions counteract
Brownian motion gravitational forces and the
kT
D system will be stable
6a • For larger particles
a

2d g 2
v
18
2a 2 g
v
mpart*g
9 • Density matching will hinder
sedimentation


 Size and Morphology
From descriptors
• Elongation (aspect ratio): L/B or dFeret(max)/dFeret(min)

• Circularity: for example, deq/dcirc

2
d  dv 
2
   
v

S p  ds 
• Sphericity (Wandells):

S p  f x d a2
• Form factors: f/k will describe the form
V p  k x d a3

• Space Filling Factor: The ratio between the area of a circumscribed

rectangle or circumscribed circle of the image and that of the particle
 Material properties: Density
• Theoretical density: calculated from the crystallography
• True particle density: The density of the material
• Pyncometric density: Density of the powder/compact
determined by He-pycnometry.
• Apparent particle density: Density of the particle when inner
porosity is included
• Apparent density of powder: Density of the loose powder
filled in density cup following MPIF std. 4-45.
• Tap density of powder: : Density of the tapped powder filled
in density cup following MPIF std. 4-45.
• Effective or aerodynamic particle density: Density if outer
porosity is included. Related to the density that a air or gas
stream will measure.
• Green and sintered density: Will be discussed subsequently
 Powder
Density, air content and porosity

• Density (b)= weight of

powder/Volume of powder
• Air content= air in pores(entrapped
air) and air in between particles (void
air)
• Porosity
• In particle
• Between particles
 Powder: Flow properties and powder density
(MPIF std. 3-45)
• Angle of repose: measure of
friction

Flow Angle Carrs

characte of index
• Density
r repose
– Bulk Very good <20 5-15
– Apparent density
Good 20-30 12-16
– Tapping density
Ok 18-21
– Carrstapped
indexdensity  poured density Poor 30-34 25-35
Carr index 
tapped density Very poor 33-38
Extremely >40 >40
– Hausner ratio poor
tapped density
Hausner ratio 
poured density
 ASTM B 212 ASTM B 329

Hall Flow meter and Carney Funnel Scott volumeter

 Surface properties
Particle surface
• Properties
– Roughness of the surface
– Composition
– Surface energy
• Influences
– Stability
– Total area
– Particle size reduction
– Adsorption of other
substances to the surface
– Aggregation
– Release of adsorbed
material
 Powder
Specific surface

• Surface per weight • Importance

• Factors that increase surface
area
– Dissolution
– Decrease in particle size – Chemical reactions
– Increase in surface
roughness
– Adsorption of other
– Inner porosity (if available) molecules
• Method dependent parameter – Flow though
– Permeatry
particle beds
– Gas adsorption
– Gas diffusion
– Porosimetery
 SURFACE AREA MEASUREMENT

BET (Stephen Brunauer, Paul Hugh Emmett, and Edward Teller) Surface area measurement
technique: Based on physical adsorption of gas molecules on a solid surface. The concept of the
theory is an extension of the Langmuir theory, which is a theory for monolayer molecular adsorption,
to multilayer adsorption with the following hypotheses:
(a) gas molecules physically adsorb on a solid in layers infinitely;
(b) there is no interaction between each adsorption layer; and
(c) the Langmuir theory can be applied to each layer.
Po=saturation pressure is the pressure for a
The resulting BET equation is expressed by: corresponding saturation temperature at
P 1  P  which a liquid boils into its vapor phase
 1   C  1 
X  P0  P  X m C  P0 
Where
P Partial pressure of adsorbate
P0 Saturation pressure of adsorbate
X Amount of gas adsorbed at a pressure
X m Monolayer capacity of the powder
C Constant related to adsorption enthalpy

Surface area S is given by:

X m N A A0
S
wM
 BET vs. Langmuir theory
five assumptions:
1. Adsorptions occur only on well-defined sites of the sample surface (one
per molecule)
2. The only considered molecular interaction is the following one: a molecule
can act as a single adsorption site for a molecule of the upper layer.
3. The uppermost molecule layer is in equilibrium with the gas phase, i.e.
similar molecule adsorption and desorption rates.
4. The desorption is a kinetically-limited process, i.e. a heat of adsorption
must be provided:
4.1. these phenomenon are homogeneous, i.e. same heat of
adsorption for a given molecule layer.
4.2. it is E1 for the first layer, i.e. the heat of adsorption at the solid
sample surface
4.3. the other layers are assumed similar and can be represented
as condensed species, i.e. liquid state. Hence, the heat of
adsorption is EL is equal to the heat of liquefaction.
5. At the saturation pressure, the molecule layer number tends to infinity (i.e.
equivalent to the sample being surrounded by a liquid phase)
 BLENDING/MIXING
• To make a homogeneous mass with uniform distribution of
particle size and composition
– Powders made by different processes have different sizes
and shapes
– Mixing powders of different metals/materials
– Add lubricants (<5%), such as graphite and stearic acid, to
improve the flow characteristics and compressibility of
mixtures
• Combining is generally carried out in
– Air or inert gases to avoid oxidation
– Liquids for better mixing, elimination of dusts and reduced explosion
hazards
• Hazards
– Metal powders, because of high surface area to volume ratio are
explosive, particularly Al, Mg, Ti, Zr, Th
 Equipment for Blending/Mixing Powders

cylindrical rotating cube

double cone
twin shell

•Under controlled condition  contamination, deterioration

•High shape factor  explosive: Al, Mg, Ti, Zr, Th
 Variables in powder mixing process
 Type of mixer
 Volume of mixer
 Geometry of mixer
 Inner surface area of the mixer
 Constructional material and surface finish of the mixer
 Volume of the powder in the mixer before and after mixing
 Volume ratio of mixer to powder
 Characteristics of component powders
 Type, location and number of loading and emptying devices
 Rotational speed of mixer
 Mixing time
 Mixing medium (gaseous or liquid)
 Humidity, when mixing in air
 Shaping and Compaction
Conventional Compaction Powder Injection Moulding Binder Assisted Processing

•Uni-axial-single action/double action • Slurry techniques-slip/tape casting

•CIP •Freezing techniques
•Extrusion
 COMPACTION
A die cavity that is closed on one end (vertical die, bottom end closed by a
punch tool) is filled with powder. The powder is then compacted into a shape
and then ejected from the die cavity.

•Green compact: as-

pressed
- shape
- (green) density
- contact of particles
•Compressibility 
green density
COMPACTION PRESS
 THEORY

Release of the compact from its mold is usually

accompanied by small volume increase called
"spring-back.“
Pressure distribution inside a die
Ff μF 4 μ k P dH
dP  Pb  P    n 
A A D

 4μk H
Ph  P exp  
 D 
Parametric relationship: COMPACTION
Source: ASM Handbook Volume 7: Powder Metallurgy
Density variation in compacting metal powders in various dies: (a) single-action press; (b), (c)
and (d) double-action press.

Note in (d) the greater uniformity of density, from pressing with two punches with separate
movements, compared with (c).

(e) Pressure contours in compacted copper powder in a single-action press.

Four classes of PM parts (side view shown; cross-section is circular):

(a)Class I - simple thin shapes, pressed from one direction;
(b)Class II - simple but thicker shapes require pressing from two directions; 4 zh / D
•Uniform density by multiple punches: (d) p  p e
h
(c)Class III – two levels of thickness, pressed from two directions; and o
(d)Class IV - multiple levels of thickness, pressed from two directions, with separate controls for
each level
 P/M parts design
Dimensions
Shapes
Tolerances
Holes
Wall Thickness
Flatness
Edges
Fillets and Radii
Countersinks
Undercuts
Slots and Grooves
Defects during/post compaction operations

Inhomogeneous strain fields

Mold ejection - cohesion
Macro/micro defects
Typical Compacting Pressures for Various
Metal and Ceramic Powders
Isostatic Pressing

•Pressure: 400MPa
•( up to 1000MPa)

•Hot isostatic pressing:

compaction + sintering
Cold isostatic compaction has following advantages:
1. Uniform density of compacted bodies.
2. High green density, about 5–15 per cent higher than that achieved with die
compaction at the same pressure.
3. High green strength and good handling properties of the powder body.
4. Reduction in internal stresses.
5. Possibility to compact powder without binding or lubricant additives.
6. Possibility to compact bodies having complex shapes or with a large length
to cross-section ratio and achieve a high, uniform density.
7. Composite structures can easily be obtained.
8. Low tool costs through the use of rubber or plastic moulds.
9. Low material and finish machining costs.

Some disadvantages are:

1. Dimensional control of green compacts is less precise than in rigid die
pressing
2. The surfaces of isostatically pressed compacts are less smooth.
3. In general the rate of production in isostatic pressing is considerably lower.
4. The flexible moulds used in isostatic pressing have shorter lives than rigid
steel or carbide dies.
Compressibility is a measure to which a powder will
compress or densify upon application of external pressure.
Compressibility is reported as the density in g/cm3, rounded to
the nearest 0.01 g/cm3, at a specified compaction pressure, or
as the pressure needed to reach a specified density.

Compressibility of the powder is influenced by factors like:

inherent hardness of the concerned metal or alloy, particle
shape, internal porosity, particle size distribution, presence of
nonmetallics, addition of alloying elements or solid lubricants.
Compression ratio: It is the ratio of the volume of loose
powder to the volume of the compact made from it.

A low compression ratio is desirable because of following

reasons:
– Size of the die cavity and tooling can be reduced
– Breakage and wear of tooling is reduced
– Press motion can be reduced
– A faster die fill and thus a higher production rate can be
achieved.
Green strength is promoted by:
– increasing particle surface roughness, since more sites are
available for mechanical interlocking;
– increasing the powder surface area. This is achieved by
increasing the irregularity and reducing the particle size;
– decreasing the powder apparent density.
– decreasing particle surface oxidation and contamination;
– increasing green density (or compaction pressure);
– decreasing the amount of certain interfering additives. For
example, the addition of small alloying elements, such as soft
graphite to iron and lubricant, prevents mechanical interlocking.
Powder densification-compaction pressure (P) relations
used to characterise the densification mechanism
 Other compacting processes

• Rolling
• Forging
• Extrusion
• Injection Molding
• Pressureless compaction
• Ceramic molds
Powder Rolling
The roll compaction operation can be
divided into three distinct zones:
1. The free zone where blended powder
in the hopper is transported freely
downward under gravity. Here all the
usual criteria of hopper flow apply.
2. The feed zone where the powder is
being dragged by the roll surface into
the mill bite, but has not yet attained
coherence.
3. The compaction zone close to the roll
nip, where the powder becomes
coherent, the density changes rapidly
and air has to be expelled.
 Or
nip angle
The powder characteristics have the following effect on powder rolling:

Particle Shape: The generation of maximum ‘green’ strip strength to withstand

the rigours of handling through the process line require the particle shape to be
very irregular.

Compressibility: Good compressibility is required to ensure that sufficient

particle interlocking takes place to give adequate ‘green’ strip strength. Good
green strip has a density of at least 80/85 % theoretical. Compressibility is also of
importance in determining the limiting dimensions of the roll compaction mill.

Particle Size: The thickness of the finished strip and particle segregation
severely restricts the maximum particle size which can be tolerated in the powder
feed to the compaction mill.

Flowability: The powder must flow smoothly and quickly through hopper
systems with minimum tendency to stick slip or bridging.

Surface Oxidation: This plays a significant part in determining subsequent

powder behaviour.
 Powder Extrusion

Screw extruder

Ram extruder
Advantages
 The formation of complicated cross sections
 The small amount of binder/liquid added to the solids
The ability to shape very hard powders
A uniform density distribution
The construction of long, thin sections
Competitive capital and operating costs relative to other processes

Disadvantages
The final structure is dependent on the powder properties.
The strength is not imparted during the extrusion process itself.
Structural defects may be introduced.
Structure or strength are not generally adjustable by changing the
extrusion conditions.
Binder and rheology modifiers can adversely affect product
properties, and the rate at which the binder and rheology modifiers
can be removed from the extrudate is slow.
POWDER INJECTION MOLDING (PIM)
Or
Metal Injection Molding (MIM)
 POWDER INJECTION MOULDING (PIM)
Utilizes pressurized injection of suitably designed liquid slurries containing fine powders into
prefabricated water-cooled dies. Powder injection-moulding (PIM), used to make both ceramic
and metal parts, combines the knowledge and experience gained in plastics injection-moulding
with that in sintering of ceramic and metal powders. The feed material in PIM consists of nearly
40% polymer binders and 60% metal or ceramic powders. The binders and the powders
are mixed in a hot extruder to create the feed material for injection moulding. The feed material
is heated to about 150C above the glass transition temperature of the plastic binders, injected
into a water-cooled die under 30-100 MPa pressure, and allowed to solidify. The part is ejected
and transferred to a debinding system, where the major portion of the binder is removed. The
binder system used in powder injection moulding is actually a combination of a major binder
(polystyrene, paraffin, cellulose, etc.) and a minor binder (e.g., liquid epoxy). The major
binder should burn out at a lower temperature and provide pore channels for escape of gas
produced on the decomposition of the minor binder. The minor binder provides strength
while gaseous products from the major binder diffuse through the low-permeability structure.
Ash content and carbon residue after burnout are important considerations in selecting
the binder systems. Frequently, plasticizers (petroleum oil, stearic acid) are added to
control the glass transition temperature and flow behaviour of the binders, and
surfactants are added to improve the wetting and spreading of the liquid binders on the
powders to prevent interfacial void formation. Binders must be chemically inert to the
powders and easy to remove during debinding. They should have good thermal conductivity to
facilitate the solidification of the slurry in water-cooled dies (conductivities in the range 2.3-2.7
W/m/K are normally acceptable). Debinding creates a highly porous part in which powder
particles are held together only with the aid of the minor binder. Debinding is done by thermal
treatment (slow bake), dissolution in a solvent (e.g., heptane), or catalytic removal in which
nitric acid (or oxalic acid or formaldehyde).
POWDER INJECTION MOULDING (PIM)
POWDER INJECTION MOULDING (PIM)

Feedstock
Powders
Binders
Tooling
Molding
Debinding
Sintering
Final Processing

Advantages

*High production rates

*Design flexibility
*Repeatability within tolerances
*Can process a wide range of materials
*Relatively low labor
*Little to no finishing of parts
*Minimum scrap losses

Disadvantages

*High initial equipment investment

*High startup and running costs possible
*Part must be designed for effective molding
*Accurate cost prediction for molding job is difficult
 Slip/slurry Casting

In this method, a low-viscosity slurry (typically from 10 to 50 Pa ·

s) is prepared with a liquid carrier and powder. The slurry mixture
is then poured into a porous mould usually fabricated from plaster
of paris. The carrier is evaporated and absorbed into the porous
mould, and a free standing shape is thus achieved. In the case of
cements, a chemical bond can be created during the drying or
curing process. For many powders, sintering is required to
achieve particle bonding and to produce a part having useful
mechanical properties. This process is more applicable to ceramic
powders, and the most popular application is the production of
ceramic bathroom fixtures. Slip casting is not commonly used for
metal powders. For steels, the largest application is rapid
fabrication of prototype shapes and pilot tool steels. Slip casting is
very cost effective for large shapes due to inexpensive tooling.
 Slip/slurry Casting

Sequence of operations in slip-casting a ceramic part. After the slip

has been poured, the part is dried and fired in an oven to give it
strength and hardness.
 Extruding and Jiggering

(a) Extruding and (b) jiggering operations.

 Powder Forging
In powder forging, a preform shape is cold pressed to between 75 and 85% of full
density, sintered, heated to a forging temperature, and then forged in trapped dies
using one blow to produce a fully dense net or near-net shape. The sintering step
is optional, but it is normally included as a particle surface cleaning step
(deoxidation) and to improve the workability of the porous preform. Normally,
powder forging is performed hot (1000 to 1200 °C, or 1800 to 2200 °F, for steel
powders), but it can also be conducted at warm or cold forging temperatures.
Typical steel powder forging pressures are 550 to 950 MPa. Because the
workability of a porous preform is poor, the design of the preform is critical to the
process in terms of avoiding defects. Local surface tensile stresses and
internal hydrostatic tension must be avoided. Nonetheless, with a correct
preform shape and a well controlled process, powder forged parts have sound
microstructures, good hardenability, and performance that meets or exceeds cast-
wrought part performance.
There are two classes of forging practice. In repressing, the preform shape is
nearly identical to the forged shape.
In true forging, considerable shear deformation is involved since the preform is
different in shape from the forging.
The dynamic properties of toughness and fatigue resistance are higher for forged
parts than for repressed parts.
Powder Forging
Capabilities Available from P/M Operations
Hot-pressing

Pseudo-HIP
 Hot isostatic pressing (HIP)

•Common condition: 100MPa at 1100oC: 100% density, good metallurgical

bonding, good mechanical properties
•Relatively expensive  superalloy components
 Sinter-HIP
• Sintered metals ~ 92% density is
sufficient to ensure that open porosity
at surface has been eliminated 
HIPed to full density.

• This process start from sintering then

high pressure argon is introduced or
vacuum sinter followed by HIPing in a
separate apparatus for hard metal
cutting tools.
Criteria for Selection of Powder Processing Route