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Microscopy
Dr. G. P. Chaudhari
Metallurgical and Materials Engineering
Microscope- transforms an object into an image
Our interest: make image larger magnify!
diverse ways to magnify
TEM: most efficient and versatile tools for the characterization of
materials over spatial ranges from the atomic scale, through the
ever-growing nano regime (from < 1 nm to 100 nm) up to the m
level
WHAT MATERIALS TO STUDY IN THE TEM?
Metals, alloys, ceramics, glasses, polymers, semiconductors, and
composites
Nanotechnology
the ability to understand and control matter at dimensions of roughly 1
to 100 nanometers, where unique phenomena enable novel applications
WHY USE ELECTRONS?
limited image resolution in light microscopes imposed by the wavelength
many other equally sound reasons
Introduction- TEM
Same principles as light microscope- uses
electrons to produce image
Lower wavelength of electrons allows for much
higher resolution than is possible with light
microscope.
Electrons accelerated to defined energy behave as a
wave.
Objects to order of 10-10 m are visible
The total volume of the material investigated by
TEM since it started in the fifties, is less than 1
cm3!
Electron Microscopy
Scanning EM (SEM) an electron beam falls on
the specimen and the image is derived from
the scattered and reflected electrons.
Surface relief (external morphology)
reflection method
scanning technique, pixels (picture elements)
http://photo.stackexchange.com/question
s/8304/what-is-a-diffraction-limit
http://www.olympusmicro.com/primer/techniques/confocal/resoluti
onintro.html
Rayleigh criterion
When the maximum of intensity of an airy disc coinsides with the first
minimum of the second, then the two points can be just distinguished
Resolution
Closest spacing (r) of two points which can be clearly seen
through the microscope to be separate entities
Resolution is limited by diffraction effect- restricted openings-
lenses and apertures esp. objective aperture: light from every
small point in the object suffers diffraction!= Airy ring/disc
wavelength
0.61 0.61
r
sin N . A.
Refractive Semi-angle subtended
by the aperture at the
Index specimen
Resolution limit of a light microscope
can decrease to 400 nm (green light)
sin is limited to ~ 1.6
Thus R. P. = 0.61 /N.A. = 0.61x 400/1.6 = 152 nm
h
2meV
h is Plancks constant (6.626x10-34 Js), m is electronic
mass (9.11x10-31kg) and e is electronic charge
(1.602x10-19C).
Variation of wavelength with applied voltage
Applied voltage, keV Wave length, nm
20 0.0086
50 0.0054
80 0.0042
100 0.0037
200 0.0025
500 0.0014
1000 0.00087
Light VS Electrons
= 0.5m 150
~ 0.055A (@ 50kV )
V
0
= 1.5 (glass) = 1.0 (Vacuum)
= 70 = 1
r = 0.2m=2000 r = 0.00016m=1.6A
Lens Aberrations
Analogies:
Best electromagnetic lens ~ bottom of a coke bottle used as magnifying glass
If your eye lens was ~ best electromagnetic lens => legally blind!
Spherical aberration
Chromatic aberration
Astigmatism
Chromatic Aberration
Reasons:
For object points off the optic axis, the path length criterion shows that, there
will be a focus for rays traveling in the horizontal plane at a different position
from the focus for the rays traveling in the vertical plane.
All monochromatic aberrations can be reduced if only the central portion of
the lens is used.
no astigmatism overfocused underfocused
h Plane of
optimum focus
d1
But
resolution
decreases!
Trade-off
Thermionic gun:
Single crystal W
Electron Sources
Thermionic Emitters
Field Emitters
Thermionic Electron Gun
Electrons are emitted from a heated tungsten
filament and then accelerated towards an anode; a
divergent beam of electrons emerges from the
anode hole.
Energy Spread:
filament imperfections
High tension instability
Surface temperature
Boersch effect (mutual interaction)
Field Emitter
Single oriented
crystal of tungsten
etched to a fine tip
Wave behavior
Images and diffraction patterns
Wavelength can be tuned by energies
Charged particle behavior
Strong electron specimen interactions
Chemical analysis is possible
INFORMATION AVAILABLE
Elastic scattering
Coulombic interaction
Primary e energy does not change
Direction may change
Strongly forward peaked distribution of scattered e
Probability of scatter through angle
p() 1/(E02sin4); for small , p() is high
Importance of elastic scattering in EM
It is the major mechanism by which e are deflected
Scattered e mainly contribute to the diffraction patterns
Inelastic scattering
Primary e loses detectable amount of energy
K.E. of primary e
Heat (almost all)
X-rays
Secondary e very small energy
Light useful for imaging or analysis
Electron-specimen interactions
Inelastic scattering & absorption
Interaction volume: 95
% of primary e are
brought to rest by
inelastic processes.
A few primary e are
backscattered and
leave the specimen
Thick specimen & the interaction
volume
Electron beam-sample interactions
Objective lens:
magnification,
introducing contrast
Intermediate lens:
further magnification,
imaging or diffraction
r r Incident beam
tan 2 ,2 ,since is very small
L L specimen
bcc
Imaging Defects
Diffraction Contrast- dominant mechanism for
imaging dislocations and defects in the specimen
The size of the objective aperture in bright-field
mode directly determines the information to be
emphasized in the final image. When the size is
chosen so as to exclude the diffracted beams-
so-called diffraction contrast .
a crystalline specimen is oriented to excite a
particular diffracted beam (g vector), or a
systematic row of reflections, and the image is
sensitive to distortion of crystal lattices due to
defects, strain and bending. (g.b#0 )
The resolution of this imaging technique is 1-3
nm. Diffraction contrast mainly reflects the long-
range strain field in the specimen.
Diffraction Pattern- Spot to Ring
Polycrystalline Au
Ring Patterns- what information?
Amorphous materials
Bulk ceramics
Mechanical grinding, polishing, dimpling
Ion erosion, focused ion thinning
Metals
Mechanical grinding, polishing
Electrolytic thinning
Organic Materials
Freeze drying, embedding,
ultramocrotomy
Preparation of powder samples
Small particles:
Direct transfer to carbon film mounted on Cu grid
Ultrasonic dispersion of suspension on C/Cu
Membrane filtration and subsequent dissolution
of the filter
Large particles:
Embedding in resin (phenyl formaldehyde)
La2RuO5 particles
In resin
Powder Samples
Dimpling
3 mm diameter disc- punch/ultrasonic cutter
Ion beam thinning
Electrothinning- Twin-jet electropolisher
specimen punch
sample
grids
Drawbacks
Can take a lot of time to make sample thin
enough to be transparent to electrons
Viewing area only shows a small section of the
sample being analyzed, which can differ from
the rest of the sample
The sample can be damaged by the electrons,
especially when dealing with biological samples
Uses optical system lens aberration
Vibration of stage
Reference Books
Transmission Electron Microscopy: A Textbook
for Materials Science (4-Vol Set) by David B.
Williams, C. Barry Carter
Transmission Electron Microscopy and
Diffractometry of Materials by Brent Fultz, James
Howe
Electron Microscopy of Thin Crystals by Peter B.
Hirsch
Electron Microscopy and Analysis, 3rd ed. (2000)
by Peter J. Goodhew, John Humphreys, and
Richard Beanland