Engineering Metrology

and Measurements

N.V. Raghavendra
L. Krishnamurthy

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 Chapter 17

Nanometrology

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 Introduction
 Nanometrology is the science of
measurement at the nanoscale level.
Figure illustrates where nanoscale
stands in relation to a meter and
sub-divisions of meter.

 Nanometrology addresses two main

issues; the precise measurement of
sizes in the nanometre range, and
adapting existing or developing new
methods to characterize properties
as a function of size.

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 Types of Nanomaterials
Type of Material Diameter /
nanomaterial thickness
in ‘nm’
Nanocrystals Metals, Inorganic materials (oxides, 1-50
nitrides, sulphides, etc)

Nanofilms Layers of quantum dots made of lead 1-10

selenide, indium arsenide, etc

Nanowires Metals, oxides, nitrides, sulphides, etc 1-100

Carbon, metals, inorganic materials

Nanotubes 1-100
Various materials

Nanosurfaces 1-1000

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Applications of Nanotechnology
 Nanosensors

 Water Purification

 Lighting

 Nanocomputers

 Nano technology based Garments

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 Nanometrology Techniques
Sl. No. Parameter / Property Measurement Technique
1 Morphology: size and shape of Transmission Electron
particles, Crystallographic information: Microscopy (TEM)
detection of atomic scale defects

2 Topography: the surface features, Scanning Electron Microscopy

Morphology: shape and size of the (SEM)
particles, Composition: the elements
and compounds the sample is
composed of, Crystallographic
Information: the arrangement of atoms

3 Three dimensional surface topology: Scanning Tunneling Microscopy

size, shape, roughness, defects, (STM)
electronic structures

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 Nanometrology Techniques
Sl. No. Parameter / Property Measurement
Technique
4 Topology, roughness and elasticity Atomic Force
of surface, grain size, frictional Microscopy (AFM) or
characteristics, specific molecular Scanning Force
interactions and magnetic features Microscopy (SFM)
on surface.

5 Crystallographic information: type X- Ray Diffraction (XRD)

of crystal structure, film thickness,
interface roughness and surface
topology.

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Transmission Electron Microscope
 It is possible to form a transmission electron diffraction pattern
from electrons that have passed through a thin specimen. If these
transmitted electrons are focused, their very short wavelength
would allow the specimen to be imaged with a spatial resolution
much better than the light-optical microscope.

 In a transmission electron microscope (TEM), electrons penetrate

a thin specimen and are then imaged by appropriate lenses, quite
similar to optical microscope.

 One limitation of the TEM is that, unless the specimen is made

very thin, electrons are strongly scattered within the specimen, or
even absorbed rather than transmitted.

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Transmission Electron Microscope

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Transmission Electron Microscope

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 Scanning Electron Microscope
 The scanning electron microscope is arguably the most versatile
microscope with magnification ranging from 5X to as high as 106X.
It provides excellent resolution, amenable to automation and user
friendly.

 These features have made it the most widely used of all electron
beam instruments. The sample preparation and examination is
also relatively simple compared other techniques.

 A wide range of nanomaterials, starting from powders to films,

pellets, wafers, carbon nanotubes, and even wet samples can be
examined. It is also possible to correlate the observations made at
nan scale to macro scale and draw reliable conclusions.

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 Scanning Electron Microscope
Signals generated in an SEM

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 Scanning Electron Microscope
Components of Scanning Electron Microscope

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 Scanning Electron Microscope
Scan Pattern in SEM

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 Scanning Tunneling Microscope
 The STM works on the principle of quantum tunneling. When an
atomically sharpened tip under a small voltage is brought close to the
surface of a sample, so that the separation is of the order of a
nanometer, there is a small change in current in the circuit. This effect is
called the quantum tunneling effect.

 The induced current is referred to as the tunneling current. The

tunneling current increases as the gap between the tip and the sample
decreases.

 The change in tunneling current can be calibrated with respect to the

change in gap. In other words, if we scan the tip over the sample
surface while keeping the tunneling current constant, the tip movement
depicts the surface topography, because the separation between the tip
apex and the sample surface is always constant
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 Scanning Tunneling Microscope
Components of STM

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 Atomic Force Microscope
 An AFM is rather different from other microscopes,
because it does not form an image by focusing light or
electrons onto a surface, like an optical or electron
microscope.

 An AFM physically ‘feels’ the sample’s surface with a

sharp probe, building up a map of the height of the
sample’s surface.

 By scanning a probe over the sample surface it builds up

a map of the height or topography of the surface as it
goes along.

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 Atomic Force Microscope
Laser Deflection contact AFM

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 X Ray X-ra
Diffraction System
Diffraction System (XRD)
(XRD)
 X-ray diffraction is an ideal method for examining samples of
metals, polymers, ceramics, semiconductors, thin films and
coatings.

 It can also be employed for forensic and archeological analysis.

 A two-dimensional diffraction pattern provides abundant

information about the atomic arrangement, microstructure,
and defects of a solid or liquid material.

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 X Ray Diffraction System (XRD)
Bragg’s Law

Bragg law describes the relationship between the diffraction pattern

and the material structure. If the incident X-rays hit the crystal planes
with an incident angle θ and reflection angle θ as shown in figure in
the next slide, the diffraction peak is observed when the Bragg
condition is satisfied

That is, nλ = 2d.sin θ

where λ is the wavelength, d is the distance between each adjacent

crystal planes, θ is the Bragg angle at which one observes a diffraction
peak, and n is an integer number, called the order of reflection.

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 X Ray Diffraction System (XRD)
Bragg Law

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2D X Ray Diffraction System (XRD)

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