Introduction to Nanotechnology

09106500

Chapter 3: Nanotools for Materials Characterization

(Continued)

Prof. Dr. Wisanu Pecharapa

College of Materials Innovation and Technology

King Mongkut’s Institute of Technology Ladkrabang
1
Important characterization methods
for nanoscience and nanomaterials

➢ X-ray based techniques

➢X-ray diffraction
➢X-ray photoelectron spectroscopy
➢X-ray fluorescence spectroscopy
➢ Fourier transform Infrared
spectroscopy (FTIR)
➢ Electron Microscopy
Electron-based Technique
 Basic Theory of Electron Acceleration
Electron beam accelerated under electrical
potential difference of V will have kinetic
- +
energy (K) of

- +

- + Then, its final velocity is,

- +
 de Broglie wavelength (revisited)

◼ The de Broglie wavelength of a particle is

h h
= =
p mv
Under V
 Example 1: wavelength of accelerated electrons

Calculate the corresponding velocity and de Broglie wavelength of

electron under bias voltage of 150 Volt.
 Basic Theory of Magnetic force on
moving charge
Magnetic Force on a moving charge
◼ proportional to electric charge

◼ perpendicular to velocity v

◼ proportional to speed v (for a given geometry)

◼ perpendicular to Magnetic Field B

◼ proportional to field strength B (for a given

geometry)
F=qvB
 Magnetic force direction
Right hand rule

◼ The force is perpendicular to both the field and the velocity

◼ Oppositely directed forces exerted on oppositely charged particles will cause
the particles to move in opposite directions
F=qvB F
F = |q| v B sin B
= |q| v B (v ⊥ B) +
v

F
F=qvB
B
F = |q| v⊥ B +
v⊥
v
F
F=qvB
F = |q| v B⊥ + B⊥
v
B
Charged Particle moving perpendicular to a
uniform Magnetic Field

mv 2
F =| q| vB =
R v
mv
R
R=
| q| B

+
v | q| B
= =
R m + v
= cyclotron frequency
 Velocity Selector

makes use of crossed E and B to provide opposing forces

+ + + + + + + upwards
F=qvB
E downwards
− − − − − − − F = qE

No net deflection => forces exactly cancel:

|q| v B=|q| E
v = E/B
J. J. Thomson’s Measurement of e/m

Electron Gun + + + + + + +

E
− − − − − − −
V
and velocity selector:
E e/m = 1.76x1011 C/kg
v=
B with Millikan’s measurement of e
1 2
mv = eV => mass of electron
2
e E2
=
m 2VB 2
 Example 2: Velocity selector

Using an accelerating Potential of 150 V and a transverse Electric Field of

6x106 N/C. Determine
a) the speed of the electrons,
b) the magnetic field magnitude required for no net deflection
 Mass Spectrometer

R2

+ + + + + + R1

− − − − − − E

E
One method v=
B
velocity selector + circular mv
trajectory R=
qB
RqB RqB 2
m= =
v E
 Example 3: Helium ions

Vacuum System Leak Detector uses Helium atoms. Ionized helium atoms (He +)
are detected with a mass spectrometer with a magnetic field strength of 0.1 T.
With a velocity selector tuned to 1x105 m/s, where must the detector be placed
to detect 4He + ions? (mass of He+ = 6.7 x 10-27 kg)
Electron Microscope
 Light vs. Electron Microscope

LIGHT MICROSCOPE ELECTRON MICROSCOPE

Electrons are used to “see” –
The source of The ambient light source is
light is replaced by an electron
illumination light for the microscope
gun built into the column

The lens type Glass lenses Electromagnetic lenses

Focal length is charged by

Magnification Magnification is changed by
changing the current through
method moving the lens
the lens coil

Viewing the Fluorescent screen or

Eyepiece (ocular)
sample digital camera

Entire electron path from

Use of vacuum No vacuum gun to camera must be
under vacuum

*www.fei.com
 Light vs. Electron Microscope

◼ Similar to optical microscopy except with electrons rather

than photons
◼ Used to image samples with a resolution of 10 Å
◼ Can image many different structural geometries
◼ Mostly limited by radiation damage from the electron beam
KEY CONCEPT: Resolution
Resolution
is defined as the act, process, or capability of
distinguishing between two separate, but adjacent
objects or sources of light, or between two nearly
equal wavelengths.

Resolving Power
is the ability to make points or lines which are
closely adjacent in an object distinguishable in
an image.
 Resolving Power of the Human Eye

What can we see?

*www.fei.com
 Resolution & Magnification

*www.fei.com scale
 OM vs SEM

m
radiolarian
OM SEM
Small depth of field Large depth of field
Low resolution High resolution
 How is resolution affected by wavelength?

*www.fei.com © 2013 FEI

Electron Properties
◼
 Microscope Setup
◼ Transmission Electron
Microscope
◼ Phase contrast Image is
formed by the interference
between electrons that
passed through the sample
and ones that did not
◼ Scanning Electron
Microscope
◼ Electron beam is scanned
across the sample
◼ The reemitted electrons are
measured in order to form
the image
Major components of electron microscope
 Electron Generation
◼ Thermionic Electron Gun
◼ Heated filament produces
electrons
◼ Typically made of Tungsten or
Lanthanum hexaboride
◼ Electrons drawn towards an
anode
◼ An aperture in the anode creates
a beam
 Field Emission Gun
 A very strong electric field is
used to extract electrons from a
metal filament
 Filament typically a single
tungsten crystal
 Requires a vacuum
 Similar anode setup
Electron beam Source
LaB6

W or LaB6 Filament
Thermionic or Field Emission Gun
 Magnetic Lens

◼ Condenser lens – focusing

controls the spot size and convergence ()
of the electron beam which impinges on
the sample.
◼ Objective lens – final probe forming
determines the final spot size of the
electron beam, i.e., the resolution of a
SEM.
How Is Electron Beam Focused?

We can change the

strength of the lens
(i.e. the focal plane) by
changing the current.

f  B2
 Why vacuum is required?

When a SEM is used, the electron-optical column

and sample chamber must always be at a vacuum.

1. If the column is in a gas filled environment,

electrons will be scattered by gas molecules which
would lead to reduction of the beam intensity and
stability.

2. Other gas molecules, which could come from the

sample or the microscope itself, could form
compounds and condense on the sample. This
would lower the contrast and obscure detail in the
image.
Electron Detectors and Sample Stage

Sample stage
Electron Beam and Specimen Interactions

(1-50keV)

Electron Beam Induced Current (EBIC)

 Why secondary electrons?

• SE is produced by inelastic interactions of high energy

electrons with electrons of atoms in the specimen, causing
the ejection of the electrons from the atoms.
• These ejected electrons with energy less than 50eV are
termed "secondary electrons".
• Production of SE is very topography related. Due to their low energy,
only SE that are very near the surface (<10nm) can exit the sample
and be examined.
 Topographic contrast

❑ Topographic contrast arises because

SE generation depend on the angle
of incidence between the beam and
sample.
❑ Local variations in the angle of the
surface to the beam (roughness)
affects the numbers of electrons
leaving from point to point.
❑ The resulting “topographic contrast” is
a function of the physical shape of the
specimen.
Interaction volume

*https://myscope.training/
 Comparing SEM and TEM
TEM SEM
Beam focused to fine point;
Electron Beam Broad, static beams
sample is scanned line by line

TEM voltage ranges from Accelerating voltage much lower; not

Voltages Needed
60-300,000 volts necessary to penetrate the specimen
Wide range of specimens allowed;
Interaction of the
Specimen must be very thin simplifies
beam electrons
sample preparation
Information needed is
Electrons must pass through and
Imaging collected near the surface
be transmitted by the specimen
of the specimen

Transmitted electrons are

Image Rendering Beam is scanned along the surface of
collectively focused by the
the sample to
objective lens and magnified to
build up the image
create a real image

*www.fei.com