Powder Characterization 2.

Particle Size and Distribution

Metal powders are produced by a variety of methods,
each method providing different particle morphology.
There are essentially six methods for metal powder
production. These are:
(i) atomization of liquid metal using water, nitrogen,
argon or a combination of these. Easily oxidizable
metals are atomized using inert atmosphere
(ii) reduction of metal oxides in hydrogen or using
carbon. These metal oxides could be materials such as
iron ore or iron oxide generated from pickling plants
in steel strip mills
(iii) reduction of metal oxide with higher carbon-
containing metal powder
(iv) mechanical milling of metal turnings or tailings
(v) chemical decomposition of metal carbonyls
(vi) electrolytic processing of cathodic deposition
from molten metal salts.
Each of these processes produces powder with
different particle shapes. Figures 1 and 2 show powder
morphology of metal powders produced by these
processes.
The characterization of metal powders involves
studying particle size, particle size distribution, surface
area, flowability of the powders, apparent density, tap
density, compressibility, and green strength. The
following is a brief review of powder characterization
methods employed in the powder metal industry.
1. Particle Shape
Particle shape is greatly influenced by the production
method employed and subsequent processing of the
powder. Particle shape influences powder packing,
powder flowability, green strength, and, in an indirect
way, the sintering of compacts made from these
powders. Table 1 lists typical particle shapes and a
brief description of each shape. In uniaxial compaction
of powders, spherical powders are seldom used.
Irregular-shaped particles are typically used as they
tend to interlock and form a cohesive compact when
they are compacted.
Particle size and particle size distribution are im-
portant to characterize metal powder. The size of a
nonspherical particle is often difficult to define. While
spherical particles are described by their diameter,
irregular particles have to be approximated to an
equivalent sphere diameter when automated tech-
niques using light, laser, x-ray or other optical
methods are used. The definition of particle size is
given in Table 2. There are several techniques available
for measuring particle size and these are described
below.
2.1 SieŠe Method
Sieves are mesh made of metal, fiber, or cloth,
assembled to provide defined openings. Sieves are used
to screen and separate powder into various size
fractions. Generally, particle sizes larger than 250
micrometers are unsuitable for the P\M (Powder
Metal) process. Sieves with different opening sizes are
stacked and powder is allowed to percolate through
various screens. Mechanical vertical tapping and
lateral motion assist the screening operation. The
finest powder fraction is collected in the bottom pan.
The residue on each of the screens represents a particle
size above the maximum opening in the sieve. The
residue can be weighed and the statistical diameter of
the particle can be calculated using the formula shown
in Table 3.
Certified sieves are selected from American Society
for Testing and Materials (ASTM) Specification E-11
and International Standard Organization (ISO) Stan-
dard 565. A typical cloth wire used in mesh screens has
variations that can be calibrated using certified glass
beads from National Institute of Standards (NIST).
Certifying each screen is time consuming and hence a
master set is used as a reference. Particle size dis-
tribution is reported as a mean and a particle size
range. The residue on each screen in a stack of sieves is
weighed and plotted as a function of screen opening
size in logarithmic scale on x-axis and weight percent
on y-axis. Another form of plotting the data is to

Table 1
Definition of particle shape.
Type Description
Acicular Needle shaped
Angular Sharp edged or having roughly polyhedral shape
Crystalline Freely developed in a fluid medium of geometric shape
Dendritic Having branched crystalline shape
Fibrous Regularly or irregularly thread like
Flaky Plate like
Granular Having approximately an equidimensional irregular shape
Irregular Lacking any symmetry
Modular Having rounded, irregular shape
Spherical Global shape

1
Powder Characterization

Atomization
Using Water Using Gas

Iron 1,000X Copper 1,200X

Reduction
of Iron Oxide of Iron Ore

500X 500X

Figure 1
Morphology of metal powders made by various manufacturing processes (Atomization\Reduction).

Table 2
Definitions of particle size (after Allen 1975).
Symbol Name Definition
ds Surface diameter The diameter of a sphere having the same surface area
as the particle
dv Volume diameter The diameter of a sphere having the same volume as
the particle
dd Drag diameter The diameter of a sphere having the same resistance
to motion as the particle in a fluid of the same
viscosity and at the same velocity
da Projected area diameter The diameter of a sphere having the same projected
area as the particle when viewed in a direction
perpendicular to a plane of stability
df Free-falling diameter The 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
dSt Stokes’ diameter dSt l Ndv$\dd The free-falling diameter in the lamina flow region
(Re 0.2)
dA Sieve diameter The width of the minimum square aperture through
which the particle will pass
dvs Specific surface diameter dνs l dν$\ds# The diameter of a sphere having the same ratio of
surface area to volume as the particle

present cumulative finer percentages on the y-axis and
particle sizes on the x-axis on a logarithmic scale. Sieve
analyses are carried out using procedures in standards:
ASTM B214-99 (Standard Test Method for Sieve
Analysis of Metal Powders); ISO 4497 (Metallic
Powders-Determination of Particle Size by Dry Siev-
ing); ISO 2591 (Test Sieving Part 1—Methods Using
Test Sieves of Woven Wire Cloth and Perforated
Metal Plate); MPIF-05 (Metal Powder Industries
Federation, Method for Determination of Sieve
Analysis of Metal Powders).
Obtaining a representative sample of powder from a
lot for analysis is always difficult due to segregation of
fine and coarse powders during the packaging of the

2

Electrolytic
Iron 390X
Carbonyl
Nickel 10,000X
Figure 2
Morphology of metal powders made by various manufacturing processes (Electrolytic\Carbonyl).
metal powders. Standards have been established to
assist in procuring representative samples: ASTM B-
215-96 (Standard Practices for Sampling Finished
Lots of Metals Powders); ISO 3954 (Powders for
Metallurgical Purposes—Sampling); MPIF-01 (Meth-
od of Sampling of Finished Lots of Powders). It is
important to note that accurate sampling requires the
collection of numerous small in-process samples from
the entire lot. Various practical methods of sampling
have been devised: scoop sampling; cone and quarter,
where a conical heap of powder is cut into four
quarters and recombined and repeating the step; chute
rifler, where flowing powder is divided into two halves
which can be further divided until a required sample is
reached; and rotary rifler, where a stream powder is
divided and placed in rotating bins. Table 4 lists the
error in each of these techniques.
Although the sieve method is widely used for
particle size determination, there are a variety of other
methods available. The sedimentation technique uses
Stokes Law, which states that the time of fall of a
particlethroughaviscousmediumisproportionaltothe
particle size and its density. A light or x-ray beam is
passed through a tank containing dispersed powder.
The collimated beam passing through the powder is
collected and the intensity measured over time is a
measure of particular particle sizes of specific times.
Centrifugation in conjunction with sedimentation
analysis is used to speed up the process.
Powder Characterization
Copper 2,400X
Iron 8,000X
Light scattering or laser diffraction techniques
measure particle size on the principle that suspended
particles in a collimated light beam will scatter the
light in a conical diffracted pattern that is related to
the particle size. The scattering information is ana-
lyzed using a microprocessor assuming a spherical
model. Fraunhofer diffraction theory is documented
by Allen (1983).
The Electrozone technique, also called the Coulter-
Counter method, uses disturbances in an electric field
when a particle passes through an aperture. These
disturbances are caused by the volume of a particle.
Changes in resistance of the medium can be correlated
to the particle size.
Microscopy, although a direct method of measuring
particle size, is tedious and complicated due to
problems associated with representative sampling.
Typically, powder is dispersed in a solvent and
spread on microscopic slides and examined. Particles
are counted. An automated image analysis system
attached to a microscope can count the particles
effectively.
Proton correlation microscopy measures fluctu-
ations in light intensity due to Brownian motion or
electrophoretic mobility of particles suspended in a
liquid. This technique is useful for particle size in the
range of 0.003 µm to 5 µm.
The Optical Sensing Zone technique utilizes light
blockage of particles moving through a sensing zone.
3
Powder Characterization

Table 3 Table 5
Statistical diameters of powder particles (after Allen Particle size analysis methods.
1975).
Useful range
nd Standard Measurement type (µm)
Arithmetical average dav l
n ASTM B214 Sieve analysis 30–1000
ISO 4497
nd # MPIF 05
Mean diameter (length) dl l
nd ASTM B 430 Turbidimetry 0.01–500
ISO 10076
Mean volume diameter dν l p$ nd $
n
ASTM B761
ISO 10076
X-ray sedimentation 0.1–300

Mean surface diameter ds l p d #

n
ASTM B822
ASTM B330
Light scattering
Permeametry
0.1–2000
0.2–50
ISO 10070
nd $ MPIF 32
Mean volume-surface diameter dss l
nd# ASTM E20 Microscopy 0.2–75

nd %
Weight-mean diameter dω l
nd $ persing metal powder. There are several other tech-
niques for particle size measurement. Air classification
Where n l number of particles in a mass of powder; d l the diameter
of the n particles.
by centrifuge is also a common method employed.

Table 4
Comparison of sampling methods.
Standard deviation
Cone & Quarter 6.3
Scoop 5.7
Chute rifler 1.0
Rotary rifler 0.2
Particle sizes ranging from 0.2 µm to 1000 µm can be
measured.
The Field Flow Fractionation technique separates
particles according to their flow resistance in a
chromatographic flow column. Particles are counted
as they exit the column. As in the case of sedi-
mentation, this technique requires single density
particles.
The Gas (Air) Permeation technique utilizes the
principle of a permeating gas of known flow rate
through a packed powder bed and the pressure drop is
measured to determine the permeability. The surface
area of particles is related to the permeability and the
surface area is converted into an equivalent specific
surface diameter. This technique gives an average
particle size but does not correlate with mean particle
size measured using the dispersion techniques de-
scribed above. A well-known gas permeation instru-
ment is a Fisher-Sub Sieve Sizer.
Table 5 lists a summary of particle size analysis
methods and Table 6 lists the cost of typical units and
analysis time.
In the dispersion techniques mentioned above,
dispersion of metal powder particles is important to
separate individual particles during measurement.
ASTM Standard B 821-91 details techniques of dis-
3. Surface Area
% Error
The surface area of powder particles can be measured
19.2 by the permeation technique or by the BET
19.6 (Braunauer–Emmett–Taylor) method, which meas-
3.6 ures gas adsorption on powder surfaces. Specific
0.7 surface area is calculated from the required amount of
inert gas to cover the surface and the area of the
molecule of adsorbate. The specific surface areas of
water atomized and sponge powders are roughly
0.1–0.12 m# g−" and 0.1–0.2 m# g−", respectively. Al-
though surface area is a useful tool, it is rarely used in
the characterization of metal powders.
Particle shape, size and distribution are important
characteristics that define powder. These properties
affect various other parameters used in the compaction
process for the production of powder metal parts.
Discussed below are powder characteristics that are
most utilized in the P\M industry.
4. Apparent Density
In the compaction process, a known volume of powder
is admitted into a die cavity and this volume is closely
monitored to ensure that each compacted part has
nearly the same weight (dimensions). Apparent density
is a useful powder characterization parameter to
achieve this goal. Apparent density is a ratio of the
mass of loose powder to its volume. A precisely
machined cup fixes the volume and a free-flowing
powder fills the preweighed cup to the brim. The
powder is leveled with a nonmagnetic straight edge
and the cup is weighed with the powder. Apparent

4
 Powder Characterization

Table 6
Analysis times and instrument costs for various particle size analysis methods
(source: Pohl M, Horiba Instruments Inc., Irvine, CA).
Method Analysis time Instrument cost ($)
Sieving 15–45 minutes 500–5000
Microscopic examination 1 hour–several hoursa 500–150,000
Zone sensing 10–20 minutes 15,000–30,000
Elutriation 10–30 minutes 500–10,000
Gravity sedimentation 5 minutes–several hoursb 1,000–35,000
Centrifugal sedimentation 5–30 minutesb 10,000–40,000
Centrifugal classification 5–25 minutes 500–5000
Hydrodynamic chromatography 20–30 minutes 30,000–40,000
Gas permeability 10–20 minutes 50–5000
Gas adsorption 10–15 minutes 5000–50,000
Brownian motion 10–30 minutes 20,000–35,000
Mercury intrusion 30–45 minutes 15,000–45,000
Cascade impaction 10–20 minutes 2,000–20,000
Notes: a Depending on the number of particles being counted. b Depending on sample density and size.

the commercial compaction of actual parts. ASTM B-

703 and MPIF-48 Standards address this issue by
describing a device that simulates production con-
ditions. This device, an Arnold meter, consists of a
steel block of 20 cm$ simulating a die (see Fig. 4) and is
16 microinch (4i10 –7 m) finish or better
placed on a wax paper. A brass bushing is filled with
(3.18 ± 0.13 mm)

powder to three-quarters of its height. The bushing is

0.126 ± 0.005”

30°
moved forward over the hole with a twisting motion
on the forward pass and slowly moved back, allowing
0.100 ± 0.003”
the steel block to fill with the powder. The weight of
(2.54 ± 0.05 mm) the powder in the steel block is measured and the
apparent density is calculated.

Figure 3
Hall flow meter.
5. Tap Density
density in g cm−$
is calculated by dividing the mass of Tap density is the maximum density achieved when
the powder by the volume of the cup. There are four metal powder is vibrated or tapped under specific
different ASTM methods which are applicable: B-212; conditions. MPIF-46 test method standard is used.
B-329; B-417; and B-703. B-212 and MPIF-04 are ASTM B-527 and ISO 3953 also describe the
most widely used for free-flowing powders and a procedures for tap density measurements.
typical setup is shown in Fig. 3. In the manufacturing process of making powder
Figure 3 is referred to as the Hall flow meter. A metal parts, pure metal powders are mixed with
preweighed amount, 50 g, is placed in the cup with a alloying ingredients such as copper, nickel, graphite,
precise orifice; a finger covers the orifice. As the finger ferroalloys, and lubricants. These premixes can also be
is removed, a stop clock measures the time required for tested for flow and apparent density by the above
the powder to flow through the orifice. Atomized iron methods.
powders have a flow of 22 s to 26 s with an apparent The particle size and morphology of additives
density in excess of 2.8 g cm−$. In instances where the influence both apparent density and flow. Lubricants
powder is not free flowing, the orifice is made twice the can influence interparticle friction and change the
diameter of Hall flow meter and the instrument is then apparent density. The particle size and type of lu-
called a Carney cup. MPIF-28 Standard, ASTM bricant used will affect flow and apparent density
6-417, and ISO 3923\1 describe the procedure for this differently. A new technology developed during the
measurement. Flow of powder is dependent on inter- 1990s called Binder Treatment Technology improves
particle friction and powder surface area. Fine flow and increases apparent density by binding finer
powders have higher flow rates than coarser powders. particles to larger base metal powder.
Powder morphology also plays a key role. Other important parameters for the characteriz-
Although useful, Hall flow and apparent density ation of metal powder are green strength, green density
measurements often cannot be correlated directly with and compressibility.

5
Powder Characterization

Dimensions shown in millimeters (inches). 7. Green Strength

165.1
[6.5]
44.45 DIA.
The green strength of a powder is important in-
1.6 [0.083] 45° (4X) 82.55
[3.25]
[1.75]
formation that allows parts manufacturers to assess
the degree of difficulty in handling the pressed part

[1.35]
31.75
through various automated devices, and the ability of

[2.5]
13.5
a part to withstand green expansion when the parts are
ejected from the die. Green strength is affected by

[0.375]
30.1 DIA.
31.6640 ± 0.0025 [1.5]
particle shape, particle size, and particle hardness.

9.5
[1.241 ± 0.0001]

[0.25]
6.35
0.8 ± SWIP (BOTH ENDS) Spherical powders have poor green strength when

[1.0000 ± 0.0001]
[6.031]
uniaxially compacted, whereas irregular shape allows

[1.0]
27.4 ± 1.0125

58.1
NO.
better interlocking between particles and increased
green strength. Particle size influences green strength
[0.25]
6.35

PART NO. 1 PART NO. 2

NOTE: BREAK ALL EDGES
EXCEPT NOTED, MATL: TOOL STEEL, HARDENED
MATL: BRASS since fine powders have a tendency to bridge during
0.8i45° [0.031] TEMPERED 60 HRC MIN
GRIND ALL OVER DEMAGNETIZED compaction or introduce local restriction of particle
movement. Lubricants used in the compaction process
Figure 4 can alter green strength and compressibility.
Arnold apparent density meter. During the compaction process, powder particles
are coated with lubricant to prevent particle to particle
6. Green Density and Compressibility contact until such compaction pressure is reached, at
which the lubricant either extrudes to the die wall or is
The compressibility of metal powder determines the
trapped in the pores formed between particles. There is
green density that can be achieved at a given com-
a transition pressure below which the lubricant facili-
paction pressure. Compressibility is dependent on
tates particle movement by reduced friction and above
particle shape, particle density, particle hardness,
which the lubricant is trapped in the pores, making
chemical composition, and, to a degree, particle size.
further compaction of powder particle difficult. Above
A smooth surfaced powder results in higher com-
the transition pressure, the lubricant behaves like an
pressibility as the pores created during the compaction
incompressible fluid. Although lubricants generally
are essentially between particles. An irregularly shaped
reduce green strength, recently developed lubri-
particle can fold on itself creating porosity that cannot
cants provide increased green strength by increasing
be removed by further compaction, resulting in lower
polymer–polymer bonding.
green density. Particle density is higher for atomized
Green strength is measured using standard proce-
powder when compared to a chemically reduced
dures described in ASTM B 312-96, MPIF-15, or ISO
powder, as the latter tends to be spongy. More internal
3995. The powder to be tested is compacted to a
porosity is present in a sponge iron particle than in
rectangular shape and the green (unsintered) bar is
atomized iron powder and this porosity cannot be
broken in a three-point bending fixture. A load is
entirely removed during compaction. Hence, the den-
applied in the middle of the bar supported on two
sity of compacted sponge particles will be lower than
sides. Green strength is calculated using the flexural
less porous atomized particles.
formula:
Particle hardness should be as low as possible to
allow conforming of particles to their neighbors.
Purity of the powder can play a role in reducing 3PL
Sl
compressibility as the hardness of a particle can 2t#W
increase due to elements in solution. Surface oxides
can prevent effective particle to particle contact, where S l Green strength is pounds per square inch
making compaction more difficult. MPIF Standard 45 (Newtons per square millimeter); P l force in 1 bf (N)
and ASTM B 331-95 describe the procedure for required to rupture; L l length of speacimen in inches
measuring compressibility of metal powders. This test (mm); t l thickness in inches (mm); and W l width of
method consists of uniaxially compacting a sample of the specimen in inches (mm).
metal powder in a confining die and measuring the
density of the ejected part. Compaction is done at
different compaction tonnages to generate green den-
8. Chemical Properties
sity versus compaction tonnage plots. This plot is
called a compressibility curve, useful information in The chemical properties of metal powder are de-
setting up presses to make parts to a specified density. termined by conventional analytical procedures:
Green density is measured by the Archimedes prin- atomic absorption; X-ray fluorescence; and wet chem-
ciple. Green parts are oil impregnated before the ical methods. These provide information on residual
density is measured. MPIF Standard 42, ASTM B 328, impurities and chemical composition of the powder.
and ISO 2738 describe the procedure for the measure- The most important parameter for metal powders is
ment of density. oxygen content, which can be chemically combined

6
 Powder Characterization

Table 7
A typical powder characteristic for atomized iron powder (Ancorsteel 1000B) and
sponge iron powder (Ancor MH-100).
Ancor MH-100 Ancorsteel 1000B
Apparent density, g cm−$ 2.55 2.93
Flow rate, g (50 g)−" 30 26
Chemical analysis (w\o)
Mn – 0.13
Ni – 0.03
Mo – –
C 0.01 0.01
O – 0.14
Hydrogen loss 0.21 –
S 0.009 0.016
P – 0.009
Cu – 0.09
Screen analysis (w\o)
Microns (mesh size)
j250 µm (j60) Trace Trace
k250\j150 µm (k60\j100) 10 13
k150\j45 µm (k100\j325) 69 67
k45 µm (k325) 21 20
Green properties (measured with a 1.0 w\o zinc stearate lubricant addition)
Green density, g cm−$ 6.47 6.83
Compacting pressure, MPa (tsi) 410 (30) 410 (30)
Green strength, MPa (psi) 19 (2560) 11 (1650)

and\or on the surface of metal particles. This is Bibliography

measured and reported as hydrogen loss for reduced
metal powder and as oxygen content for atomized
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4491\2 describe procedures for determining hydrogen
loss. Oxygen and carbon are typically measured using
a LECO analyzer. Acid insoluble oxides or silicates in
metal powders can be measured using MPIF-06,
ASTM E 196, and ISO 4496 methods.
A typical powder characteristic for atomized iron
powder (Ancorsteel 1000B) and sponge iron powder
(Ancor MH-100) is given in Table 7.
9. Summary
Typical characterization techniques for metal powders
are reviewed along with relevant standards. Particle
size measurement using the sieve method and light
scattering technique are widely used. There are a
number of techniques available for measuring particle
size and distribution, but the choice employed depends
on required measurement speeds, equipment budget,
and the size range being measured. Knowledge of
important powder characteristics such as apparent
density, flow, green strength, compressibility, and
green density is required in molding powder metal
parts. A brief description of the methods used for the
measurement of these key properties is presented.
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K. S. Narasimhan

7
Powder Characterization

Copyright ' 2001 Elsevier Science Ltd.

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Encyclopedia of Materials : Science and Technology
ISBN: 0-08-0431526
pp. 7781–7788