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EM Course – Introduction to SEM

Professor Rodney Herring


What can we do with an SEM?
Features of a SEM

SEM – Hitachi S4800


(+ Bruker EDS)
Compare the Light Microscope to a SEM

Increase magnification 
Compare the Light Microscope to a SEM
(cont’d)
Observation and Compositional Analysis of Fiber Cross-section
Principles and Structure of the SEM
Principles and Structure of the SEM
Configuration of the SEM

Written explanation
given in next slide.
Configuration of the SEM
Configuration of the SEM
Configuration of the SEM

We will cover each one of these components of the SEM in more detail
later in the lecture.
Procedure for SEM Imaging
Procedure for SEM Imaging

You’re done!
Procedure for SEM Imaging
Procedure for SEM Imaging
Appendices
Appendix 1:
How to make samples from:
• Bulk materials, powders, wafer and glass
• Biological, food stuff
Appendix 2:
• Why and how to use metal and carbon coatings
• Ion Milling, plasma and UV cleaning of surfaces
Appendix 3:
Examples observations:
• Metals, semiconductors, polymers
• Powders, microparticles, nanoparticles
• Toner, cosmetics
• Semiconductor wafers, Liquid Crystal Display
• Organisms, cells, micro-organisms (fungi)
• Food stuffs
Imaging Problems

External disturbance:
Stray magnetic and
Electromagnetic fields
(DC fields, low frequency)
Charge-up + Other:
Electro-static build-up and
discharge (usually due to
build up of contamination
or poor-conducting
specimen)
Charge-up Problem
Charge-up Problem
Contamination Problem

The electron beam is negatively charged and moves from the top to the bottom
of the microscope as an electric current. Many residual gas atoms and
molecules (hydrocarbons) can be polarized by the electron beam such that a
positive potential points towards the electron beam resulting in the attraction of
the hydrocarbon to the electron beam. The electron beam then carries the
hydrocarbon down the microscope. If the specimen is in its path, the
hydrocarbon is deposited on the specimen’s surface.
Similarly, free hydrocarbons existing on the surface of the specimen migrate
towards the electron beam from far distances.
Contamination Problem
Beam Damage by Irradiation

(< 80 keV for biological & polymers)


Disturbances

(Faraday cage or mu metal)


Formation of a Fine Electron Beam
Formation of a Finer Electron Beam
Electron Guns Used in SEM
Electron Guns Used in SEM & TEM

Tungsten is not heated


Comparison of Electron Guns
Configuration & Operating Principles of Electron Lens

The pole piece is


made of soft,
pure iron that
concentrates the
magnetic field to
make the
objective lens the
strongest,
highest magnifier
resulting in its
aberrations being
the most
important for
imaging.

(next slide)
Configuration & Operating Principles of Electron Lens
Lens Aberrations - Spherical

Often referred to as the “Circle of


Least Confusion”
Lens Aberrations - Chromatic
Lens Aberrations - Diffraction

Note that dd is 2x larger than the spatial resolution discussed earlier. The intensity
profile from the axis out to the sides is often modeled using an Airy Function.
Objective Lenses in SEM

Note the placement of the secondary


electron detector.
Objective Lenses in SEM

Note the placement of the secondary


electron detector.
Objective Lenses in SEM

Note the placements of the secondary


electron detectors.
Evacuation Systems
Merits of Vacuum Pumps

Scroll Pump
Generation, Detection and Usage of Electron Signals
Electron Scattering Inside Specimen
Production of Backscattered Electrons
Characteristics of Backscattered Electrons
Detection of Backscattered Electrons

(see also next slide)


Detection of Backscattered Electrons

6
ExB Filters – Signal Varying Mechanism
ExB Filters – Signal Varying Mechanism
ExB Filters – Signal Varying Mechanism
Use of Backscattered Electrons
Use of Backscattered Electrons
Production of Secondary Electrons
Secondary Electrons

14
Secondary Electron Emission Yield
Secondary Electron Emission Yield
Detection of Secondary Electrons
Use of Secondary Electrons
Use of Secondary Electrons
Acquiring Good SEM Images
In general, a good SEM image provides good:
• Topographical information
• Compositional information
• Crystal information
Bad SEM information shows:
• Artifacts
• Damage
• External disturbance
• etc.
Good SEM images also have appropriate gradation and
brightness levels.
Effect of Accelerating Energy
Effect of Condenser Lens Current
Effect of Accelerating Voltage
Please see the article, “Choosing the Right Accelerating Voltage for SEM
(An Introduction for Beginners)” V.M. Dusevich, J.H. Purk and J.D.
Eick in Microscopy Today Vol 18 No 1 (2010) pg. 48-52.

How must accelerating voltage be selected according to the sample?


Effect of Accelerating Voltage
Effect of Accelerating Voltage
Effect of Accelerating Voltage
Effect of Accelerating Voltage
Effect of Accelerating Voltage
Effect of Accelerating Voltage
Function of Objective Lens Aperture
Working Distance (WD) Affect of Image Quality
Astigmatism and Its Correction
Astigmatism and Its Correction
Astigmatism and Its Correction
Astigmatism and Its Correction
Focal Depth
Surface Charge-up
Surface Charge-up
Surface Charge-up
Surface Charge-up

a)
Surface Coatings
(Advantages & Disadvantages)

See Appendix 2 for details


Low Vacuum SEM
Low Vacuum SEM
Generation/Detection of X-rays and Elemental Analysis
Kinds of Characteristic X-rays
Bremsstrahlung or Continuous X-ray Intensity
Spread, Depth of Characteristic X-rays
Spread, Depth of Characteristic X-rays
Spread, Depth of Characteristic X-rays
X-ray Detectors
X-ray Detectors
X-ray Detectors
Multichannel Pulse Height Analyzer
Wavelength Dispersive X-ray Spectrometer (WDS)
Difference between EDX and WDX

10x
Quantitative Analysis
Quantitative Analysis
Quantitative Analysis

We’ll look at each one of these in turn.


Efficient Emission of Desired Characteristic X-ray
Sampling Location of Interest

specimen position.
Reduction of X-ray Generation Area
Shape of Specimen
Internal Specimen Structures
Internal Specimen Structures
Artificial (Artifacts) Peaks in EDX – Escape Peak
Artificial (Artifacts) Peaks in EDX – Sum Peak
Artificial (Artifacts) Peaks in EDX – System Peaks
High-accuracy EDX – Low Vacuum SEM
High-accuracy EDX – Low Vacuum SEM
Principle and Application of STEM
Principle and Application of STEM
Characteristics of STEM Signal
Characteristics of STEM Signal
Characteristics of STEM Signal
Characteristics of STEM Signal

Dark Field STEM image


Characteristics of STEM Signal
Characteristics of STEM Signal
Characteristics of STEM Signal
Appendices
Appendix 1:
How to make samples from:
• Bulk materials, ceramic powders, semiconductor
wafers and glass
• Biological, food stuff, etc
Appendix 2:
• Surface charges
• Why and how to use metal and carbon coatings
• Ion Milling, plasma and UV cleaning of surfaces
Appendix 3:
Examples observations:
• Metals, semiconductors, polymers
• Powders, microparticles, nanoparticles
• Toner, cosmetics
• Semiconductor wafers, Liquid Crystal Display
• Organisms, cells, micro-organisms (fungi)
• Food stuffs
Appendices
Appendix 4:
Example Questions
• Formation of the electron beam
• Vacuum system
• Generation, detection and usage of SEM signals
• Viewing condition for acquiring good SEM images
• Principle and applications of low vacuum SEM
• Generation/detection of x-rays and elemental analysis
• How to improve accuracy in x-ray analysis
• Principle and applications of STEM
Appendix 1 - Sampling
Tools Used
Sampling
Sampling
Appendix 2

• Sample coating methods


• Why and how to use metal and carbon
coatings
• Ion Milling, plasma and UV cleaning of
surfaces
Surface Coatings
(Advantages & Disadvantages)
Sample Coating Methods
Magnetron Sputtering Method
Plasma Deposition Method
Metal Coatings
Metal Coatings
Carbon Coating

Pelco Carbon Coater


(Cressington 208C)
Ion Milling

Fischione Ion Miller


(Model 1010)
Cross-sectional Milling
Plasma Cleaning
After ion milling a specimen, there remains free radicals on the surface of
the specimen that are mobile in the SEM and often cause contamination,
which appears as a black deposit on the surface of the specimen when
being imaged by the electron beam. These free radicals can be cleaned
off the surface of the specimen using a plasma cleaner, which comprises
of an ionized gas mixture of nitrogen + oxygen or argon + oxygen. The
plasma cleaner can be too aggressive for some surfaces. A Ultra-violet
(UV) cleaner, which is more gentle to the surface, is being developed in
our lab by David Hoyle (see below).

Fischione Plasma Cleaner Hitachi UV Cleaner


(Model 1020) (ZoneSEM)
Appendix 3 – Example Observations
Example Observations
Example Observations

See also
next slide
Example Observations
Appendix 4 – Example Questions
Example Questions
Example Questions
Example Questions
Wavelength Dispersive X-ray Spectrometer (WDS)
(additional notes)

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