Topic 3b,c

Electron Microscopy
1.0 Introduction and History
• 1.1 Characteristic Information
2.0 Basic Principles
• 2.1 The Microscope Column
• 2.2 Signal Detection and Display
• 2.3 Operating Parameters

3.0 Instrumentation
• 3.1 Sample Prep
• 3.2 Handling

4.0 Examples
5.0 Correct Presentation of Results
1.0 Introduction and History
What are they and Where did
Electron Microscopes Come From?

o Electron Microscopes are scientific instruments

that use a beam of highly energetic electrons to
examine objects on a very fine scale.

o Electron Microscopes were developed due to the

limitations of Light Microscopes which are limited
by the physics of light to 500x or 1000x
magnification and a resolution of 0.2 µm.
1.0 Introduction and History
What are they and Where did
Electron Microscopes Come From?

o In the early 1930's this theoretical limit had been

reached and there was a scientific desire to see
the fine details of the interior structures of organic
cells (nucleus, mitochondria...etc.).

o This required 10,000x plus magnification which

was just not possible using current optical
microscopes.
 Dates

• The Transmission Electron Microscope (TEM) was the first

type of Electron Microscope to be developed and is patterned
exactly on the Light Transmission Microscope except that a
focused beam of electrons is used instead of light to "see
through" the specimen. It was developed by Max Knoll and
Ernst Ruska in Germany in 1931.
• The first Scanning Electron Microscope (SEM) debuted in
1938 ( Von Ardenne) with the first commercial instruments
around 1965. Its late development was due to the electronics
involved in "scanning" the beam of electrons across the
sample.
 Chronology

1897: J.J. Thompson - Discovers the electron

1924: Louis deBroglie
Identifies a wavelength to moving electrons - λ = h / mv
where: λ = wavelength, h = Planck's constant m = mass,
v = velocity (For an electron at 60kV, λ = 0.005 nm)
1926: H. Busch - Magnetic or electric fields act as lenses for
electrons
1929: E. Ruska - Ph.D thesis on magnetic lenses
1931: Knoll & Ruska - First electron microscope built

1931: Davisson & Calbrick - Properties of electrostatic lenses

1934: Driest & Muller - Surpass resolution of the OM

1938: von Borries & Ruska

First practical EM (Siemens) - 10 nm resolution

1940: RCA - Commercial EM with 2.4 nm resolution

 Microscopy and Related
Techniques

• Light (optical) microscopy (LM) or (OM)

• Scanning electron microscopy (SEM)
Energy dispersive X-ray spectroscopy (EDS)
& Wavelength dispersive X-ray spectroscopy
(WDS)
• X-ray diffraction (XRD)/X-ray fluorescence
(XRF)
• Transmission electron microscopy/
Scanning transmission electron
microscopy (TEM)/(STEM)

Surface Characterization Techniques

• Scanning probe microscopy (AFM & STM)
 1.1 Characteristic Information
o Topography
The surface features of an object or "how it looks", its
texture; direct relation between these features and
materials properties
o Morphology
The shape and size of the particles making up the object;
direct relation between these structures and materials
properties
o Composition
The elements and compounds that the object is composed
of and the relative amounts of them; direct relationship
between composition and materials properties
o Crystallographic Information
How the atoms are arranged in the object; direct relation
between these arrangements and materials properties
 Identification of Fracture Mode
Pores
Cracks Cracks
Grain
boundary

4µm 20µm

SEM micrographs of fractured surface of two BaTiO3

samples.
OM and SEM
How Fine can You See?

• Can you see a sugar cube? The thickness of a sewing

needle? The thickness of a piece of paper? …

• The resolution of human eyes is of the order of 0.1 mm,

100µm ≈ 4 mils.

• However, something vital to human beings are of sizes

smaller than 0.1mm, e.g. our cells, bacteria,
microstructural details of materials, etc.
 Microstructural Features
which Concern Us

• Grain size: from <µm to the cm regime

• Grain shapes

• Precipitate size: mostly in the µm regime

• Volume fractions and distributions of various

phases

• Defects such as cracks and voids: <µm to the cm

regime
Phase Contrast Microscopy - Phase contrast microscopy, first described
in 1934 by Dutch physicist Frits Zernike, is a contrast-enhancing optical
technique that can be utilized to produce high-contrast images of
transparent specimens such as living cells, microorganisms, thin tissue
slices, lithographic patterns, and sub-cellular particles (such as nuclei
and other organelles). In effect, the phase contrast technique employs an
optical mechanism to translate minute variations in phase into
corresponding changes in amplitude, which can be visualized as
differences in image contrast. One of the major advantages of phase
contrast microscopy is that living cells can be examined in their natural
state without being killed, fixed, and stained. As a result, the dynamics of
ongoing biological processes in live cells can be observed and recorded
in high contrast with sharp clarity of minute specimen detail.
http://www.microscopyu.com/tutorials/java/phasecontrast/microscopealignment/index.html
 Scale and Microscopy Techniques
XRD,TEM SEM OM
Crystal Structure Microstructure Component

Valve
Grain I Turbo
charge

Grain II

Fracture Mechanics
Structure Determination

atomic

Basic Research Applied Research

Microstructure ranging from crystal structure to

Engine components (Si 3N4)
 Advantages of Using SEM over OM
Mag Depth of Field Resolution
OM: 4x – 1000x 15.5mm – 0.19mm ~ 0.2mm
SEM: 10x – 500Kx 4mm – 0.4mm 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.
 2.1 The Microscope Column
General Layout

In simplest terms, an SEM is really nothing more than a

television. We use a filament to get electrons, magnets to
move them around, and a detector acts like a camera to
produce an image.
 Scanning Electron Microscope
Virtual Source 1)
First Condenser Lens 2)
Condenser Aperture
Second Condenser Lens

Objective Aperture
Scan Coils

Objective Lens

Sample
1) The "Virtual Source" at the top represents the electron
gun, producing a stream of monochromatic electrons.

2) The stream is condensed by the first condenser lens

(usually controlled by the "coarse probe current knob"). This
lens is used to both form the beam and limit the amount of
current in the beam. It works in conjunction with the
condenser aperture to eliminate the high-angle electrons
from the beam.
 Scanning Electron Microscope
Virtual Source

First Condenser Lens

Condenser Aperture 3)
Second Condenser Lens
4)
Objective Aperture 5)
Scan Coils

Objective Lens

Sample

3) The beam is then constricted by the condenser aperture

(usually not user selectable), eliminating some high-angle
electrons.
4) The second condenser lens forms the electrons into a thin,
tight, coherent beam and is usually controlled by the "fine
probe current knob".
5) A user selectable objective aperture further eliminates
high-angle electrons from the beam.
 Scanning Electron Microscope
Virtual Source

First Condenser Lens

Condenser Aperture
Second Condenser Lens

Objective Aperture
6) Scan Coils
7) Objective Lens

8)
Sample

6) A set of coils then "scan" or "sweep" the beam in a grid

fashion (like a television), dwelling on points for a period of
time determined by the scan speed (usually in the
microsecond range).
7) The final lens, the Objective, focuses the scanning beam
onto the part of the specimen desired.
8) When the beam strikes the sample (and dwells for a few
microseconds) interactions occur inside the sample and are
detected with various instruments.
 Scanning Electron Microscope
9) Before the beam moves to its next dwell point these
instruments count the number of interactions and display a
pixel on a CRT whose intensity is determined by this number
(the more reactions the brighter the pixel).

10) This process is repeated until the grid scan is finished

and then repeated, the entire pattern can be scanned 30
times/sec.

Virtual Source

First Condenser Lens

Condenser Aperture
Second Condenser Lens

Objective Aperture
Scan Coils

Objective Lens

Sample
 Parts of the Microscope
1. Electron optical column consists of:
– electron source to produce
electrons
– magnetic lenses to de-magnify the
beam
– magnetic coils to control and
modify the beam
– apertures to define the extent of
beam, prevent electron spray, etc.
2. Vacuum systems consists of:
– chamber which “holds” vacuum
– pumps to produce vacuum
– valves to control vacuum
– gauges to monitor vacuum
 Parts of the Microscope
3. Signal Detection & Display
consists of:
– detectors which collect the
signal
– electronics which produce an
image from the signal
A Look Inside the Column

Electron gun
Gun Alignment Control

Pneumatic Air Lock Valve

Condenser Lens
Objective Aperture
Scanning Coil
Objective Lens

Motorized Stage

Sample Chamber
 Getting a Beam

• A filament is heated to a high T to emit electrons.

• A bias (of up to 45 kV) between the filament and a target

material draws the electrons to an anode.

• Up to this point, the process is identical to that used to

form x-rays. However, instead of striking a target to form
x-rays, the electrons are drawn towards an anode, where
they go through a hole, forming a beam.

• This beam is attracted through the anode, condensed by

a condenser lens, and focused as a very fine point on the
sample by the objective lens.
Electron Beam Source

Single Crystal LaB6

Heating Cup

Heating Wire (W or Re)

Support Posts

Lanthanum Hexaboride Single

Crystal Filament

W / LaB6 (Filament)
Thermionic or Cold Cathode (Field Emission Gun)
 Field Emission Gun
• The tip of a tungsten needle is made very sharp (radius < 0.1 µm)

• The electric field at the tip is very strong (> 107 V/cm) due to the sharp
point effect

• Electrons are pulled out from the tip by the strong electric field

• Ultra-high vacuum (better than 10-6 Pa) is needed to avoid ion

bombardment to the tip from the residual gas.

• Electron probe diameter < 1 nm is possible

 Electromagnetic Lenses
Lorentz force equation:
F = q0v x B

Two components to
the B field:
Nonaxial electrons will experience a force BL = longitudinal component
both down the axis and one radial to it. Only (down the axis)
BR= radial component
electrons traveling down the axis feel equal
(perpendicular to axis)
radial forces from all sides of the lens. The
unequal force felt by the off-axis electrons
causes spiraling about the optic axis.
after "Electron Beam Analysis of Materials", M.H. Loretto
 Electromagnetic Lenses

• Condenser lens – focusing determines the beam current

which impinges on the sample.

• Objective lens – final probe forming

• The objective lens determines the final spot size of the

electron beam, i.e., the resolution of a SEM.
 Electromagnetic Lenses
The Condenser Lens

• For a thermionic gun, the diameter of the first cross-

over point ~20-50µm.

• If we want to focus the beam to a size < 10 nm on the

specimen surface, the magnification should be ~1/5000,
which is not easily attained with one lens (say, the
objective lens) only.

• Therefore, condenser lenses are added to demagnify

the cross-over points.
 Electromagnetic Lenses
The Objective Lens
• The objective lens controls the final focus of the electron
beam by changing the magnetic field strength

• The cross-over image is finally demagnified to an ~10nm

beam spot which carries a beam current of approximately
10-9 - 10-13 A.

Scanning Coils

Stigmator
Beam-Limiting
Aperture
 Electromagnetic Lenses
The Objective Lens - Focusing
• By changing the current in the objective lens, the magnetic
field strength changes and therefore the focal length of the
objective lens is changed.

Objective
lens

Out of focus lens In focus lens Out of focus lens

current too strong current optimized current too weak
 Electromagnetic Lenses
The Objective Lens - Stigmator

• The objective lens is machined to very high precision and the

magnetic field pattern is very carefully designed.

• However, the precision attainable by machining cannot match

that required for controlling a beam with a 10 nm diameter.

• The stigmator, which consist of two pairs of pole-pieces

arranged in the X and Y directions, is added to correct the
minor imperfections in the objective lens.
 Electromagnetic Lenses
The Objective Lens - Aperture
• Since the electrons coming from the electron gun have spread in
kinetic energies and directions of movement, they may not be focused
to the same plane to form a sharp spot.

• By inserting an aperture, the stray electrons are blocked and the

remaining narrow beam will come to a narrow “Disc of Least
Confusion”
Electron beam

Objective
lens
Wide Narrow
aperture aperture
Narrow disc of least
Wide disc of confusion
least confusion

Large beam diameter

striking specimen Small beam diameter
striking specimen
 Electron vs. Optical Lenses
• e-’s don’t actually touch the lens
No definite interface
• e-’s rotate in the magnetic field
• e-’s repel each other
• f∝ H∝ I
- Focus and magnification controlled
electronically
- No physical movements
• e- lenses can only be positive elements
(converging)
• Can’t correct e- lens aberrations like you can
with compound optical lenses
• e- lenses always operate at small apertures
H = MFS
 Comparison of OM,TEM and SEM
Source of (Cathode Ray
Light source electrons Tube)
Condenser
Magnetic
Specimen lenses
Objective

Projector Specimen CRT

Eyepiece

Image Viewed Image on detector

Directly Fluorescent Screen
Transmission Scanning
Light Microscope
Electron Microscope Electron Microscope

Principal features of an optical microscope, a

transmission electron microscope and a scanning
electron microscope, drawn to emphasize the similarities
of overall design.
 2.2 Signal Detection and Display
When an electron beam strikes a sample, a large
number of signals are generated.
Incident e- Beam
Backscattered e-
Foil (TEM)Bulk (SEM)

X-rays Cathodaluminescence

Auger e- Secondary e-

Interaction
Volume Sample

Inelastically Scattered e- Elastically Scattered e-

Unscattered e-

Transmitted Electrons
We can divide the signals into two broad categories:
a) electron signals, b) photon signals
Electron Detectors and Sample Stage

Objective
lens

Sample stage

Example
Specimen Interaction
Volume

The volume inside the specimen in which interactions

occur while being struck with an electron beam. This
volume depends on the following factors:

• Atomic number of the material being examined; higher

atomic number materials absorb or stop more electrons
and so have a smaller interaction volume.

• Accelerating voltage: higher voltages penetrate farther

into the sample and generate larger interaction volumes

• Angle of incidence for the electron beam; the greater the

angle (further from normal) the smaller the volume
 Specimen Interaction Volume
Below is an example of a typical Interaction volume for:
• Specimen with atomic number 28, 20 kV
• 0° degrees tilt, incident beam is normal to specimen surface
noting the approximate maximum sampling depths for the
various interactions.

Electron Beam Augers 10Å to 30Å

Secondaries 100Å Backscattered <1-2µm

5 µm Range of K X-rays
Range of L X-rays
Range of Electron Penetration
At 20 KV Accelerating Voltage and Z = 28
 Beam Interaction Simulations
Theoretical SrS density: 3.7g/cm3, Long. range: 1062 Å, Long. straggle: 384 Å

SrS
5000 Å
Si 5000 Å SrS
Si

10 kV
2 µm 1 µm
15 kV

SrS SrS
5000 Å
2 kV
5 kV Si

2 µm 0.5 µm
5000 Å
 Signal Detection
and Display
• If you change the target material, the high and low
energy peaks remain (although their intensity may
change) while the low intensity peaks change position
and are characteristic of the sample.

• The reason we produce this type of profile is because

the incident electrons we send into the sample are
scattered in different ways.

• There are two broad categories to describe electron

scattering:
– elastic: Backscattered electrons
– inelastic: Secondary electrons
Electron Detectors

Objective
lens
Example
 Secondary Electrons
These electrons arise due to inelastic collisions between
primary electrons (the beam) and loosely bound electrons
of the conduction band (more probable) or tightly bound
valence electrons. The energy transferred is sufficient to
overcome the work function which binds them to the solid
and they are ejected.
Electron Orbitals
Incident e-

The interaction is Coulombic in nature and the ejected

electrons typically have ˜ 5 - 10 eV. 50 eV is an arbitrary
cut-off below which they are said to be secondary
electrons.
 Detection
Remember, secondary electrons are low energy electrons.
We can easily collect them by placing a positive voltage (100
- 300V) on the front of our detector. Since this lets us collect
a large number of the secondaries (50 - 100%), we produce a
“3D” type of image of the sample with a large depth of field.

The type of detector used is called a scintillator / photo-

multiplier tube.
 Detection Sequence
Scintillator / Photomultiplier
Al coated E field
Scintillator Light Guide
6-12 kV
(3) (5)
(2)
(1) (4)

Grid Photocathode Dinodes multiply

Photons the number of
100 - 500 v emits electrons electrons
1. Secondary electrons (SE) are accelerated to the front of
the detector by a bias voltage of 100 - 500 eV.

2. They are then accelerated to the scintillator by a bias of 6

- 12 keV, (10 KeV is normal).

3. Scintillator is doped plastic or glass covered with a

fluorescent material (e.g. Europium). A thin (700Å) layer
of Al covers it to prevent light from causing fluorescence.
The 10keV potential allows the SE to get through the Al
and fluoresce.
 Detection Sequence

Scintillator / Photomultiplier
Al coated E field
Scintillator Light Guide
6-12 kV
(3) (5)
(2)
(1) (4)

Grid Photocathode Dinodes multiply

Photons the number of
100 - 500 v emits electrons electrons

4. The light photons travel down the tube (guide) to a photo-

cathode which converts them into electrons
5. The electrons move through the detector, producing
more electrons as they strike dinodes. An output
electron pulse is then detected.
 Backscattered Electrons
Backscattered electrons (BSE) arise due to elastic collisions
between the incoming electron and the nucleus of the target
atom (i.e. Rutherford scattering). Higher Z, more BSE
emitted.
e-

Nucleus

As the name implies, elastic scattering results in little (< 1 eV)

or no change in energy of the scattered electrons, although
there is a change in momentum (p). Since p = mv and the
mass of the electron doesn’t change, the direction of the
velocity vector must change. The angle of scattering can
range from 0 to 180°.
 Detection
Since BSE have high energies, they can’t be pulled in like
secondaries. If you placed a potential on a grid to attract
them, you would also attract the incident beam!!

The most common detector used is called a surface

barrier detector. It sits above the sample, below the
objective lens. BSE which strike it are detected.

Polepiece
Backscattered
Electrons
Top Annular Backscattered
Contact Electron Detector
Thin Au Layer
Electron - Hole Production
Si P - N Junction

Base Contact

Current Monitor in External Circuit

 Detection Sequence
Surface barrier detectors are solid state devices made up of
semiconducting materials. A semiconducting material has
a filled valence band and an empty conduction band- similar
to ceramic materials.
1. When a BSE electron strikes the detector, electrons in
the material move from valence to conduction band.
2. The electrons are now free to move in the conduction
band or drop back into the valence band.

(1)

(2)
(3)
 Detection Sequence

⊕
3. If a potential is applied, the e- and e+ can be separated,
collected, and the current measured. The strength of the
current is proportional to the number of BSE that hit the
detector.

(1)

(2)
(3)
 2.3 Operating Parameters
Magnification
An image is obtained by taking the signal from the sample
and transferring it to a CRT screen. By decreasing the size
of the scanned area (from which we get the signal),
magnification is produced.
L
l Mag. Area
Information 10x (1cm)2
transferred 100x (1mm)2
1Kx (100 µm)2
10Kx (10 µm)2
Scanned Area 100Kx (1 µm)2
Console CRT 1Mx (100 nm)2
Magnification is determined by taking the ratio of the
lengths of the scans:
Mag. = L/I
 Resolution

Resolution is the ability to resolve two closely spaced points.

While you may have to be at a high magnification to see small
features, resolution is NOT the same as magnification.

One way to improve resolution is by reducing the size of the

electron beam that strikes the sample:
dmin = 1.29Cs1/4λ3/4[7.92 (iT/Jc)x109 + 1]3/8
at low current:
dmin = 1.29Cs1/4λ3/4
Jc = current density of the source, λ = electron wavelength
Cs = spherical aberration, i = current, T = temperature,
 Resolution

We can also improve the resolution by:

• Increasing the strength of the condenser lens

• Decreasing the size of the objective aperture

• Decreasing the working distance (WD = the distance the

sample is from the objective lens)
 Depth of Field (I)

The height over which a sample can be clearly focused is

called the Depth of Field. The SEM has a large depth of
field which produces the images that appear 3-dimensional
in nature.

Depth of field is improved by:

• Longer working distance

• Smaller objective apertures

• Lower magnifications
Depth of Field (II)
A beam having a semi-angle of convergence α
will converge from a radius r to a focus and
diverge again in a vertical distance D. For
small α :
D = 2r / α
In a current high-resolution CRT’s (spot size
=0.1 mm = 100 microns), the focusing
becomes objectionable when two pixels are
fully overlapped, where the pixel size on the
specimen is 0.1/M mm, where M is the
magnification, which gives us the practical
expression for the depth of focus/field:

D ≈ 0.2 / αM (mm)
 Depth of Field (III)

The angle α is determined by:

α = R/WD
R = radius of the aperture used, and WD is the
working distance of the aperture from the specimen.
 Depth of Field vs. Resolution

As for the optical microscope, the depth of field

and resolution have a reciprocal relationship:

• Improving resolution in conventional SEM’s

leads to a smaller depth of field

• While increasing depth of field decreases

resolution.useful for each particular sample.
3.0 Instrumentation

JEOL 6700F Ultra High Resolution

Scanning Electron Microscope
3.1 Sample Preparation
Sample Coating
Q: Why ?
A: Charging:

• Deflection of SE’s
• Increased emission of SE’s in cracks
• Periodic SE bursts
• Beam deflection

Solutions:
• Sputter coating with C, Cr, or Au-Pd

• Carbon tape, carbon paint, In foil

 How It Works

• e-’s are ejected from negative target

• e-’s are accelerated toward the

positive anode

• e-’s may collide with gas molecules

(Ar) and ionize, forming Ar+

• The Ar+ ions are accelerated toward the negative

target

• The target material is sputtered

 Sputtering:
A Physical Process ?
Vacuum Chamber

Anode

Negative target Ar +
Ar +

Ar ionized

Sample to be coated
Cathode
Etching and Coating

Gatan PECS Model #682

 Beam Interaction Simulations
Theoretical SrS density: 3.7g/cm3, Long. range: 1062 Å, Long. straggle: 384 Å

SrS
5000 Å
Si 5000 Å SrS
Si

10 kV
2 µm 1 µm
15 kV

SrS SrS
5000 Å
2 kV
5 kV Si

2 µm 0.5 µm
5000 Å
 Random interactions with target atoms
Ion, dose, energy

Longitudinal range
∆Rp
Rp

Longitudinal Straggle

From LSS Theory: R 2 Rp M i MT

Rp ≅ ∆Rp ≅
 MT  3 M i + MT
1+  
 3 M i
 Cathodoluminescence (CL)
CL Imaging at 15 kV, 10kX - 1kX
CL Intensity vs. Wavelength Sample: 1x1019cm-3
1
1x10^17

1x10^18 light pipe

1x10^19
0.8
Normalized CL Intensity

Te implanted
Sample
λ = 420 nm, 15 kV
0.6

0.4

420 nm
0.2 (doublet)
360 nm
(singlet)
0
300 350 400 450 500 550 600

Wavelength (nm)
10 µm
 LSS Theory of Ion Stopping

LSS: Linhard, Scharff & Schiott

Rp

Nuclear Stopping: Coulombic Scattering Electronic Stopping

m1 v1
m1
v0
m1
m2 +
m2 v2
 Nuclear Stopping

 dE 
Sn ( E ) = 
Energy loss per distance traveled as
a function of energy: 
• depends on incident ion and target
 dx  n
atom nuclear charge (Z = # protons)
and atomic masses (M)
Energy loss due to interactions with atomic nuclei is basically a
decreasing function of energy. At high kinetic energy (ion velocity)
there is a very short interaction time for any absorption of energy by
target atoms.
Approximate nuclear stopping near max of S n(E):
Sn(E) dE 2
π 2 Z1 Z 2 M 1
= Sn = N e a
Sn dx( n) 2 M1 + M 2
where
N is the atomic density (atoms/Volume)
a ~ 1.4x10 - 2 nm, subscripts1 and 2 refer to ion
E and target respectively, Z is atomic number
and M is mass number
 Electronic Stopping

Due to interactions with electrons in the target material

- like a drag force that is proportional to the ion velocity
Ion velocity α (Energy)1/2

 dE 
Se ( E ) =   ∝ E 1/ 2
= k e E 1/ 2
 dx  e
where ke is relatively independent of the incident ion

For silicon: ke ~ 107(ev)1/2/cm

Total rate of energy loss = dE/dx = Sn(E) + Se(E)

 LSS Calculations

ε & ρ are dimensionless parameters

ε α energy
ρ α range (R) (distance variable)

“like”
dE/dx
 Nuclear & Electronic Stopping

Electronic stopping dominates:

Light ions and high energies

Nuclear stopping dominates:

Heavy ions and low energies

Implant damage occurs due to *

nuclear interactions. The
extent of damage depends on
Sn(E).
Artifacts and Examples

• Thermal damage
- Sample temperature can rise up
to 40°C

• Surface Etching

• Coating Film Adhesion

- Not sticking, temperature sensitive

• Contamination

• Morphology Modification
Ag powders written by a laser on glass

Ag powders - Cerac, 190 nm average

Ag powders written by a laser on glass

Ag powders - SMP, 400 nm average

Silica Spheres, 0.5 µm, Hereisus
Space Shuttle Tile

100 µm 100 µm

10 µm 1 µm
Space Shuttle Tile

100 nm 100 µm

10 µm 10 µm
BTO and Ag powders written by a laser on Kapton
BTO and Ag powders written by a laser on Kapton

BTO sol gel matrix with BTO powders

BTO and Ag powders written by a laser on Kapton
 Summary
• The basic layout and operation of an SEM.

• The different imaging modes of the SEM.

• How an image is obtained

• Sample preparation

• Materials

• Vacuum levels

• Information: Imaging, EDS, WDS, EBL, beam

current
 Typical Thermionic Gun
A Thermionic Electron Gun functions in the following manner:

1) An positive electrical potential is applied to the anode.

2) The filament (cathode) is heated until a stream of electrons is

produced.

3) The electrons are then accelerated by the positive potential down the
column.

4) A negative electrical potential (~500 V) is applied to the Whenelt Cap.

5) As the electrons move toward the anode any ones emitted from the
filament's side are repelled by the Whenelt Cap toward the optic axis
(horizontal center).
 Typical Thermionic Gun
Cont’d
6. A collection of electrons occurs in the space between the filament tip
and Whenelt Cap. This collection is called a space charge

7. Those electrons at the bottom of the space

charge (nearest to the anode) can exit the gun area through the small (<1
mm) hole in the Whenelt Cap

8. These electrons then move down the column to be later used in

imaging

This process insures several things:

• That the electrons later used for imaging will be
emitted from a nearly perfect point source (the
space charge)
• The electrons later used for imaging will all have
similar energies (monochromatic)
• Only electrons nearly parallel to the optic axis will be allowed out of the
gun area
Other Bulk Specimen Interactions
X-rays
Source
Caused by the de-energization of the specimen atom after a
secondary electron is produced. Since a lower (usually K-shell)
electron was emitted from the atom during the secondary electron
process an inner (lower energy) shell now has a vacancy. A higher
energy electron can "fall" into the lower energy shell, filling the
vacancy. As the electron "falls" it emits energy, usually X-rays to
balance the total energy of the atom.
Utilization
X-rays or Light emitted from the atom will have a characteristic energy
which is unique to the element from which it originated. These signals
are collected and sorted according to energy to yield micrometer
diameter) of bulk specimens limiting the point-to-point comparisons
available (see Interaction Volume).
 Characteristic X-rays and Auger Electrons

We’ve already discussed

how an electron collision
can create an x-ray that is
N characteristic of the sample.

Auger

This same process also x -r a y

produces Auger ∆E
electrons
N

Generally, in the SEM we are only concerned with the

characteristic x-ray signal.
Other Bulk Specimen Interactions
Auger Electrons
Source
Caused by the de-energization of the specimen atom after a
secondary electron is produced. Since a lower (usually K-shell)
electron was emitted from the atom during the secondary electron
process, an inner (lower energy) shell now has a vacancy.

A higher energy electron from the same atom can "fall" to a lower
energy, filling the vacancy. This creates an energy surplus in the atom
which can be corrected by emitting an outer (lower energy) electron;
an Auger Electron.

Utilization
Auger Electrons have a characteristic energy, unique to each element
from which it was emitted from. These electrons are collected and
sorted according to energy to give compositional information about
the specimen. Since Auger Electrons have relatively low energy they
are only emitted from the bulk specimen from a depth of <3 nm (see
Interaction volume).
 Thin Specimen Interactions
Unscattered Electrons

Source

• Incident electrons which are transmitted through the thin specimen

without any interaction occurring inside the specimen.

Utilization

• The transmission of unscattered electrons is inversely proportional to

the specimen thickness.

• Areas of the specimen that are thicker will have fewer transmitted
unscattered electrons and so will appear darker.

• Conversely the thinner areas will have more transmitted and thus will
appear lighter.
 Thin Specimen Interactions
Elastically Scattered electrons
Source
Incident electrons that are scattered (deflected from their original
path) by atoms in the specimen in an elastic fashion (no loss of
energy). These scattered electrons are then transmitted through
the remaining portions of the specimen.
Utilization
All electrons follow Bragg's Law and thus are scattered according
to Wavelength=2*Space between the atoms in the specimen*sin
(angle of scattering). All incident electrons have the same energy
(thus wavelength) and enter the specimen normal to its surface. All
incidents that are scattered by the same atomic spacing will be
scattered by the same angle. These "similar angle" scattered
electrons can be collated using magnetic lenses to form a pattern
of spots; each spot corresponding to a specific atomic spacing (a
plane). This pattern can then yield information about the
orientation, atomic arrangements and phases present in the area
being examined.
 Thin Specimen Interactions
Inelastically Scattered Electrons

Source
Incident electrons that interact with specimen atoms in a inelastic
fashion, loosing energy during the interaction. These electrons are
then transmitted trough the rest of the specimen

Utilization
Inelastically scattered electrons can be utilized two ways
•Electron Energy Loss Spectroscopy: The inelastic loss of energy by
the incident electrons is characteristic of the elements that were
interacted with. These energies are unique to each bonding state of
each element and thus can be used to extract both compositional and
bonding (i.e. oxidation state) information on the specimen region
being examined.
•Kakuchi Bands: Bands of alternating light and dark lines that are
formed by inelastic scattering interactions that are related to atomic
spacings in the specimen. These bands can be either measured (their
width is inversely proportional to atomic spacing) or "followed" like a
roadmap to the "real" elasticity scattered electron pattern.
 Characteristic X-rays
1) Core electron is knocked out

2) Outer shell electron drops down

3) Energy difference is emitted as an X-Ray

4) Electron shells have discreet energy levels

5) The X-Ray energy is characteristic of the particular element in question

(energy levels)

X-Ray Detection: X-Ray intensity is ∝ Z

• Two types of detectors:

a) Wavelength dispersive:
- Separates X-Rays by wavelength
b) Energy Dispersive (EDXA, EDS, EDX):
- Separates X-Rays by energy
- Can monitor one energy
 Characteristic X-rays

Energy-level diagram for an atom, illustrating the excitation

of the K, L, M, and N shells and the formation of Kα, Kβ, Lα,
and Mα x-rays.
 X-ray Detection I

(2)
(4)
(1)

(3)

1. X-rays enter the detector and strike a Si crystal, creating e - / ⊕ pairs.

The number of e - / ⊕ pairs is related to the energy of the incoming x-
ray.
2. A potential is placed across the crystal to cause the e- to move to
the + side and the ⊕ to move to the - side, producing a charge pulse.
3. The charge pulse is amplified and sorted. The size of the pulse is
again a function of the energy of the incoming x-ray.
4. The number pulses are plotted as a function of pulse size (which =
energy of the x-ray).
 Charge to Voltage Conversion
Process

(a) Representation of the detector charge-to-voltage converter, and pulse-

shaping linear amplifier from an electronic perspective. (b) Output of the
charge-to-voltage converter after the detection of a series of x-ray
photons.