Lecture 5

Metal Powder Characteristics 1

Dr. Nimu Chand Reger (Assistant Professor)

Metallurgical and Materials Engineering
National Institute of Technology Tiruchirappalli, Tamilnadu
620015
28/10/2022 nimu@nitt.edu 1
 Overview

 Metal powder characteristics:

 Powder Sampling
 Scoop sampling
 Coining and
quartering
 Chute Riffler
 Spinning
Riffler
 Chemical
composition
analysis.
 Oxygen content
of the powder
 Particle shape
and size analysis
 Sieving
 Microscopic
Sizing
 Sedimentation
Method
 Turbidimetric 3
Metal powder characteristics

4
 Metal powder characteristics

 The powder characteristics influence the properties of the final product.

Powder used in are characterized by several features and each characteristics has it own influence on processing as
well as on the composition, microstructures and final properties of the product.

 Characteristics of powders can include the following

 Material Characteristics like physical and chemical characteristics. Physical
characteristics include structure, porosity and density. Chemical characteristics
include purity and composition.
 Morphological Characteristics like shape, size, texture and surface area.

 Bulk or behavioural characteristics like flow rate, apparent density, compressibility and green
strength.

Standard procedures are developed by Metal Powder Industries Federation (MPIF) and American
Society for Testing of Materials (ASTM) to determine metal powder characteristics.

4
Metal powder characteristics

Powder Sampling
 Scoop sampling
 Coining and quartering
 Chute Riffler
 Spinning Riffler

5
 1. Powder Sampling

 Powder sampling
Sampling is the first activity in the characterization of metal powders.
 Scoop Sampling
The first technique, scoop sampling, consists of inserting a scoop into a thoroughly
mixed powder in a container and withdrawing a scoopful of powder as a sample.

 Coining and quartering

 The powders are poured on to a polished sheet of aluminium in the
form of a cone.
 The cone is then flattened and split into a four equal segments, with thin
sheets of polished brass and a suitable quantity for testing is collected.

6
 Powder Sampling

 Chute riffler
The sample powder is introduced in a V-shaped trough with two powder collecting trays
placed on either side of the trough. The sample powder flows through a series of chutes
feeding into the two collection trays. This process is repeated with powder from one of the
trays until the desired amount of sample is obtained.
.

 Spinning riffler
It consists of a closed ring of containers spinning under a steady stream of powder feed
so that each container collects a series of small portions of the powder feed as it passes several
times beneath the powder feed.
8
C ont…
Metal powder characteristics

Chemical composition
 Oxygen content of the powder
 2. Chemical composition

 The purity of a powder, the type and amount of impurities indicated by compositional
analysis depends strongly on the production method.
 Electrolytic powders may contain dissolved gases (oxygen, hydrogen) as impurity.
 Many metals are strongly hardened and embrittled by even a small amount of dissolved
oxygen.

 The metal powders may absorb moisture during storage as well as handling and
form surface oxides.
(The difficulties are encountered during compaction due to the presence of oxides (compound
such as SiO2 in iron powders) which are abrasive in nature.)
 In addition, non-metallic inclusions can lead to non-uniform sintering of the compact
leading to poor dynamic properties (e.g. fatigue strength).
(In general, chemical composition refers to the percentage of the base metal in the case of pure
metals, e.g. 99.9% iron, 99.8% copper etc., which can be taken as a measure of the purity of the
metal.)
 Oxygen content of the powder

 Oxygen content of the powder

Oxygen content of powders is measured by hydrogen loss method.

To measure the hydrogen loss, a 5 g sample powder is placed in a combustion

boat and exposed to a specific period of time and temperature in an
atmosphere of dry, purified hydrogen.
The weight loss of the powder specimen due to the hydrogen exposure is
measured by weighing the original weight of boat and specimen in grams and
the weight of the boat and specimen after reduction in grams.

Standard conditions for hydrogen loss testing for different metal powders are
given in Table.

11
C ont…
Various chemical characterization method

C1o2nt
Metal powder characteristics

Particle shape analysis

 Dimensionality of the powder particle
 Surface contour of the powder particle
 3. Particle shape analysis

Particle shape can be defined as, “the recognized pattern of relationship between points that
form the external surface of the particle.”
 Particle shape analysis is a fundamental characteristic of powder particles, which
influences other parameters like flow rate, apparent density, compressibility and
sinterability.
Two different concepts used to describe and differentiate particle shapes are based on:
 Dimensionality of the particle
 Surface contour of the particle

The most common particles shapes encountered in powder metallurgy are listed in Table:
 Powder
dimensionality
and shape
classification

14
C
 Particle dimensionality and shape analysis

Microstructures of
powders having different
shapes produced by
different methods

Powder shapes: (i) rounded shape with porosity (titanium powder), (ii) spherical shape (nickel
base superalloy), (iii) porous (reduced iron). and (iv) dendritic shape (electrolytic copper).
15
C
 Particle dimensionality and shape analysis

 The particle shape plays an important role on the final properties of the component.
 For example, Irregular-shaped particles have reduced apparent density and flow rate but
good pressing and sintering properties.
 On the other hand, spherical particles have maximum apparent density and flow rate but
reduced pressing and sintering characteristics.
 Dendritic powders also have poor apparent density and poor flow rate.

 Particle shape can be determined by several methods.

Optical microscopy, Scanning Electron Microscope (SEM), Transmission
Electron Microscope (TEM) as well as image analyzer (Image J software)
are all used to evaluate particle shape.

16
C
Metal powder characteristics

Particle size analysis

Sieving
Microscopic Sizing
Sedimentation Method
Turbidimetric Method
Elutriation

Coulter counter and particle analysis by light observation

Laser light Scattering
 4. Particle size analysis

 Particle size can be defined as, “the total space occupied by a powder particle.”
The particle size has a great importance in powder metallurgy because it affects some of the
important properties such as green strength, density of compact as well as agglomeration,
porosity, expulsion of trapped occluded gases, dimensional stability, flow and mixing
characteristics.
 Fine metal powders result in poor apparent density, poor flow rates and maximum
sinterability while coarse powders give good apparent density, good flow rate but
minimum sinterability.
 It is possible to maintain a narrow size distribution by close control of process
parameters; however, it is not possible to have a single particle size in a powder lot.

Majority of metal powders used in PM industry vary in size between 4 and 200 μm
Particle size analysis
C20
 Particle size analysis

 Among the different particle sizing techniques,

 Sieve analysis is a cheap and efficient method capable of accommodating a wide
size range of particles ranging from 5 to 1,000 microns.
 Sedimentation technique gives size distribution by measuring the settling velocity of
powders in water. (This method is used for classification of very fine powders).
 Coulter counter measures conductivity of powders suspended in a non-
conducting liquid.
 In laser light scattering analysis, the particles are dispersed in water. Size is determined
by the light scattering from each particle as it passes through a detection zone.
(Particle size can also be measured indirectly from the surface area of the powders).
(Surface area gives no information about the distribution in particle size
or other differences between powders).
 The two main analysis techniques for measuring surface area are, gas adsorption
and gas permeability.

C21
 4.1 Sieve analysis

 Sieve analysis is the most widely used method of determining particle size distribution of
metal powders.
 Sieve analysis for particle size relies on a stack of screens with decreasing openings that
classify particles based on size. (Woven-wire-cloth sieves made of copper, brass, bronze,
nickel and stainless steel (and recently nylon) with square mesh pattern are used
commonly).
 The standard step is an opening that changes by almost a constant factor
21Τ4 ,
indicating a step size of 21Τ4 between each mesh.
For example, the ratio of the 60-mesh opening size to the 70-mesh opening size
(250-212 μm) is 1.18, the ratio of 170-mesh opening size to the 200-mesh opening size (90-75
μm) is 1.20 and the ratio of 325-mesh opening size is to 400-mesh opening size (45-38 μm) is
1.18.

23
Sieve analysis (Standard Sieve Sizes (US)

C24ont…
Sieve analysis
 The sieves are stacked with largest mesh
size at the top and a pan at the bottom.
(An appropriate sample weight of metal powder
(100 g) is spread on the top sieve which is then
closed).
 The stack of sieves is agitated for a
specified period of time by one or more of
methods such as manual vibration,
gyratory motion with tapping, mechanical
shaking, mechanical-cum-electromagnetic
vibration, accelerating air column or
vacuum.
 Care is taken to avoid clogging of the sieve
openings by the powder particles.

 The powder fractions remaining on each

Fig. Sieve analysis for particle sizes sieve and the bottom pan are weighed
relies on a stack screen with decreasing separately and reported as % retained or
openings. passed by each sieve.
25
 Sieve analysis Cont…

Fig. Sieve analysis for particle size

measurement: the larger particle is retained
in the sieve, while the smaller particle passes
through.

 The powder passing through a particular mesh is designated by a minus (-) sign, and that
retained on a mesh is designated by a plus (+) sign.
 Sieve analysis is usually applied only to particles having sizes greater than 325 mesh or 44
μm, although there are now screens with smaller openings. Special sieves known as
micromesh sieves having accurate opening down to 5.5 nm have been introduced for
subsieve particle size analysis.
For example, the designation of -120/+230 mesh for a powder indicates that it passed
through a 120 mesh opening but not through a 230 mesh opening. The size of the powders
26
would be in the range between 125 and 63 µm.
 Sieve analysis (Particle size distribution)

Histogram showing typical particle

size distribution in a (iron) powder
sample is given in Figure.

 The histogram is generated by plotting the incremental weight percentages of the total
powder mass versus the screen opening size on which the powder was collected.
(In such plots, the mode is the peak or most frequent particle size, ~140/ +200 mesh (106 to 75
microns) in this case).

C26
 Sieve analysis

 This is generated by adding the percentages accumulated in each interval. The cumulative
sum (as a percentage of the total) is plotted against the upper particle size for the interval.
It is commonly provided by the automated size analyzers.
 This results in a smooth cumulative particle size distribution, showing the amount of
powder smaller than any given size.
 Most important is the median size that corresponds to the particle size at the 50%
value.
Cumulative size analysis curve is also commonly used to represent sieve analysis data.

Representation of
sieve analysis
results.
(i) Relative
size
distribution,
(ii)Cumulative size
distribution of
particles
C27
 Sieve analysis (Different types of particle size distributions)

Different types of particle size distributions: (i) unimodal, (ii) bimodal, and (iii) broad band.
 One reason for new size analysis tools is the large degree of error associated with the
technique. Variation up to 20% is reported in particle size due to differences in sieves,
techniques, screen damage, and even operators.
 Usually, the manufacturing tolerances allow for at 4% variation on the opening sizes for the
small mesh numbers.
(For example, a 35-mesh sieve having a size of 500 μm can range from 480 to 530 μm, but the
allowed variation increases to nearly 7% at high-mesh numbers (at 325 mesh, where the
opening can range from 42 to 48 um). Consequently, screen or sieve analysis is no2t9 very
accurate.
Sieve analysis (Video) https://www.youtube.com/watch?v=AM-NrQoRIYY
 4.2 Microscopic Method

 Microscopy is the most definitive method of particle shape and size analysis, as it involves
actual counting of individual particles on a slide containing a sample of powder.
(Though this is a tedious and time-consuming process, it is the most reliable and
standard method for checking the accuracy of other methods.)
 Optical microscope is used for particles ranging from 100 to 0.1 µm.
 Scanning Electron Microscope (SEM) is used for particles ranging from 10 µm to 0.01 µm.
 Transmission Electron Microscope (TEM) is used for particles in the range 10 µm to
0.0001 µm.
 Observation of the powder particles by SEM and TEM, though may not be used for
quantitative purposes, is generally very useful since these allow examination of individual
particles which can reveal features not given by other methods
orfnokyurdiatten
onit