SCANNING ELECTRON

MICROSCOPY

METALLURGICAL AND MATERIALS

ENGINEERING
Interactive volume

Electron
Microscopy
 Interaction Volume: I

e-

Monte Carlo simulations of 100 electron trajectories

The incident electrons do not go along a

straight line in the specimen, but a zig-zag
path instead.
 Interaction Volume: II

The penetration or,

more precisely, the
interaction volume
depends on the
acceleration voltage
(energy of electron)
and the atomic
number of the
specimen.
Escape Volume of Various Signals
• The incident electrons interact with specimen
atoms along their path in the specimen and
generate various signals.
• Owing to the difference in energy of these
signals, their ‘penetration depths’ are
different
• Therefore different signal observable on the
specimen surface comes from different parts
of the interaction volume
• The volume responsible for the respective
signal is called the escape volume of that
signal.
 Escape Volumes of Various Signals

If the diameter of primary

electron beam is ~5nm
- Dimensions of escape
zone of
•Secondary electron:
diameter~10nm; depth~10nm
•Backscattered electron:
diameter~1m; depth~1m
•X-ray: from the whole
interaction volume, i.e., ~5m
in diameter and depth
 Advantages of Using SEM over OM
Magnification Depth of Field Resolution
OM 4x – 1000x 15.5m – 0.19m ~ 0.2m
SEM 10x – 3000000x 4mm – 0.4m 1-10nm

The SEM has a large depth of field, which allows a large

amount of the sample to be in focus at one time and
produces an image that is a good representation of the
three-dimensional sample. The SEM also produces
images of high resolution, which means that closely
features can be examined at a high magnification.

The combination of higher magnification, larger depth of

field, greater resolution and compositional and
crystallographic information makes the SEM one of the
most heavily used instruments in research areas and
industries, especially in semiconductor industry.
 Scanning Electron Microscope
– a Totally Different Imaging Concept

• Instead of using the full-field image, a point-

to-point measurement strategy is used.
• High energy electron beam is used to excite
the specimen and the signals are collected and
analyzed so that an image can be constructed.
• The signals carry topological, chemical and
crystallographic information, respectively, of
the samples surface.
 Main Applications
• Topography
The surface features of an object and its texture
(hardness, reflectivity… etc.)
• Morphology
The shape and size of the particles making up the
object (strength, defects in IC and chips...etc.)
• Composition
The elements and compounds that the object is
composed of and the relative amounts of them
(melting point, reactivity, hardness...etc.)
• Crystallographic Information
How the grains are arranged in the object
(conductivity, electrical properties, strength...etc.)
SEM Column
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4
 Why Vacuum is necessary

1)If the column is in a gas filled environment, electrons

will be scattered by gas molecules which will 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 of the
image.
Electron
Sources

Thermionic emission

Field emission
W - Filament Single crystal of LaB6 tip

W – crystal tip
Thermionic Field
emission emission
 Earth
Potential
 Secondary Electrons (SE)
Produced by inelastic interactions
Primary of high energy electrons with
valence (or conduction) 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".
Each incident electron can produce
several secondary electrons.
SE yield: d=nSE/nB independent of Z BaTiO3
d decreases with increasing beam
energy and increases with decreasing
glancing angle of incident beam
Production of SE is very topography Growthstep
related. Due to their low energy, only SE
that are very near the surface (<10nm)
can exit the sample and be examined 5m
SE image
(small escape depth).
 Topographical Contrast
Everhart-Thornley
SE Detector

Bright lens polepiece

e-
SE Scintillator
light pipe PMT
Dark
sample Quartz
Faraday window
cage +200V +10kV
Photomultiplier
tube

Topographic contrast arises because SE generation depend on the

angle of incidence between the beam and sample.
Thus local variation in the angle of the surface to the beam
(roughness) affects the number of electrons leaving from point to
point.
This is a function of physical shape of specimen.
 Z Contrast Imaging

BSE are produced by elastic interactions of beam

electrons with nuclei of atoms and they have high
energy and large escape depth
(total fraction of beam electrons Number of backscatter
that backscatter) electrons

Number of beam electrons

The total BSE yield from a randomly oriented

polycrystalline tends to increase monotonically with
the atomic number, Z
Backscattering
η = -0.0254 + 0.016Z - 1.86*10- coefficient
4 Z2 + 8.3*10-7Z3
Effect of Atomic Number, Z, on
BSE and SE Yield
 Depth of Field

Depth of Field

4x105W
D= (m)
AM

To increase D
Decrease aperture size, A
Decrease magnification, M
Increase working distance, W (mm)
 Field Contrast

Electron trajectories are affected by both

electric and magnetic fields

• Electric field – the local electric potential at the surface

of a ferroelectric material or a semiconductor p-n
junction produce a special form of contrast (Voltage
contrast)

• Magnetic field – imaging magnetic domains

SE electrons emitted from a clean surface ferromagnet are
spin-polarized, the sign of the polarization being opposite
to the magnetization vector in the surface of the material
(Magnetic field contrast).
 Voltage contrast

+U
-U

500m

Voltage contrast from integrated circuit recorded at 5kV.

The technique gives a qualitative view of static (DC)
potential distributions but, by improvements in
instrumentation, it is possible to study potentials which may
be varying at frequencies up to 100MHz or more, and to
measure the potentials with a voltage resolution of 10mV
and a spatial resolution of 0.1m.
 Magnetic Field Contrast
(monolayer)

t
+ - tc

SE electrons emitted from a clean surface ferromagnet are

spin-polarized, the sign of the polarization being opposite
to the magnetization vector in the surface of the material.

High resolution SEM image of a magnetic microstructure in

an ultrathin ‘wedge-shaped’ cobalt film.
 Other Imaging Modes
Cathodoluminescence (CL)
Nondestructive analysis of impurities and defects, and
their distributions in semiconductors and luminescence
materials
Lateral resolution (~0.5m)
Phase identification and rough assessment of
defect concentration

Electron Beam Induced Current (EBIC)

Only applicable to semiconductors. Electron-hole pairs
generated in the sample. External voltage applied, the
pairs are then a current – amplified to give a signal
Image defects and dislocations
 CL micrographs of Te-doped GaAs

a. b.

a. Te=1017cm-3, dark-dot dislocation contrast

b. Te=1018cm-3, dot-and-halo dislocation contrast which
shows variations in the doping concentration around
dislocations
 EBIC Image of Doping Variations
in GaAs Wafer

The variations in brightness across the material are due to

impurities in the wafer. The extreme sensitivity (1016cm-3) and
speed of this technique makes it ideal fro the characterization
of as-grown semiconductor crystals.
Energy-dispersive X-ray spectroscopy (EDS, EDX, EDXS or
XEDS), sometimes called energy dispersive X-ray analysis
(EDXA) or energy dispersive X-ray microanalysis (EDXMA), is
an analytical technique used for the elemental analysis or
chemical characterization of a sample.
The number and energy of the
X-rays emitted from a specimen
can be measured by an energy-
dispersive spectrometer.

As the energies of the X-rays are

characteristic of the difference in
energy between the two shells and
of the atomic structure of the
emitting element, EDS allows the
elemental composition of the
specimen to be measured.
 semiconductor detector (Si
(Li)) is used. To maintain
detector integrity and
resolution it should be cooled
with liquid nitrogen.
Counts
A trend towards a newer EDS detector, called
the silicon drift detector (SDD).
Advantages
1) High count rates and processing
2) Better resolution than traditional Si(Li) detectors at
high count rates,
3) Lower dead time (time spent on processing X-ray
event),
4) Faster analytical capabilities and more precise X-
ray maps or particle data collected in seconds,
5) Ability to be stored and operated at relatively high
temperatures, eliminating the need for liquid
nitrogen cooling
 Wavelength Dispersive Spectroscopy

WDS differs from EDS in that it uses the diffraction of X-rays on

special crystals to separate its raw data into spectral
components (wavelengths).

WDS has a much finer spectral resolution than EDS.

WDS also avoids the problems associated with artifacts in EDS

(false peaks, noise from the amplifiers, and microphonics).

WDS is only sensitive to a repeating pattern of atomic species,

usually referred to as the crystal structure, while EDS gathers
a spectrum of all elements, within limits, of a sample.
 For a particular element
Principle of WDS
1) Known d spacing
2) Known incident angle

Single λ to satisfy
Braggs law

For a https://serc.carleton.edu/research_education/geochemsheets/wds.htmlKNOWN
 EBSD – Electron Backscatter Diffraction

Electron backscatter diffraction (EBSD) is a microstructural-

crystallographic characterization technique to study any
crystalline or polycrystalline material.

The technique involves understanding the structure, crystal

orientation and phase of materials.

Typically it is used to explore microstructures, revealing texture,

defects, grain morphology and deformation. It can be combined
with complementary techniques within the SEM for phase
discrimination.
EBSD
EBSD Detector
Kikuchi Pattern
http://www.ebsd.com/ebsd-for-beginners