Table of Contents

Definition of powder..................................................................................................................2
Powder size measurement techniques (optional explained in chapter 2)...................................3
Laser Diffraction....................................................................................................................3
Chapter 02..................................................................................................................................3
Powder Sampling.......................................................................................................................4
a) Agglomerates and aggregates........................................................................................4
b) Dispersion......................................................................................................................5
c) Particle size measurement..............................................................................................6
Particle size measurement techniques........................................................................................9
Microscopy.............................................................................................................................9
Screening..............................................................................................................................10
Sedimentation.......................................................................................................................12
Light scattering and diffraction............................................................................................13
X-Ray Techniques................................................................................................................14
Comparison of different techniques.....................................................................................16
Data analysis............................................................................................................................17
Surface and Surface area..........................................................................................................19
Gas adsorption surface area analysis................................................................................20
Visualization of particle size distribution........................................................................22
Ball milling...............................................................................................................................23
Principle...........................................................................................................................24
Types................................................................................................................................24
The powder metallurgy and particulate materials process, commonly abbreviated as P/M 2 to
shape different bodies like casting but different roots are adopted. Casting is usually applied
to low melting point metals, but powder techniques are applied to almost all types of
materials.

Thus, many of the products created via P/M 2 are not viable through castings, such as
composites, high temperature ceramics, polymers, intermetallic compounds and cermets.

For large volume production powder economy rely on die cavities which are being replicated
over and over. Powder techniques use automation with relatively low-cost automation.

Definition of powder
Particles are discrete small divisions of solids, ranging from size of a virus to sand. Usually,
particle size is measured in microns. Mostly engineering particles size ranges between 0.1 to
200 microns with ceramics particles tending towards smaller size while plastics particles
usually have large size. A powder is a collection of particles. Powder may contain polymeric,
metallic or ceramic particles. For engineering applications, the amount, size and placement of
phases is selected to get desired properties. For example for automobile connecting rod the
powder consist of iron, copper, graphite and zinc stearate mixture.

After processing the powder is bonded in solid and individual particles lose their
characteristics. At that point, discrete crystal regions are termed as grains. So, particles
combine to form powder. Powder usually flows under the action of gravity. After sintering
the powder consist of grains which are bonded together to form solid.
Powder size measurement techniques (optional explained in chapter 2)
For reading

Laser diffraction and explanation

Sedimentation

Analysis of particle size data(optional)

Laser Diffraction

1. Sample Preparation:

o A suspension of particles is placed in a transparent chamber.

o These particles can be in a liquid or gas medium.

2. Laser Illumination:

o A laser beam passes through the suspension.

o When the laser interacts with the particles, light is scattered in different
directions depending on the particle size.

3. Scattering and Focusing:

o A lens collects and focuses the scattered light.

o The scattering pattern depends on the size of the particles.

o Larger particles scatter light at smaller angles (forward scattering).

 o Smaller particles scatter light at larger angles (wide-angle scattering).

4. Detection and Analysis:

o A detector records the intensity and angles of scattered light.

o Using Mie theory or Fraunhofer diffraction theory, a computer calculates

the particle size distribution in the sample.

Key Principles

 Scattering Angle vs. Particle Size:

o Small particles scatter at wide angles.

o Large particles scatter at narrow angles.

 Intensity of Scattering:

o Stronger for larger particles.

o Weaker for smaller particles.

 Mathematical Models Used:

o Fraunhofer Approximation: Works well for large particles (>10 µm).

o Mie Theory: Used for small particles (<10 µm), considering refractive index.

Largest & smallest particles can be measured simultaneously.

 This is because Laser Diffraction covers a wide range of sizes, with a Dynamic
Ratio of 60:1.

 Example: If the largest measurable particle is 600 µm, the smallest measurable one
could be 10 µm (since 600÷60=10600 \div 60 = 10600÷60=10).

Minimum detectable particle size:

 The smallest particle measurable depends on the wavelength of the laser and the
sensitivity of the detector.

 Typically, Laser Diffraction can measure down to 40 nm (0.04 µm).

Measurement Principle

 Particle size is determined by:

o Intensity of scattered light (brightness of the scattered signal).

o Angular extent of scattering (how far the light spreads).

  How it's detected:

o Photocells & Computers analyze the scattered light pattern.

o The data is processed using Mie theory or Fraunhofer diffraction

equations.

Key Relationships

1. Angle of Scattering θ is inversely proportional to particle size d:

o Smaller particles scatter light at larger angles.

o Larger particles scatter light at smaller angles (mostly forward).

2. Intensity of Scattered Light is proportional to the square of the particle size:

o Larger particles scatter more intensely.

o Smaller particles scatter less intensely.

5. Assumption of Spherical Particles

 The technique assumes all particles are spherical because:

o Spheres have well-defined scattering patterns that match theoretical models

(Mie scattering).

o Irregular-shaped particles introduce errors unless correction models are

applied.
Chapter 02
A particle is the smallest unit of the powder that cannot be subdivided. Generally powder
processing deals with particles that are greater than (0.01-1 microns) but smaller than (0.1 to
3 mm).
Metric: A way to measure something.

Attribute: A specific property or characteristic of something.

The way we measure the size of a particle changes depending on what we are focusing on.

For example:

 If we care about how a particle moves in air, we use aerodynamic diameter.

 If we want to know how much space it takes up, we use volume-equivalent

diameter.

 If we are measuring what size sieve it passes through, we use sieve diameter.

Each metric gives a different "size" because particles are not perfect spheres—they come in
different shapes, and we need different ways to describe them based on the situation.
 s

Powder Sampling
Few grams of powder represent whole lot. So, it must be selected without errors. Sampling
errors can be avoided by some simple rules. Whenever possible samples are taken from
moving stream, and many small samples are preferred. A major problem arises when
sampling is done after shipping or vibrations which cause the particle segregation with larger
particles at top while smaller particles at bottom. After vibrations, if any, whole lot of powder
should be tumbled, and many small samples from different locations should be taken. Then
these small samples should be mixed to form a aggregate which represents the lot. In industry
rotary rifflers are used for sampling.

a) Agglomerates and aggregates

Agglomerates and aggregates are clusters of particles that form due to different bonding
mechanisms, impacting powder characterization and processing. Agglomerates are
loosely bound particle clusters held together by weak forces, such as surface moisture or
van der Waals interactions. These clusters can be easily broken apart using mild
mechanical force or by dispersing them in a liquid. Since agglomerates cause small
particles to stick together, they can lead to inaccurate size measurements, making
dispersion an essential step before analysis.

On the other hand, aggregates are strongly bonded particle clusters formed due to
chemical forces or cementing. Unlike agglomerates, aggregates are very hard and difficult
to break apart, even with mechanical forces. This makes them more stable but also
problematic when accurate particle size distribution is required. In powder
characterization, both agglomerates and aggregates can interfere with size analysis,
leading to incorrect data representation.

Smaller particles tend to cluster together, and this can be explained through surface
energy per unit volume or Ostwald ripening. Surface energy plays a key role in particle
interactions, with smaller particles having higher surface energy per unit volume. For a
spherical particle, the energy per unit volume (E) is inversely proportional to the particle
diameter (D), given by the equation E=6γ/D , where γ represents surface energy. This
means that as particle size decreases, the tendency for agglomeration increases. This
creates challenges in powder processing, as small particles improperly measured as larger
agglomerates can affect material properties such as flowability, compaction, and
reactivity. Many industrial processes rely on accurate particle size distribution, making
proper sample preparation and dispersion essential to avoid errors in material
characterization.

b) Dispersion
Dispersion is the process of breaking apart clusters of particles (agglomerates) into their
individual components to ensure accurate measurement and characterization. In powder
analysis, proper dispersion is crucial because small particles tend to stick together due to
attractive forces like capillary forces, van der Waals forces, and electrostatic
interactions. If not properly dispersed, particle size measurements may show
agglomerate size instead of actual particle size, leading to incorrect data.

Methods of Dispersion

 Drying the Powder: Removes moisture that causes agglomeration.

 Using Dispersing Agents: Adding surfactants (e.g., hydroxyl (OH⁻), sulphate

(SO₄²⁻), or ammonium (NH₄⁺) groups) helps break particle interactions.

 Mechanical Stirring or Ultrasonic Agitation: Breaks weak particle bonds to

improve dispersion.
c) Particle size measurement

Particle size is measurement of the dimensions of the powder particles. But this
determination depends upon the measurement techniques, the specific parameter being
measured and particle shape. Particle size can be measured through various techniques
whose results necessarily matches each other because different parameters of interest.
Most techniques measured a single parameter and make assumption of spherical particle
shape. Typical measured parameters are particle surface area, projected area, maximum
length, minimum cross-sectional area or volume.
Particle size measurement techniques
Microscopy
A universal way to measure particle size is to capture an image which is subsequently
digitized or quantified. A simple approach is to overlay circles of various sizes on the particle
images, counting the number of particles of each size. This can be performed in a microscope
and today it is possible via automated image analysis. Doing this analysis by hand is tedious,
so statistically significant sizing is usually performed via computers attached to microscopes.
The image for analysis is generated by optical reflected light, transmitted light, scanning
electron, or transmission electron microscopes. The instrument choice depends on the particle
size, so microscopy can be applied to particles from a few nm to mm in size; however, the
larger depth of field in the SEM is a distinct advantage, especially since it shows surface
topography and can provide X-rays for compositional analysis. By microscopic counting of
diameter, length, height or area, a frequency distribution is generated to show the relative
frequency of each size.
The first task in image analysis is to disperse the powder. Frequently, agglomeration or
coincidence occurs, as shown in Figure 2.6, making it difficult to distinguish the discrete
particle size from the agglomerate size. Deagglomeration can be simply performed by adding
the powder to water with a drop of detergent followed by ultrasonic agitation.

Discrimination between single and multiple particles is a common problem in particle size
analysis. Counting two or more small particles as a large particle skews the distribution
toward the larger sizes. To avoid shape- and orientation-dependent particle sizes, it is best to
use parameters such as the equivalent spherical diameter based on the projected area D A.
Thus, the shadow of each particle is measured for area and that shadow size is converted into
a diameter by assuming that it came from a sphere. If at the same time the maximum and
minimum dimensions are recorded (the ratio of maximum to minimum size is the aspect
ratio), then dispersion diagrams of size versus aspect ratio can be generated. Such plots show
particles created by different fabrication techniques cluster in different regions.

Screening
Screening (Sieve Analysis)

Screening, also known as sieve analysis, is an older technique for measuring the size
distribution of larger particles. A square grid of evenly spaced wires creates a mesh.

 Mesh size: Determined by the number of wires per unit length.

 Inverse relationship: A larger mesh number (e.g., 325) means smaller openings
(e.g., 45 µm), while a smaller mesh number means larger openings.

 The number of wires per inch defines the mesh size (e.g., 200 mesh = 200 wires
per inch).

 Opening size: For example, a 200-mesh screen has a 127 µm spacing between wire
centers, with wire thickness reducing the actual opening size to 75 µm.

Sieve Analysis Process

1. Stacking Screens: A series of screens with decreasing mesh openings is stacked.

2. Agitation: The sample is placed on the top screen, and the stack is agitated for 15
minutes.

3. Weight Measurement: After vibration, the powder is weighed in each size fraction,
and the percentage is calculated.

Mesh Sign Conventions

  “-” sign: Particles pass through a given mesh (e.g., -100 mesh means the particle
passed through a 100-mesh screen).

 “+” sign: Particles are retained on a given mesh.

 Example: -100/+200 mesh means particles passed through a 100-mesh screen but
were retained on a 200-mesh screen (size between 150 and 75 µm).

 Sub-sieve powder: Particles smaller than 45 µm (-325 mesh) are termed sub-sieve
powder.

Errors in Screening

1. Mesh Tolerance: Mesh openings vary by 3-8% due to weaving inconsistencies.

2. Defects in Screens: Some openings can be 25-50% larger than specified, leading to
oversized particles being miscounted as small.

3. Screening Duration:

o Too short: Small particles do not fully pass, giving a false larger size
distribution.

o Too long: Particles break down, creating false smaller sizes.

4. Overloading Screens: Excess powder blocks mesh openings, preventing small

particles from passing.

Accuracy and Repeatability

 Repeatability (same person, same test) is good (~1% variation).

 Inter-laboratory tests show 8% variation in size results.

 Using standardized screens can reduce error to 4%, but perfect accuracy is not
feasible.

Screening for Classification

 Size classification: Screens can be used to separate size fractions for controlled
applications.

 Industrial Use: Some screens are as large as 2 meters (6 feet) for large-scale
operations.
Sedimentation
Sedimentation is a technique used for particle size analysis, particularly for smaller particles.
It relies on the principle that particles settling in a fluid (liquid or gas) reach a terminal
velocity, which depends on both particle size and fluid viscosity. This method is applicable
to particle sizes ranging from 0.02 to 100 µm.

Key Principles of Sedimentation:

1. Terminal Velocity & Stokes' Law

o Particles accelerate to a constant terminal velocity due to the balance of

gravitational, buoyancy, and viscous drag forces.

o Stokes' Law is used to estimate particle size from the settling velocity.

o The settling velocity (v) is given by: v=D2(ρM−ρF)g/18η where D is particle

diameter, ρM is particle density, ρF is fluid density, g is gravitational
acceleration, and η is fluid viscosity.

2. Types of Sedimentation Analysis

o Free-fall sedimentation (natural gravitational settling) is useful for 1-20 µm

particles in water.

o Centrifugal sedimentation is required for particles smaller than 1 µm.

o Higher viscosity fluids are needed for particles larger than 20 µm to slow
down their settling for accurate measurement.

3. Error Sources & Limitations

o Stokes' Law assumptions (immediate terminal velocity, spherical particles)

can introduce errors.

o Brownian motion affects very small particles (below 2 µm).

o Turbulence and Reynolds number effects limit the technique for particles
above ~60 µm in water.

o Irregular particle shapes can lead to inconsistent settling behavior.

4. Extensions & Related Techniques

o Elutriation: Uses a fluid flowing against gravity to separate particle sizes.

o Air Classification: Uses centrifugal force and airflow to separate particles

(typically for 1-150 µm).
Light scattering and diffraction

1. Light Scattering and Diffraction for Particle Size Analysis

 Automated particle size analyzers disperse particles in a moving fluid and pass them
through a detector.

 The detector measures changes in light scattering, electrical conductivity, or

other signals proportional to particle size.

 Errors may arise due to artificial discontinuities like bubbles.

2. Advantages of Light Scattering Methods

 They have a large dynamic ratio, meaning they can measure a wide range of particle
sizes simultaneously.
  Laser instruments using multiple detectors can measure particle size ratios as large
as 7000 to 8000.

3. Fraunhofer and Mie Scattering Techniques

 Fraunhofer light scattering (low-angle) uses monochromatic laser light and is

widely used for automatic size analysis.

 Mie scattering applies to particles smaller than 3 µm and relies on detecting light at
90°.

 The dynamic range for analysis is typically 2 nm to 2 mm.

4. Time-of-Flight and Doppler Methods

 A laser technique can track particle motion to estimate velocity, helping in

measuring particle size.

 For small particles, the Stokes-Einstein equation relates particle size to Brownian
motion.

 Doppler shift techniques analyse frequency shifts in laser reflections to determine

particle size distribution.

X-Ray Techniques
In material science, two X-ray-based techniques are commonly used to measure the size of
very small particles and crystals. These are X-ray Line Broadening (Scherrer Method) and
Small Angle X-ray Scattering (SAXS).

1. X-ray Line Broadening (Scherrer Method):

This method is based on the broadening of diffraction peaks in an X-ray Diffraction

(XRD) pattern. The peak broadening occurs due to the small crystal size, as destructive
interference becomes inefficient at angles slightly off the Bragg condition.

Bragg's Equation:

λ=2dhklsin(θ)

where:

 λ is the X-ray wavelength

 dhkl is the interplanar spacing

 θ is the diffraction angle

Scherrer Equation:

D=0.9λ/Bcos(θ)

where:

 D = average particle size

 B = Full Width at Half Maximum (FWHM) of the peak

 λ = X-ray wavelength

 θ= diffraction angle

Instrumental Broadening Correction:

The total observed broadening BT includes both instrument broadening BS and particle size
broadening B. The corrected broadening is calculated as:

B2=B2T−B2S

Key Features:

 Measures average particle size up to 200 nm.

 Provides no information about particle shape or size distribution.

 Commonly used for nanomaterials and crystalline structures.

2. Small Angle X-ray Scattering (SAXS):

In this technique, X-rays are scattered at very small angles (0° to 3°) by small particles or
nanostructures. The scattered intensity depends on the volume of the particles.

Working Principle:

When X-rays interact with tiny particles, they get scattered due to density fluctuations.
Analyzing the scattered intensity helps in determining particle size, shape, and distribution.

Key Features:

 Ideal for particles smaller than 50 nm.

 Provides size distribution and shape information.

 Suitable for nanoparticles, polymers, and biomaterials.

Comparison of different techniques

Data analysis
Surface and Surface area
Surface area is average measure of external conditions of large number of particles. It often
correlates with chemical reactivity, packing, sintering, compaction, adsorption and
compaction. However, surface tells little about distribution in properties of the powder but
combined with other parameters it has a significant effect.

The specific area is expressed as area per unit mass e.g. m2/g.
Gas adsorption surface area analysis
There are two techniques we have been taught to estimate the surface area of powder.

BET (Brunauer–Emmett–Teller) Method

The BET method is the most widely used technique for determining the specific
surface area of porous and non-porous materials. It is an extension of the Langmuir
adsorption theory, accounting for multilayer adsorption instead of just a single
monolayer.

Principle:

 A gas (usually nitrogen, N₂) is adsorbed onto the surface of a solid material
at cryogenic temperatures (typically 77 K).
 As the gas molecules accumulate, they form multiple adsorption layers on
the solid surface.
 The amount of gas adsorbed at different relative pressures is measured.
 The BET equation is used to calculate the specific surface area from the
volume of adsorbed gas.

BET Equation:

where:

 Va = Volume of adsorbed gas

 P/Po = Relative pressure (P (Actual Gas Pressure): The pressure exerted by

the gas in the system at a given moment. This is the pressure of the gas inside
your experiment. Po (Saturation Vapor Pressure): The maximum pressure at
 which the gas can exist in equilibrium with its liquid phase at a given
temperature (e.g., for nitrogen at 77 K, Po is fixed). This is the maximum
pressure at which the gas can stay in its vapor phase before it starts condensing
into a liquid.

 Vm = Monolayer adsorbed gas volume

 C = BET constant (related to adsorption energy)

Procedure:

 Sample Preparation: The sample is degasified to remove moisture and

contaminants.
 Gas Adsorption: The sample is exposed to adsorptive gas (N₂) at low
temperatures.
 Pressure Variation: The relative pressure (P/Po) is gradually increased, and
the volume of adsorbed gas is recorded.
 BET Plot & Calculation: A BET plot is constructed to determine the
specific surface area (m²/g) of the material.

Langmuir Adsorption Method

The Langmuir method is based on the assumption that adsorption occurs in a
single monolayer on the solid surface. Unlike BET, it does not consider multilayer
adsorption.

Principle:

 Gas molecules adhere to the surface at specific active sites.

 Once a site is occupied, no further adsorption can occur at that location.
 Adsorption follows a dynamic equilibrium between gas molecules attaching
to and detaching from the surface.

Langmuir Equation:

where:

 θ = Fraction of surface covered

 P = Gas pressure

 Va = Adsorbed gas volume

  K = Adsorption equilibrium constant

 Vm = Monolayer gas volume

Procedure:

 A non-porous sample is exposed to adsorptive gas at controlled pressure.

 The amount of gas adsorbed is measured at different pressures.
 A Langmuir isotherm is plotted to determine monolayer coverage.
 Surface area is calculated based on monolayer adsorption capacity.

Visualization of particle size distribution

After measuring the powder size and categorizing it we have different scales and different
ways for even a single scale. If we have particle size distribution for a powder stock we can
present it as a number percentage, weight percentage or in other ways.

Particle size vs frequency:

Particle size vs weight percentage:

Number Percentage vs. Particle Size

  Shows the fraction of particles at each size based on count (number of particles).

 Small particles (since they are more numerous).

 Peaks at smaller sizes because fine particles are present in large numbers.

 Applications: Used in pharmaceuticals, aerosols, and biological systems where the

number of particles matters.

Weight Percentage vs. Particle Size

 Shows the fraction of particles at each size based on weight (mass of particles).

 Large particles (since they are heavier).

 Peaks at larger sizes because bigger particles contribute more to the total mass.

 Applications: Used in metallurgy, ceramics, and bulk material industries where mass
matters more than count.

Volume Percentage vs. Particle Size

 Shows the fraction of particles at each size based on total volume contribution.

 Weight percentage (since mass is proportional to volume).

 Almost the same as weight-based distribution but slightly adjusted for density
differences.

 Applications: Used in construction materials, powder processing, and geological

studies.

Further reading

Ball milling
Ball milling is a mechanical process used to grind or mix materials into fine powders using a
rotating cylindrical container filled with grinding media (typically balls). The process is
widely used in material science for synthesizing nanomaterials, alloying, and particle size
reduction.
Principle
 The rotating motion of the mill causes the grinding balls to impact and crush the
material.
 The material is reduced in size due to impact, attrition, and shear forces.
 The energy imparted by the balls determines the degree of size reduction.

Types
Tumbler ball mill

Planetary ball mill