Electron-Sample Interaction, Scattering Process - Electron Microscopy and Diffraction

Do Minh Nghiep
Materials Science Center
Electron Microscopy
and Diffraction
4. Electron
Electron-- specimen interaction,
Scattering process and application
Content
 Interaction of primary beam and specimen

 Interaction volume and signals obtained
 Scattering process
 Secondary electron image (SEI) and detector
 Backscattered electron image (BSEI) and detector
 X-ray spectra
 Factors influencing resolution: voltage and Zsample
01.01.2009 Materials Science Center, HUT 2

Interaction
mode
and volume

Monte
Monte--Carlo simulation
The size and shape of the
region of primary
excitation can be
estimated by carrying out
simulations that use
Monte Carlo calculations
and take into account the
composition (Z
(Z), thickness
(d) of the specimen and
accelerated voltage ((V
V)

Monte
 An interaction
volume can also be
used to predict the
types of signals that
will be produced and
the depth from which
they can escape.
 Monte Carlo simulations of electron trajectories are based on 1) the

energy of the primary beam electron, 2) the likelihood of an interaction, 3)
the change in direction and energy of the electron, 4) the mean free path
of the electron and 5) a “random” factor for any given interaction
interaction..
Monte
http://www.small-world.net/efs.htm
Interaction volume
Incident beam
Interaction
volume
 Electron
Electron--sample interaction volume has a pear shape (left)
(left)..
 Actual image of interaction volume between incident beam and
sample surface (right) showing shape and size of primary excitation region
Interaction depth of signals
Prim.
beam
1. Auger electron
Spec.
1. Auger electron (0,1
0,1--2 nm)
nm
surface 2. Sec. electron 2. Secondary
electron (10 nm)
nm
3. Backscattered
3. Back-scat.
electron electron ( 5 mm)
6. Xray fluorescence
4. Charact. X-ray
Primary Signals: 4. Charac. 5. Continiium X-ray
§iÖn tö thø cÊp Xray
6. Fluorescence
§iÖn tö t¸n x¹ ngîc 5. Xray continium
Xray (  10 mm)
Tia r¬ngen
Determination of interaction depth
Ec = 7 eV; Eo = 20 keV; r = 7 g.cm-3; d = 0.8 mm

Use of signals
When the electron beam strikes a sample, both photon and
electron signals are emitted:
Backscattered electron
electron::
Xray: sample
Xray:
Incident electron topographic info and phase
composition (Z) contrast (SEM)
(SEM+EDS/WDS) Xray fluorescence
fluorescence::
elemental composition
Secondary electron
electron:: (EPMA)
surface topography Auger electron
electron::
(SEM) surface composition
Electric current
current::
Specimen electrical property
Transmitted electron:
electron: microstructure, crystal structure, composition (TEM+EELS)

Informations from interaction
Electron and photon signals give infos about

- Topography of surface
- Microstructure and /or morphology
- Crystal and/or defect structure
- Chemical composition
- Electrical current
- Local magnetic field

Scattering process

Electron
scattering
 Scattering
Scattering:: change in the
primary motion direction
 Names:
- without energy loss:
elastic scattering
- with energy loss:
inelastic scattering
Electron scattering
 Elastic (coherent) scattering: electron changes its
trajectory but energy unchanged
- Scattered transmitted electron (diffraction)
- Back-scattered electron
 Inelastic (incoherent) scattering: electron changes its
trojectory and loses a part of energy for secondary
processes
- Secondary electron
- Auger electron
- Continium and characteristic X-ray radiation
- Cathodoluminiscence

Electron scattering
The probability of an
elastic vs..
vs an
inelastic collision is
based primarily on
the atomic weight of
the specimen (Z).

Electron scattering
Elastic scattering Inelastic scattering

 A beam electron interacts with the electrical field  A beam electron interacts with the
of the nucleus of a specimen atom electrical field of electrons of a specimen
 Resulting in: atom
- a change in the direction of the beam electron  Resulting in:
without a significant change in the energy of the - a transfer of energy to the specimen atom
beam electron - secondary electrons (<50 eV), Auger
- backscattered electrons (>50 eV) and continuous electrons, characteristic x-x-rays and
x-rays are formed, electron diffraction cathodoluminescence are formed
How signals are formed
High
High--energy Secondary electron
primary electron
Primary electron inin--
elastically scattered
A hole is created
L M in the shell
K
Auger electron Characteristic X-

X-ray
Shell electron released
as an Auger electron
A shell electron falls

to the vacant shell
De-
De-excitation occurs by
release of X-
X-ray photon

Signal
Inelastically
scattered e-
energy
Backscattered
Electron Signal
 Secondary electron:
< 50 eV
 Back-scattered
electron: > 80 % of
primary electron
energy
 X-ray: 0.520 keV

Auger electron

Auger electron
 Low energy electrons emitted from the upper 2-

2-3 nm of the surface and
 Contains information about the element that produced it based on its energy
Auger electron spectrum
An Auger spectrum for Aluminum showing peaks

for different electron replacement events
Secondary electron
(SE) image and detector

Secondary electron (SE)
 Secondary electrons are
usually the result of an
inelastic collision in which
the energy of the primary
beam is partly transferred
to an electron that is then
emitted from the atom as
SE.
 Secondary electrons
typically have an energy
of 50 eV or less.

Secondary
electron
 Although secondary
electrons are produced
throughout the interaction
region, they can only escape
from the uppermost portion
due to their low energy.
 SE gives info of topography
Primary electron Edge effect and Surface
sample thickness
Primary electron
topography
Fewer SE
escape MoreSE
escape
on edges Fewer SE
contrast by SE
escape on
flat areas
Thick sample  The angle at which the beam

strikes the specimen and the
Primary electron distance from the surface are
SE escape from both sides
important factors in how much
of signal escapes from the
specimen.
specimen.
Thin sample
 Rough area: more signals,
Flat area: fewer signals
 Thick sample  thin sample
Surface
Sample
surface
topography
contrast by SE
Sometimes one can take
advantage of the this effect
and increase useable
signal by tilting the
specimen towards the
detector and at an angle
relative to the primary
beam.
Detectors
 SE detector:
- Lateral: side mounted
- Annular: in
in--lens
 BSE detector:
- Solid state detector

SE detector
 The position of the
secondary electron
detector also affects signal
collection and shadow.
 An in-
in-lens detector within
the column is more
efficient at collecting
secondary electrons that
are generated close to the
final lens (i.e. short
working distance).

SE detector
 An in
in--lens detector does not
use a faraday collector as
this would affect the primary
beam electrons, but instead
depends on the natural
trajectory of the secondary
electrons to strike it
it..
 It takes advantage of the
focusing action of the lens to
bring these SE to cross over
and then spread out to strike
the annular detector
detector..

SE detector
Side mounted: deep image In

In--lens: distinckt surface

SE detector
Phosphorus crystal
2. Scintillator
1. Faraday Electrode
cage/grid Photocathode 4. Photomultiplier tube
SE
Photons Photoelectrons SE
~ 300V +10kV 3. Light guide pipe Dinodes
Amplifier
CRT
SE detector system usually consists of 4 parts: (1) a Faraday cage,

(2) a scintillator, (3) a light guide pipe, (4) a photomultiplier.
SE detector
Everhart -Thornley detector setup with

Faraday cage biased to +300 V to collect SE
Photomultiplier

SE detector: Faraday cage
A conventional secondary electron detector is positioned off to the side of the

specimen. A faraday cage (kept at a positive bias) draws in the low energy
secondary electrons. The electrons are then accelerated towards a scintillator
which is kept at a very high bias in order to accelerate them into the phosphorus.
SE detector: scintillator
Scintillator
The Everhart
Everhart--Thornley detector has an aluminum coating (+ (+10
10--12
keV) that also serves to reflect the photons back down the light pipe
pipe..

The scintillator is a
phosphor crystal that
absorbs an electron
and generates a
photon.

The photons
produced in the
scintillator are
carried down a
fiber optic light
pipe out of the
microscope.

SE detector: photomultiplier
Most of the secondary electron detector lies outside of the SEM

chamber and is based on a photomultiplier tube (PMT)
The PMT is converting the incoming photons into electrons which are then drawn to
dynodes kept at a positive bias. The dynodes are made of material with a low work
function and thus give up excess electrons for every electron that strikes them. The
result “multiplies” the signal contained in each photon produced by the scintillator.
1. The electronic signal from
the PMT is further increased
by a signal amplifier.
2. Thus an increase in “gain”
is accomplished by voltage
applied to the dynodes of the
PMT and alters the contrast of
the image.
3. An increase in the “black”
level is made by increasing
the current in the amplifier and
alters the brightness of the
image.
4. Signal is thus increased at
the scintillator, PMT, and
amplifier.
Back
Back--scattered
electron (BSE) image
and detection

Back-
Back-scattered electron (BSE)
 Backscattered electrons
are the result of elastic
collisions with atoms of the
specimen.
 They result in emitted
electrons that have an
energy of 80 % or more of
the original energy of the
primary beam electron.

Back-
Back-scattered electron (BSE)
 Backscattered
electrons are also
produced throughout
the interaction region
but because of their
greater energy can
escape from deeper in
the specimen.
 Backward scattering
about 180 o.

Z-contrast SEI
by BSE
 Production of backscattered
electrons varies with atomic
number (Z).
 Higher atomic number
elements appear brighter (or BSEI
scatter more effectively) than
lower atomic number
elements.
 Resulting image shows
elemental contrast.
BSE detector
Backscatter electrons
have a greater energy
and can escape from
deeper within the
specimen than can
secondary electrons, but
because they are more
readily produced by high
atomic weight elements
they can be used to
visualize differences in
elemental composition.
Repulsed SEs Primary e-
BSEs BSE detector
Primary e-
Objective
Primary e-
BSEs
Convert
target
Backward
SEs
SEs from
sample
+300V
-50 V
Grid

BSE detector
The topography of the specimen will also affect the

amount of backscatter signal and so backscatter
imaging is often carried out on flat polished samples
BSE detector
Since backscattered electrons have a high energy they

cannot be collected by way of a Faraday cage or other device
BSE detector
The most common design is a four quadrant solid state

detector that is positioned directly above the specimen
BSE detector
Two image modes:

- COMPO (A+B)
composition image
- TOPO (A-B)
topography image

Example 1
SEI
Blood cells with

nuclei stained with
a silver compound
are visible in
backscatter mode,
BSEI even though they
are beneath the
surface of the cell
membrane.

Example 2
Gold particles on E. coli appear as bright white dots due to

the higher percentage of backscattered electrons compared
to the low atomic weight elements in the specimen.
Example 3
Ni
Backscatter image of nickel in a leaf

Example 4
Backscatter image of a composite (polished cement

fragment) in which low atomic weight particles appear
dark and high atomic weight particles are white.
Electron detectors in
Environmental SEM
• BSE Detector: Large-area scintillator detector
is more suitable than E-T detector. Because of
electric discharge of the last, BSEs lose a bit
of energy in the gas medium and have enough
energy to activate scintillator.
• SE Detector: Gas-Amplification Detector (Gas
Phase Detector)

Environmental SEM

Environmental
SEM
SE detector in Environmental SEM
Environmental electrons are a form of secondary electrons that

are produced via interactions of secondary electrons produced
by the specimen that strike gas molecules in the chamber, thus
amplifying the signal.
Movie of melting sample in ESEM
An environmental SEM or ESEM actually requires gas of

some sort (usually water vapor) to create the signal and
can operate at elevated pressures as high as 1 x 10 Torr
Watching paint dry in ESEM
0 min. 15 min.
10 min.
20 min.
Example
The ESEM uses a special detector
X-ray spectrum

X-rays
 X-rays are indirectly produced
when an electron is displaced
through a collision with a
primary beam electron and is
replaced by another electron
electron..
 The resultant loss of energy is
given off in the form of an X-ray.
ray.
 The energy will always be less
than the energy of the primary
beam electron
electron..

X-ray spectrum
EDS
 Because of their high

energy (5-20 keV) X-rays
can escape from very
deep in the specimen.
 X-rays are used for
elemental analysis (EDS,
WDS)
Resolution and its
influencing factors

Resolution decreases as
interaction volume increases
 Resolution in an SEM is
ultimately determined by
the size of the region
from which signal is
produced.
 Thus for the same
region of excitation the
resolution from the three
signals differs and
decreases from
secondary to backscatter
and X-X-rays.
Resolution and excitation region
If the region of excitation remains small then signal will be

produced from a small region and there will be no overlapping
from adjacent regions. In this case each individual spot is
resolved from its neighbors.
Even a slight increase in size of the region of signal

production can result in decreased resolution.
If the beam is scanned in exactly the same positions but

the region of excitation is larger then the regions of signal
production will also be larger and overlap with adjacent
ones. Such an image would therefore not be resolved
resolved..
Interaction volume are affected by
dB, EB and Zsamp
Factors affecting size of

the interaction region are:
 Diameter of the primary
beam dB
 Energy of the primary
beam EB
 Atomic weight of the
specimen Zsamp
 Coating of specimen

How dB, EB and Zsamp affect
the resolution
Resolution Interaction Beam Beam Atomic

Resolution Power, volume, diameter, energy, weight, Coating
RP Vint dB EB Zsamp
      thin, heavy
      thick, light

Affect of beam crossover
 Final primary beam probe size
dB from a field emitter is (10-
10-
100)x
100 )x smaller than that of a
conventional tungsten filament
or LaB6 emitter
emitter.. This is one
reason why FESEMs have the
best image resolution
resolution..
 FESEMs also tend to remain stable at very low accelerating

voltages (0.5 – 5 keV) resulting in shallow (nông
(nông)) regions of
excitation and thus higher image resolution.

Resolution and stigmatism
Overlapping of signal production is also the primary reason why it

is so critical to have the beam of an SEM properly stigmated.
Even if the size of the region is kept small, it is only those regions
which are perfectly circular that will produce the best resolution.

Astigmatic regions may not reduce image

resolution in one dimension.
But can still reduce resolution by overlapping

with adjacent regions.
Example 1: affect of coating
Chromium
Gold
Mycoplasma pneumonia sputtered by

Au gives better image than by Cr
Affect of
accelerated
Increasing E
voltage Increasing Z Z RP
and atomic
weight
E RP

Affect of accelerated voltage
and atomic weight
The relationship of accelerating voltage (Eo) to atomic weight

(Z) of the specimen and its affect on the depth of penetration
is in reverse order.
Example 2:
affect of accelerating voltage
3,0 keV 20,0 keV
At higher voltage image is brighter due to more signal

Example 3:
affect of accelerating voltage
3,0 keV 20,0 keV
But reduced resolution because of

larger interaction volume caused.
Resolution - cathode material -
voltage relationship

Electron-Sample Interaction, Scattering Process - Electron Microscopy and Diffraction

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Electron-Sample Interaction, Scattering Process - Electron Microscopy and Diffraction

Uploaded by

Copyright:

Available Formats

Do Minh Nghiep

Materials Science Center

 Interaction of primary beam and specimen

01.01.2009 Materials Science Center, HUT 2

01.01.2009 Materials Science Center, HUT 3

01.01.2009 Materials Science Center, HUT 4

 Monte Carlo simulations of electron trajectories are based on 1) the

Ec = 7 eV; Eo = 20 keV; r = 7 g.cm-3; d = 0.8 mm

01.01.2009 Materials Science Center, HUT 9

01.01.2009 Materials Science Center, HUT 10

Electron and photon signals give infos about

01.01.2009 Materials Science Center, HUT 11

01.01.2009 Materials Science Center, HUT 12

01.01.2009 Materials Science Center, HUT 14

01.01.2009 Materials Science Center, HUT 15

Elastic scattering Inelastic scattering

Auger electron Characteristic X-

A shell electron falls

01.01.2009 Materials Science Center, HUT 17

01.01.2009 Materials Science Center, HUT 18

01.01.2009 Materials Science Center, HUT 19

 Low energy electrons emitted from the upper 2-

An Auger spectrum for Aluminum showing peaks

01.01.2009 Materials Science Center, HUT 22

01.01.2009 Materials Science Center, HUT 23

Thick sample  The angle at which the beam

01.01.2009 Materials Science Center, HUT 27

01.01.2009 Materials Science Center, HUT 28

01.01.2009 Materials Science Center, HUT 29

Side mounted: deep image In

01.01.2009 Materials Science Center, HUT 30

SE detector system usually consists of 4 parts: (1) a Faraday cage,

Everhart -Thornley detector setup with

01.01.2009 Materials Science Center, HUT 32

A conventional secondary electron detector is positioned off to the side of the

01.01.2009 Materials Science Center, HUT 34

01.01.2009 Materials Science Center, HUT 35

01.01.2009 Materials Science Center, HUT 36

Most of the secondary electron detector lies outside of the SEM

01.01.2009 Materials Science Center, HUT 40

01.01.2009 Materials Science Center, HUT 41

01.01.2009 Materials Science Center, HUT 42

01.01.2009 Materials Science Center, HUT 45

The topography of the specimen will also affect the

Since backscattered electrons have a high energy they

The most common design is a four quadrant solid state

Two image modes:

01.01.2009 Materials Science Center, HUT 49

Blood cells with

01.01.2009 Materials Science Center, HUT 50

Gold particles on E. coli appear as bright white dots due to

Backscatter image of nickel in a leaf

Backscatter image of a composite (polished cement

01.01.2009 Materials Science Center, HUT 54

01.01.2009 Materials Science Center, HUT 55

Environmental electrons are a form of secondary electrons that

Movie of melting sample in ESEM

An environmental SEM or ESEM actually requires gas of

01.01.2009 Materials Science Center, HUT 62

01.01.2009 Materials Science Center, HUT 63

 Because of their high

01.01.2009 Materials Science Center, HUT 65

If the region of excitation remains small then signal will be