SCANNING ELECTRON MICROSCOPE

(SEM)
 What is SEM?
 It is a microscope that produces an image by using an
electron beam that scans the surface of a specimen inside a
vacuum chamber.
What can we study in a SEM?
 Topography and morphology “Easy” sample
 Chemistry preparation!!
 Crystallography
“Big” samples!
 Orientation of grains
 In-situ experiments:
Reactions with atmosphere
Effects of temperature
 What does it looks like….

AFM Cantilever Tip Ant Head Blood Cells

Diamond Thin Film Microstructure of a plain carbon Calcium Phosphate

(Numerous Multifaceted Micro- steel that contains 0.44 wt% of Crystal
crystals) carbon
The instrument in brief
Components of the instrument
• electron gun (filament)
• electromagnetic optics
• scan coils
• sample stage
• detectors
• vacuum system
• computer hardware and
software (not trivial!!)
Electron guns
We want many electrons per time unit per area (high
current density) and as small electron spot as possible
Traditional guns: thermionic electron gun (electrons
are emitted when a solid is heated)
W-wire, LaB -crystal
6
Modern: field emission guns (FEG) (cold guns, a
strong electric field is used to extract electrons)
Single crystal of W, etched to a thin tip
 Detectors
Our traditional detectors
Backscattered electron
detector:
(Solid-State Detector)

Secondary electron detector:

(Everhart-Thornley)

 Secondary electrons: Everhart-Thornley Detector

 Backscattered electrons: Solid State Detector
 X-rays: Energy dispersive spectrometer (EDS)
 HOW THE SEM WORKS?
 The SEM uses electrons instead of light to form an
image.
 A beam of electrons is produced at the top of the
microscope by heating of a metallic filament.
 The electron beam follows a vertical path through
the column of the microscope. It makes its way through
electromagnetic lenses which focus and direct the beam
down towards the sample.
 Once it hits the sample, other electrons
( backscattered or secondary ) are ejected from the
sample. Detectors collect the secondary or
backscattered electrons, and convert them to a signal
that is sent to a viewing screen similar to the one in an
ordinary television, producing an image.
Scanning Electron Microscopy (SEM)
SEM: A focused electron
beam (2-10 keV) scans on
the surface, several types of
signals are produced and
detected as a function of
position on the surface. The
space resolution can be as
high as 1 nm. Different type
signal gives different
information: a. Secondary
electrons: surface structure.
b. Backscattered electrons:
surface structure and
average elemental
information. b. X-rays and
Auger electrons: elemental
composition with different
thickness-sensitivity.
The image formation
TV screen

e-beam

The selection of signal

 Advantages of Using SEM over OM
Magnification Depth of Field Resolution
OM 4x – 1000x 15.5mm – 0.19mm ~ 0.2mm
SEM 10x – 3000000x 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.

OM SEM
 Schematic set-up
of SEM

Topographic contrast arises

because SE generation depend on
the angle of incidence between the
beam and sample.
Electron beam-sample interactions
 The incident electron beam is scattered in the sample, both
elastically and inelastically
 This gives rise to various signals that we can detect (more on
that on next slide)
 Interaction volume increases with increasing acceleration
voltage and decreases with increasing atomic number
 Signals from the sample
Incoming electrons
Secondary electrons
Auger electrons
Backscattered Cathodo-
electrons luminescence (light)

X-rays

Sample
Secondary electrons (SE)
Generated from the collision between
the incoming electrons and the loosely
bonded outer electrons
Low energy electrons (~10-50 eV)
Only SE generated close to surface
escape (topographic information is
obtained)
Number of SE is greater than the
number of incoming electrons
We differentiate between SE1 and
SE2
Backscattered electrons (BSE)
 A fraction of the incident electrons is

retarded by the electro-magnetic field of the

nucleus and if the scattering angle is greater
than 180° the electron can escape from the
surface
 High energy electrons (elastic scattering)

 Fewer BSE than SE

 We differentiate between BSE1 and BSE2

BSE vs SE
SE produces higher resolution
images than BSE
By placing the secondary
electron detector inside the lens,
mainly SE1 are detected
Resolution of 1 – 2 nm is
possible
X-rays
Photons not electrons
Each element has a fingerprint X-
ray signal
Poorer spatial resolution than BSE
and SE
Relatively few X-ray signals are
emitted and the detector is
inefficient
 relatively long signal
collecting times are needed
Some comments on resolution
Best resolution that can be obtained: size of the
electron spot on the sample surface
The introduction of FEG has dramatically improved the
resolution of SEM’s
The volume from which the signal electrons are
formed defines the resolution
SE image has higher resolution than a BSE image
Scanning speed:
a weak signal requires slow speed to improve signal-to-noise
ratio
when doing a slow scan drift in the electron beam can affect
the accuracy of the analysis
TRANSMISSION ELECTRON
MICROSCOPE (TEM)
 TEM

Control
brightness,
convergence

binocular
screen
Control contrast
Why TEM
The uniqueness of TEM is the ability to obtain full morphological
(grain size, grain boundary and interface, secondary phase and
distribution, defects and their nature, etc.), crystallographic,
atomic structural and micro-analytical such as chemical
composition (at nm scale), bonding (distance and angle),
electronic structure, coordination number data from the sample.
TEM is the most efficient and versatile technique for the
characterization of materials. It has many mechanism for contrast
in TEM for different application purpose.

limitation
More or less bulk-like information, the sample
cannot be too thick, Sample preparation can be
difficult.
Comparison of OM,TEM and SEM
Source of
Light source electrons
Condenser
Magnetic
lenses
Specimen
Objective

Projector Specimen
Eyepiece CRT
Cathode
Ray Tube

detector
OM TEM SEM

Principal features of an optical microscope, a transmission

electron microscope and a scanning electron microscope,
drawn to emphasize the similarities of overall design.
X-Ray Diffraction (XRD)
 Introduction
Motivation:
• X-ray diffraction is used to obtain structural
information about crystalline solids.
• Useful in biochemistry to solve the 3D structures of
complex biomolecules.
• Bridge the gaps between physics, chemistry, and
biology.

X-ray diffraction is important for:

• Solid-state physics
• Biophysics
• Medical physics
• Chemistry and Biochemistry

X-ray Diffractometer
 How Diffraction Works
Wave Interacting with a Single Particle
Incident beams scattered uniformly in all directions
Wave Interacting with a Solid
Scattered beams interfere constructively in some
directions, producing diffracted beams
Random arrangements cause beams to randomly
interfere and no distinctive pattern is produced
Crystalline Material
Regular pattern of crystalline atoms produces regular
diffraction pattern.
Diffraction pattern gives information on crystal structure

NaCl
How Diffraction Works: Bragg’s Law
X-rays of
wavelength l

nl=2dsin(Q)

l
d
Q Q

• Similar principle to multiple slit experiments

• Constructive and destructive interference patterns depend on
lattice spacing (d) and wavelength of radiation (l)
• By varying wavelength and observing diffraction patterns,
information about lattice spacing is obtained
 How Diffraction Works: Schematic

NaCl

http://mrsec.wisc.edu/edetc/modules/xray/X-raystm.pdf
How Diffraction Works: Schematic

NaCl

http://mrsec.wisc.edu/edetc/modules/xray/X-raystm.pdf
 Analyzing Diffraction Patterns
Data is taken from a full range of angles
For simple crystal structures, diffraction patterns are
easily recognizable
Phase Problem
Only intensities of diffracted beams are measured
Phase info is lost and must be inferred from data
For complicated structures, diffraction patterns at each
angle can be used to produce a 3-D electron density map
 Applications of X-Ray Diffraction
Find structure to determine function of proteins
Convenient three letter acronym: XRD
Distinguish between different crystal structures with
identical compositions
Study crystal deformation and stress properties
Study of rapid biological and chemical processes
 Summary and Conclusions
X-ray diffraction is a technique for analyzing
structures of biological molecules
X-ray beam hits a crystal, scattering the beam in a
manner characterized by the atomic structure
Even complex structures can be analyzed by x-ray
diffraction, such as DNA and proteins
This will provide useful in the future for combining
knowledge from physics, chemistry, and biology