TEM

Do it with
electrons !
II
TEM - transmission electron microscopy
Typical accel. volt. = 100-400 kV
(some instruments - 1-3 MV)
Spread broad probe across

specimen - form image from
transmitted electrons
Diffraction data can be obtained

from image area
Many image types possible (BF, DF,

HR, ...) - use aperture to select
signal sources
Main limitation on resolution -

aberrations in main imaging lens
Basis for magnification - strength

of post- specimen lenses
Instrument components
Electron gun (described previously)
Condenser system (lenses &

apertures for controlling
illumination on specimen)
Specimen chamber assembly
Objective lens system (image-

forming lens - limits resolution;
aperture - controls imaging
conditions)
Projector lens system (magnifies

image or diffraction pattern onto
final screen)
Instrument components
Electron gun (described previously)
Condenser system (lenses &

apertures for controlling
illumination on specimen)
Specimen chamber assembly
Objective lens system (image-

forming lens - limits resolution;
aperture - controls imaging
conditions)
Projector lens system (magnifies

image or diffraction pattern onto
final screen)
Examples
Matrix - '-Ni2AlTi
Precipitates - twinned L12 type '-Ni3Al
Examples
Precipitation in an
Al-Cu alloy
Examples
dislocations SiO2 precipitate

in superalloy particle in Si
Examples
lamellar Cr2N
precipitates in
stainless steel
electron
diffraction
pattern
Specimen preparation
Types
replicas
films as is, if thin enough
slices ultramicrotomy
powders, fragments crush and/or disperse on carbon film
foils
Foils
3 mm diam. disk
very thin (<0.1 - 1 micron - depends on material, voltage)
Specimen preparation
Foils
3 mm diam. disk
very thin (<0.1 - 1 micron - depends on material, voltage)
mechanical thinning (grind)

chemical thinning (etch)
ion milling (sputter)
examine region
around perforation
Diffraction
Use Bragg's law - = 2d sin
But much smaller
(0.0251 at 200kV)
if d = 2.5, = 0.288
Diffraction
2 sin 2 = R/L
specimen
= 2d sin d (2)
R/L = /d
Rd = L
image plane
L is "camera length"
L is "camera constant"
Diffraction
Get pattern of spots around transmitted beam from one grain (crystal)
Diffraction
Symmetry of diffraction pattern reflects

symmetry of crystal around beam direction
Example:
6-fold in hexagonal, 3-fold in cubic
[111] in cubic [001] in hexagonal
Why does 3-fold diffraction pattern look hexagonal?

Diffraction
P cubic reciprocal lattice
layers along [111] direction
Note: all diffraction
patterns are
centrosymmetric,
even if crystal structure l = +1 level
is not centrosymmetric
(Friedel's law)
Some 0-level patterns 0-level

thus exhibit higher
rotational symmetry than
structure has
l = -1 level
Diffraction
Cr23C6 - F cubic Ni2AlTi - P cubic

a = 10.659 a = 2.92
Diffraction - Ewald construction
Remember crystallite size?

when size is small, x-ray reflection is broad
To show this using Ewald construction, reciprocal lattice points

must have a size
Diffraction - Ewald construction
Many TEM specimens are thin in one direction - thus, reciprocal

lattice points elongated in one direction to rods - "relrods"
Also, very small, 1/ very large
Only zero level in

position to reflect
Ewald
sphere
Indexing electron diffraction patterns
Measure R-values for at least 3 reflections


Index other reflections by vector sums, differences
Next find zone axis from cross product of any two (hkl)s
(202) x (220) > [444] > [111]

Find crystal system, lattice parameters, index pattern, find zone axis
ACTF!!! Note symmetry - if cubic, what

direction has this symmetry (mm2)?
Reciprocal lattice unit cell

for cubic lattice is a cube
Why index?
Detect epitaxy
Orientation relationships at grain boundaries
Orientation relationships between matrix & precipitates
Determine directions of rapid growth
Other reasons
Polycrystalline regions
polycrystalline BaTiO3
spotty Debye rings
Indexing electron diffraction patterns - polycrystalline regions

Same as X-rays smallest ring - lowest - largest d
Hafnium ()
Indexing electron diffraction patterns - comments
Helps to have some idea what phases present
d-values not as precise as those from X-ray data
Systematic absences for lattice centering and

other translational symmetry same as for X-rays
Intensity information difficult to interpret

Sources of contrast
Diffraction contrast - some grains diffract more strongly than

others; defects may affect diffraction
Mass-thickness contrast - absorption/

scattering. Thicker areas or mat'ls w/
higher Z are dark
Bright field imaging
Only main beam is used. Aperture in back focal plane blocks

diffracted beams
Image contrast mainly due to subtraction of intensity from the

main beam by diffraction

diffracted beams


diffracted beams


diffracted beams

What else is in the image?
Many artifacts
surface films
local contamination
differential thinning
others
Also get changes in image because of

annealing due to heating by beam
Dark field imaging
Instead of main
beam, use a
diffracted beam
Move aperture to
diffracted beam
or tilt incident
beam
Dark field imaging
Instead of main beam, use a diffracted beam
Move aperture to diffracted beam or tilt incident beam
strain field contrast

Dark field imaging
Instead of main beam, use a diffracted beam
Move aperture to diffracted beam or tilt incident beam

Lattice imaging
Use many diffracted beams
Slightly off-focus
Need very thin specimen region
Need precise specimen alignment
See channels through foil
Channels may be light or dark in image
Usually do image simulation to

determine features of structure

Examples
M23X6 (figure at top

left).
L21 type '-Ni2AlTi

(figure at top center).
L12 type twinned '-

Ni3Al (figure at bottom
center).
L10 type twinned NiAl

martensite (figure at
bottom right).

TEM

Transféré par

Informations du document

Titre original

Copyright

Formats disponibles

Partager ce document

Partager ou intégrer le document

Options de partage

Avez-vous trouvé ce document utile ?

Ce contenu est-il inapproprié ?

Droits d'auteur :

Formats disponibles

TEM

Transféré par

Droits d'auteur :

Formats disponibles

Do it with

Spread broad probe across

Diffraction data can be obtained

Many image types possible (BF, DF,

Main limitation on resolution -

Basis for magnification - strength

Electron gun (described previously)

Condenser system (lenses &

Specimen chamber assembly

Objective lens system (image-

Projector lens system (magnifies

Electron gun (described previously)

Condenser system (lenses &

Specimen chamber assembly

Objective lens system (image-

Projector lens system (magnifies

dislocations SiO2 precipitate

mechanical thinning (grind)

Use Bragg's law - = 2d sin

But much smaller

Symmetry of diffraction pattern reflects

[111] in cubic [001] in hexagonal

Why does 3-fold diffraction pattern look hexagonal?

Some 0-level patterns 0-level

Cr23C6 - F cubic Ni2AlTi - P cubic

Diffraction - Ewald construction

Remember crystallite size?

To show this using Ewald construction, reciprocal lattice points

Diffraction - Ewald construction

Many TEM specimens are thin in one direction - thus, reciprocal

Also, very small, 1/ very large

Only zero level in

Indexing electron diffraction patterns

Measure R-values for at least 3 reflections

Indexing electron diffraction patterns

Indexing electron diffraction patterns

Index other reflections by vector sums, differences

(202) x (220) > [444] > [111]

Indexing electron diffraction patterns

ACTF!!! Note symmetry - if cubic, what

Reciprocal lattice unit cell

Indexing electron diffraction patterns - polycrystalline regions

Indexing electron diffraction patterns - comments

Helps to have some idea what phases present

d-values not as precise as those from X-ray data

Systematic absences for lattice centering and

Intensity information difficult to interpret

Diffraction contrast - some grains diffract more strongly than

Mass-thickness contrast - absorption/

Bright field imaging

Only main beam is used. Aperture in back focal plane blocks

Image contrast mainly due to subtraction of intensity from the

Bright field imaging

Only main beam is used. Aperture in back focal plane blocks

Image contrast mainly due to subtraction of intensity from the

Bright field imaging

Only main beam is used. Aperture in back focal plane blocks

Image contrast mainly due to subtraction of intensity from the

Bright field imaging

Only main beam is used. Aperture in back focal plane blocks

Image contrast mainly due to subtraction of intensity from the

What else is in the image?

Also get changes in image because of