Scanning Electron Microscopy

 Instrument
 Imaging
 Chemical Analysis (EDX)

 Structural and Chemical Analysis of Materials

J.P. Eberhart
John Wiley & Sons, Chichester, England, 1991.
 Scanning Electron Microscopy and X-Ray Microanalysis
J. Goldstein, D. Newbury, D. Joy, C. Lyman, P. Echlin, E. Lifshin, L. Sawyer, J. Michael
Kluwer Academic/Plenum Publishers, New York, 2003.
1. A column which generates a beam of
electrons.
2. A specimen chamber where the electron 1
beam interacts with the sample.
4
3. Detectors to monitor the different signals
3
2
that result from the electron beam/sample
interaction.
4. A viewing system that builds an image
from the detector signal.
Reduced image
of crossover

Project the
crossover image
onto the
specimen

X-Y translation +
rotation
SEM
 Image not formed by focusing of lenses  X-ray maps can be displayed.
 Resolution not limited by lens aberrations
(in the usual sense of image forming lenses  is limited by the objective lens aberrations
which determines the minimum probe size).
 Imaging involves digital processing
 online image enhancement and offline image processing.

 Resolution limited by probe size and beam spreading on interaction with

specimen.
 Hence, resolution depends on the signal being used for the formation of the
image.
 A fine electron probe is scanned over the specimen.
 Various detectors (Secondary Electron (SE), Back Scattered Electron (BSE), X-
Ray, Auger Electron (AE) etc.) pick up the signals.
 The amplified output of a detector controls the intensity
 of the electron beam of a CRT (synchronized scanning)
 of the pixel of display

Various Detectors
Scanning Electron Beam Display on CRT
(SE, BSE, EDX, AE)
Note that the resolution
depends on the type of
signal being used

Parameter Values
Resolution ~ 40 Å (SE); ~ (100-500) Å (BSE)
Magnification 10 – 105 
Depth of field High (~ m) Importance of SEM

Size of specimen 1 – 5 cm (usual range)

Many signals are generated by the interaction of the electron beam with the specimen. Each of
these signals is sensitive to a different aspect of the specimen and give a variety of information
about the specimen.

Incident
High-kV Beam Secondary
Backscattered Electrons (SE)
Electrons (BSE)
Characteristic
X-rays
Auger Electrons
Bremsstrahlung X- rays

Visible Light

Absorbed Electrons SPECIMEN Electron-Hole Pairs

In a SEM these signals are absent

Elastically Inelastically
Scattered Electrons Direct Scattered Electrons
Beam
Signals
An important point to note is the fact that the different signals are generated ‘essentially*’ from
different regions in the specimen. This determines:  as to what the signal is sensitive to  the
intensity of the signal.

Not to scale

• The X-rays generated by the electrons are the “Primary X-rays”

• The primary X-rays can further lead to electronic transitions which give rise to the “Secondary X-rays” (Fluorescent
X-rays)

 Interaction volume  volume which the electrons interact with

 Sampling volume  volume from which a particular signal (e.g. X-rays) originates
* Monte Carlo simulations are used to find the trajectory of electrons in the specimen and determine the probability of various processes
 X-ray fluorescence and Auger electrons

1
3-10 keV
e− Electron from beam knocks out a core electron

Photoelectrons

Transition from higher energy level to

fill core level
3

Generation of x-rays accompanying the transition

Further the x-ray could knock out an

electron from an outer level → this
electron is called the Auger electron
 Photoluminescence
Electron-hole pairs and cathodoluminescence  Photon induced light emission

e Incident electron excites an electron from the valence band Cathodoluminescence

to the conduction band → creating an electron hole pair  Electron induced light emission

Conduction band e
Semiconductors
Band gap

Valence band hole

Cathodoluminescence (CL) Spectroscopy

h

Electron beam induced current ( EBIC)

Bias
OR  Charge collection microscopy
Secondary Electrons (SE)

 Produced by inelastic interactions of high energy electrons with valence electrons of

atoms in the specimen which cause the ejection of the electrons from the atoms.
 After undergoing additional scattering events while traveling through the specimen, some
of these ejected electrons emerge from the surface of the specimen.
 Arbitrarily, such emergent electrons with energies less than 50 eV are called secondary
electrons; 90% of secondary electrons have energies less than 10 eV; most, from 2 to 5
eV.
 Being low in energy they can be bent by the bias from the detector and hence even those
secondary electrons which are not in the ‘line of sight’ of the detector can be captured.
 Secondary Electrons

Some Z contrast!

SE are generated by 3 different mechanisms:

 SE(I) are produced by interactions of electrons from the incident beam with specimen
atoms
 SE(II) are produced by interactions of high energy BSE with specimen atoms
 SE(III) are produced by high energy BSE which strike pole pieces and other solid objects
near the specimen.
http://www.emal.engin.umich.edu/courses/semlectures/se1.html
Back Scattered Electrons (BSE)

 Produced by elastic interactions of beam electrons with nuclei of atoms in the specimen
 Energy loss less than 1 eV
 Scattering angles range up to 180°, but average about 5°
 Many incident electrons undergo a series of such elastic event that cause them to be
scattered back out of the specimen
 The fraction of beam electrons backscattered in this way varies strongly with the atomic
number Z of the scattering atoms, but does not change much with changes in E0.

nBSE

nIE

 Dependence on atomic number  BSE images show atomic number contrast

(features of high average Z appear brighter than those of low average Z)

http://www.emal.engin.umich.edu/courses/semlectures/se1.html
Detectors
Note that SE not in traveling in the line of
sight can also be captured by the detector

Secondary Electrons

Backscattered Electrons
Magnification

 The magnification in an SEM is of ‘Geometrical origin’

(this is unlike a TEM or a optical microscope)
 Probe scans a small region of the sample, which is projected to a large area
(giving rise to the magnification).

Area scanned on
specimen

Area projected
onto display
Depth of field

 Dependent on the angle of convergence of the beam

 Depth of field is the same order of magnitude as the scan length
 Magnification  10,000 
 Scan length  10 m
 Depth of Field  8 m
What determines the resolution in an SEM?
 Probe size (probe size is dependent on many factors)
 Signal being used for imaging
This is because the actual interaction volume/cross section is different from the
probe diameter. Additionally, each signal is sensitive to a different aspect of the
specimen.

 In terms of parameters:
 Accelerating voltage
 Beam current
 Beam diameter
 Convergence angle of beam
Topographic Contrast in SEM

Inclination Effect

Shadowing Contrast Line of sight with the detector

Edge/Spike Contrast
Operating parameters affecting signal quality

Accelerating Voltage

Probe Current

Working Distance

Specimen Tilt

Aperture Size

Edge effect

Contamination

Charging
 Operating Parameter Values
Gun voltage ~20 keV

Working distance ~26 mm

Probe size W filament ~30 Å

LaB6
Field Emission

Vacuum W filament 10−5 Torr

LaB6 10−8 Torr

Field Emission 10−10 Torr

 Probe current   Probe diameter   Resolution 

 This leads to decrease in image intensity  we have to use a brighter source
(W filament < LaB6 < Field Emission gun)
 Comparison of Electron Sources at 20kV

Units Tungsten LaB6 FEG (cold) FEG FEG

(thermal) (Schottky)
Work eV 4.5 2.4 4.5 - -
Function
Operating K 2700 1700 300 - 1750
Temperature
Current A/m2 5*104 106 1010 - -
Density
Crossover μm 50 10 <0.005 <0.005 0.015-0.030
Size
Brightness A/cm2 sr 105 5 × 106 108 108 108
Energy Speed eV 3 1.5 0.3 1 0.3-1.0

Stability %/hr <1 <1 5 5 ~1

Vacuum PA 10-2 10-4 10-8 10-8 10-8

Lifetime hr 100 500 >1000 >1000 >1000

Increasing Resolution
 strength of condenser lens
 Probe size
 Working Distance
Probe Current Leads to  Beam convergence angle   spherical aberration

Working Distance

Specimen Tilt

Aperture Size

Edge effect

Contamination

Charging
Image Processing

Any signal picked up by a detector can be converted to an electrical signal

and be used of imaging
 Contrast processing  +ve to –ve contrast, gamma control etc.
 Contrast quantification  contour mapping, colour mapping
 Image integration  signal integration over a number of scans ( SNR)
 Usual image analysis  phase fractions etc.
 Backscattered Electron Images

 Emission of Backscattered electrons

= f(composition, surface topography, crystallinity, magnetism of the specimen)
 Composition  Z number
 Topography and composition information is separated using detector
 Crystallinity  channeling contrast (& EBSD)
(the BSE intensity changes drastically on or around Bragg’s condition)
 Poorer spatial resolution
Backscattered Electron Signals
Detectors

Signal A

Signal B

A+B

A−B

Composition (COMPO) Topography (TOPO)

 COMPO: A + B TOPO: A − B

Specimen: Metallic 20 kV, 1100 

Ref: SEM Manual, JEOL
Secondary Electron Image (SEI) Backscattered Electron Image (BEI)

X-ray image (Si) X-ray image (Al)

Specimen: Metallic 20 kV, 1100 

Composition via:  BEI  EDX Ref: SEM Manual, JEOL
www.nanoed.org/courses/zheng_electron/Dravid_part2.pdf
 High Resolution  Unclear surface structures
 More edge effect
 More charge-up
 More damage

Accelerating
Voltage

 Clear surface structures  Low resolution

 Less damage
 Less charge-up
 Less edge effect
 Low atomic number High atomic number

Low
accelerating
voltage

High
accelerating
voltage
 2500 

5 kV
30 kV

Specimen: Toner
 Accelerating voltage
 Increased contribution of BSE
 Low surface contrast
 Charging

Ref: SEM Manual, JEOL

 7200 

5 kV 25 kV

Specimen: Sintered powder

 Accelerating voltage
 Better surface contrast
 Not sharp at high magnifications
  WD or  probe diameter
Ref: SEM Manual, JEOL
 36000 

25 kV

5 kV

Specimen: Evaporated Au particles

 Accelerating voltage
 Better image sharpness
 Improved resolution

Ref: SEM Manual, JEOL

 2500 

25 kV

5 kV

Specimen: Paint coat

 Accelerating voltage
 Low surface contrast
 More BSE  contributions
from within the specimen

Ref: SEM Manual, JEOL

 Specimen tilt 5kV, 1100 

0

45 

Specimen: IC chip
TILT
 Improve quality of SE images
 complete survey of topography
 Stereo images  images at 2 angles
Ref: SEM Manual, JEOL
 Smooth image  Deteriorated resolution
 More damage

Probe current

 High-resolution obtainable  Grainy image

 10 kV, 5400 

1 nA

0.1 nA

Specimen: Ceramic
 Probe current
  image sharpness
10 pA   surface smoothness

Ref: SEM Manual, JEOL

  Greater depth of field  Low resolution

Working Distance
working distance 
 spherical aberration   Low depth of field
(spot size 
working distance 
 resolution improves)
 Depth of field 
 High resolution
(wide cone of electrons)

The working distance is the distance between the final condenser lens and the specimen
  Large current  Low resolution
e.g. Better for EDX  Smaller depth of field

Aperture size
(objective lens)

 High resolution  Grainy image

 Greater depth of field
 Edge Effect  SE emission from protrusions and circumferences  appear bright

 Accelerating voltage
 Greater the edge effect Tilt: 50, 720 
(edges become brighter)
5 kV 25 kV

Specimen: IC chip Ref: SEM Manual, JEOL

Charging
 Due to low conductivity of sample
 Coating with a conducting material to avoid charging
 To  charging   Voltage,  probe current, tilt specimen

4 kV 10 kV
Specimen: Foreleg of vinegar fly

 Accelerating voltage
  Charging
Ref: SEM Manual, JEOL
 Contamination
 Due to residual gas in the vicinity of the electron probe
 Leads to reduced contrast and loss in image sharpness
 Usually caused by scanning a small region for long time

Contamination

5 kV 18000 

Specimen: ITO Ref: SEM Manual, JEOL

 Backscattered Electron Diffraction

 Diffraction of Backscattered electrons:

1) Channeling contrast, 2) Diffraction patterns (EBSD)
 Weaker than atomic number contrast  required good BSE detector
 The BSE intensity changes drastically on or around Bragg’s condition
 Poorer spatial resolution
 EBSD

 A stationary electron beam strikes a tilted crystalline sample and the diffracted electrons
form a pattern on a fluorescent screen.
 Pattern is characteristic of the crystal structure and orientation of the sample region from
which it was generated.
 Used to measure the crystal orientation, measure grain boundary misorientations,
discriminate between different materials, and provide information about local crystalline
perfection.
 A diffraction pattern from nickel
collected at 20 kV accelerating voltage

http://www.ebsd.com/basicsofebsd3.htm http://www.ebsd.com/basicsofebsd2.htm
 Indexing: Kikuchi bands are labelled with the Miller indices of the crystal
planes that generated them (red). The planes project onto the screen at the
centre of the bands. Kikuchi band intersections are labelled with crystal
direction that meets the screen at this point (white). This direction is the
zone axis of the planes corresponding to the intersecting Kikuchi bands.

The nickel crystal unit cell superimposed on the diffraction

pattern in the orientation which generates this pattern. The
crystal planes are labelled which correspond to the (2-20) and
(020) Kikuchi bands in the diffraction pattern.

The Kikuchi band width depends on the d-spacing of the

corresponding plane. The (200) plane d-spacing is wider than
the (2-20) plane so the Kikuchi bands from (200) planes are
narrower than those from (2-20) planes.

http://www.ebsd.com/basicsofebsd3.htm
 The symmetry of the crystal is shown in the diffraction
pattern. For example, four fold symmetry is shown around the
[001] direction by four symmetrically equivalent <013> zone
axes.

Changes in the crystal orientation result in movement of

the diffraction pattern. The simulated diffraction pattern
is from a sample tilted 70° to the horizontal and the
crystal orientation is viewed along the direction
perpendicular to the sample

http://www.ebsd.com/basicsofebsd3.htm