MSE 205 Lecture 29

Grain, Particle and Crystalline Size

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 Recap

The arrangement of atoms in a crystal structure not only depends on

the charge on the ion and type of bonding between atoms, but also on
the size of the atoms or ions.

The special arrangement of the ligand atoms which are directly

attached to the central atom/ion forms the coordination polyhedron
around the central atom/ion. Tetrahedral, square planar, octahedral,
square pyramidal and trigonal bipyramidal are common shapes of
coordination polyhedra.

Linus Pauling studied crystal structures and the types of bonding

and coordination that occurs within them. His studies found that
crystal structures obey the five rules, now known as Pauling's Rules.

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 Grain Size
As far as material science is concerned grain size refers to that
volume of a material within which the crystal structure and the
orientation of the crystals is same.

At the grain boundaries, you have a change in orientation of the

crystal. Or Grains are volumes, inside crystalline materials, with a
specific orientation.

Grain is either a single crystalline or polycrystalline material, and is

present either in bulk or thin film form.

In case of single crystal, the whole crystal can be called as a single

grain. Here it can be considered as a particle.

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 Grain Size

A grain boundary is the interface between two grains, or

crystallites, in a polycrystalline material. Grain boundaries
are 2D defects in the crystal structure, and tend to decrease the
electrical and thermal conductivity of the material.

A finer grain size means more grain boundaries, and more

grain boundaries means a greater resistance to dislocation. It is
the measured ability of a material to withstand serious plastic
deformation, making the material less ductile

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Grain Size and Hall-Petch Relationship
The Hall–Petch relationship tells us that we could achieve
strength in materials that is as high as their own theoretical
strength by reducing grain size. In other words, the strength
increase trades off with ductility in nanostructured metallic
materials.

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 How is grain size determined?
One of the simplest techniques to estimate an average grain
size is the intercept technique. A random straight line is drawn
though the micrograph. The number of grain boundaries
intersecting the line are counted. The average grain size is
found by dividing the number of intersections by the actual
line length.

The average grain size is found by dividing the number of

intersections by the actual line length.

Average grain size =1/(number of intersections/actual length of

the line).

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What happens if grain size increases?

If the grain size increases, accompanied by a reduction in

the actual number of grains per volume, then the total area of
grain boundary will be reduced. is radius of the sphere. This
driving pressure is very similar in nature to the Laplace
pressure that occurs in foams.

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How does grain size affect strength?

Smaller grains have greater ratios of surface area to volume,

which means a greater ratio of grain boundary to dislocations.
The more grain boundaries that exist, the higher the strength
becomes.

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 Particle size

On the other hand Particle size is a macro phenomenon. It is the size

of the particles which may have 1 or several grains within it.

It is impossible to have a grain having multiple particles because

the smallest thing we could have would always represent one single
grain.

Particles are chunks/pieces (usually very small, below 1 mm) of

solid matter, ensembles of atoms.

Particles can be as small as two atoms (the nitrogen particle for

example, N2

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 Particle size
Particle size is a notation for the comparative dimension of solid
particles.

But when we are talking about the metal, the crystal contains the internal
boundaries. Any of the enclosed part by these boundaries, called as grain
and its size is called as a grain size.

Generally inside the particle, we can get grains.

Particles can be polycrystalline, single crystal or amorphous. A 100

nanometer particle of gold, for instance, can be made of:

•a single gold crystal

•many grains with a grain size <100 nm,or of amorphous gold.

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What is particle size analysis used for?

Particle size analysis is used to characterise the size distribution

of particles in a given sample. Particle size analysis can be
applied to solid materials, suspensions, emulsions and even
aerosols. There are many different methods employed to measure
particle size.

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How do you measure particle size on a
microscope?

Microscopy can be used as an absolute method of particle size

analysis, since it is the only method in which individual mineral
particles are observed and measured . The image of a particle seen in
a microscope is two-dimensional and from this image an estimate of
particle size must be made.

Particles can be polycrystalline, single crystal or amorphous. A 100

nanometer particle of gold, for instance, can be made of:
a single gold crystal,
many grains with a grain size <100 nm,
or of amorphous gold.

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 What are the different methods of
reducing the particle size?

Mechanical techniques to decrease the particle-size of solids are

generally classified in three categories: dry-milling, wet-milling, and
high-pressure homogenization.

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 Crystallite size

Crystallite size is the smallest - most likely single crystal in

powder form. The crystallite size commonly determined by XRD.

Grain is either a single crystalline or polycrystalline material, and

is present either in bulk or thin film form. Therefore, particle is
under no circumstances smaller than crystallite size.

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 Crystallite size

Crystallite Size is Different than Particle Size.

A particle may be made up of several different crystallites or just one

crystallite so in this case (particle size = crystallite size). Crystallite
size often matches grain size, but there are exceptions

Crystallites are coherent diffraction domains in X-ray diffraction.

Crystalline size sometime was written as sub-grain size,and a particle

consists of lots of grains or sometimes one crystal.

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How do you measure crystallite size?
Scherrer formula is used to calculate the average size in vertical
direction of crystal.

D=Kλ/(β cos θ).

For cubic crystal structure, K =0.94, λ is wavelength of X-ray. β =

the full width at half maximum intensity of the peak (in Rad) – you
can calculate it using Origin software.

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 Peter Dier's Rule

According to Peter Dier's Rule, Crystallite is smaller than

grain, grain is smaller than particle. Particle consists of grains
and grain consists of crystallites

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 How size can be measured?

Grain size is measured from microstructures using SEM technique where

the individual grains and grain boundaries can be observed.

But a particle is more like a morphology whose size can be analysed using
particle size analyser and particle size distribution from sieves or andersen
pipette.

A particle can be individual grain or multiple grains with grain boundaries

which can be seen in SEM images.

Crystallite size measured from scherrer equation from XRD peaks which
means the size in which particular crystalline plane is oriented. This is
equivalent to grain size (the crystalline plane inside a grain is oriented in
same direction) but different from particle size.

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 Summary

Crystalline size is smaller than grain or particle size.

Inside a grain or particle we have many crystals of identical orientation.

Particle size and grain size are not same.

one particle can have several grains. unless you produce a particle which
is single crystal.

Crystallite size is the smallest - most likely single crystal in powder

form. The crystallite size commonly determined by XRD. Grain is
either a single crystalline or polycrystalline material, and is present either
in bulk or thin film form. . Therefore, particle is under no circumstances
smaller than crystallite size.

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