Do Minh Nghiep

Materials Science Center

Electron Microscopy
and Diffraction
5. Transmission Electron Microscope
 Content
 Electron optics and instrument
 Image contrast (mass thickness contrast,
phase contrast, diffraction contrast)
 Magnification and electron beam
adjustment
 Sample preparation
 Application

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 Introduction

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 What’s TEM
The transmission electron microscope (TEM) is an analytical
tool that allows:
detailed microstructural examination through high-resolution
and high-magnification imaging: magnifications of up to
500,000x and detail resolution below 1 nm are achieved
routinely,
investigation of crystal structures and orientations through
electron diffraction pattern,
determination of chemical compositions in phases,
precipitates and contaminants through X-ray and electron
spectroscopy: qualitative and quantitative elemental analysis
can be provided from features smaller than 30 nm.
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 What’s TEM image
 Basic idea of a TEM is to
project a magnified image of
the specimen onto a
and aperture fluorescent screen where it
Objectiv
e
can be viewed by the user.
 The image itself is the result
Project
in intensity difference of
ive
beam electrons that are
forward scattered by the
specimen vs. those that are
not (transmitted unscattered)
.
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 Pros and cons
 Advantage
- TEM is the only technique that will allow the determination of the Burgers
vector.
- TEM can also provide atomic scale resolution (2 Å).
 Disadvantage
- TEM is an expensive and destructive technique.
- Some materials are sensitive to electron beam radiation, resulting in a loss
of crystallinity and mass.
- Sample preparation is very time-consuming, sample dimension small (3 mm
diameter, less than 100 nm thick)
- Artifacts cause misleading for the interpretation of transmission images.
This usually causes by the fact that the TEM presents us with 2D-images of
3D-specimens viewed in transmission.

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 3D-object → 2D-image

Each image represents a 2D

projection of the 3D object

A single projection
image is plainly
insufficient to infer the
structure of an object.
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 3D-object → 2D-image
Watch out!
A cover slide!

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 Instrument

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 TEM components
and electron path

A simplified ray diagram of a

TEM consists of
- an electron source,
- condenser lens with
aperture,
- specimen,
- objective lens with aperture,
- projector lens and
- a fluorescent screen.
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 Sîi ®èt
Cha
Anèt o
Khe cè ®Þnh
Cuén chØnh nguån
Suplementary
Condenser 1

Khe cè ®Þnh Stigmator 1 In actuality a modern TEM

Condensor 2 consists of many more
Khe tô kÝnh
Deflector
components including
Focus wobble
VËt kÝnh
- a dual condenser system,
Gi¸ gi÷ - stigmators,
mÉu
Khe vËt kÝnh Stigmator - deflector coils, and
2
KÝnh trung gian -a combination of
Khe kÝnh trung
gian (nhiÔu x¹) intermediate and dual
Dual projector projector lens.
Mµn huúnh quang
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 Conventional TEMs

200 kV (left)
and
100 kV (right)
TEM

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 Modern TEMs

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High Resolution Transmission
Electron Microscope (HRTEM)

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 HRTEM - a comparison

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 Image contrast

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 Imaging mechanism

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 Phase contrast
Bright field (BF) Dark field (DF)

Parallel incident
beam

Phase contrast/ image mode

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 Diffraction contrast
Convergent incident
beam

Diffraction contrast/ image mode

(Electron microdiffraction)

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 Diffraction contrast
 If a monochromatic e-beam of
known l strikes a crystal at the
appropriate Bragg’s angle a
number of the diffracted
electrons will be forward
scattered.
 Like the transmitted electrons
these diffracted electrons will
have nearly their same energy
but will have been significantly
altered from their trajectory.

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 Diffraction contrast
 The transmitted electrons will
be brought to convergence in
the back focal plane of the
objective lens (Y).
 Likewise the diffracted
electrons will also be brought
to convergence in the back
focal plane of the lens but at
a different spot (X).
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 Diffraction contrast
 Normally an aperture is placed in the
back focal plane of the objective lens to
stop widely scattered electrons from
reaching the viewing screen, but in the
case of diffraction it is these same
scattered electrons that contain the
information about the diffraction event.

 To operate the TEM in diffraction mode

the objective aperture is removed from
. the beam path and the microscope is
adjusted to focus an image of the back
focal plane of the objective lens, not the
image plane.

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 Diffraction contrast
Back focal plane

This is most easily

accomplished by
adjusting the strength
of the objective lens
so that an image of
the back focal plane
is projected onto the
viewing screen.

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Mass-thickness contrast (fringes)

BF DF
image image
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 Contrast image
Contrast is caused by:
- Unscattered electrons
Transmitted e
(unscattered) Scattered e coming into screen
(bright area)
- Scattered electrons
not coming into screen
(dark area)

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 Magnification

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 What’s magnification

 Total magnification in the TEM is a combination

of the magnification from the objective lens
times the magnification of the intermediate lens
times the magnification of the projector lens.
 Each of which is capable of approximately
100x.

 Mob x Mint x Mproj = Total Mag

so Mtotal can be a magnitude of 106
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 Magnification
Under different conditions of high and low magnification
the same component can have different functions:

Components High magnification Low magnification

Objective lens Image focus Diffraction focus

Diffraction lens Diffraction focus Image focus

Objective aperture Contrast forming Area selection

SA aperture Area selection Contrast forming

Object. stigmator Image stigmation Diffraction stigmation

Diffract. stigmator Diffraction stigmation Image stigmation

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Magnification and focusing

In TEM thanks
to great Dfi and
Dfo the image is
well focuced
even at high
magnification

 Depth of Field (Dfi ): the range of distance at the specimen parallel to the illuminating
beam in which the object appears to be in focus.
 Depth of Focus (Dfo ): the range of distance at the image plane (i.e. the eyepiece,
camera, or photographic plate) in which a well focussed object appears to be in focus.
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 Magnification and focusing
The depth of focus
is so great for the
projector lens
system that an
image that is in
focus on the screen
will also be in focus
on plate film
Binocular beneath the screen
viewing scope
or even a TV
Viewport Fluorescent screen camera below the
Plate camera plate film

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 Adjustment of
electron beam

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 Adjustment of condenser
Primary beam

Condenser lens

Specimen

The role of the condenser lenses is to make the beam that

is striking the specimen as nearly parallel as is possible.

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Adjustment of condenser
(-) Change in condenser lens current (+)

Screen at focal point: Screen behind focal

Screen before focal
minimum beam point: large beam
point: large beam
size/crossover, maximum (over focused)
(under focused)
brightness (focused)

As magnification increases the condenser lens must be adjusted to

properly illuminate the specimen. When the lens is brought to its
smallest spot the beam is said to be at the crossover point.

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 Stigmator

Holey (not Holy) Formvar is used to critically adjust the stigmation of a TEM.
 When the beam is under or over focused on the specimen a Fresnel fringe
becomes visible due to the effects of diffraction around the edges of the whole.
 When this Fresnel fringe is evenly distributed then the beam is said to be
stigmated.
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 Deflection coils
 In older TEMs functions such
as gun and beam alignment
were accomplished by
physically moving components
in the column.
 Today they are achieved by
use of electromagnetic
deflection coils that are
positioned throughout the
column.

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Shift / tilt of beam by deflecton coils

Using the deflection

coils the beam can be:
 shifted so that the
focused beam is
centered in the back
focal plane of the lens
and
 tilted so that the
beam is centered on
the specimen.
 α - deflection angle

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 Pivot point

Pivot
point

We call these centering spots “pivot points” and as the beam

is shifted or tilted back and forth there should be no apparent
movement if the microscope is properly aligned
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 Specimen stage position

Specimen

Specimen stage

Likewise the position of the specimen relative to the beam is of critical

importance. To adjust the height or “Z” position of the specimen it is
physically rocked back and forth until an object in the center no longer
moves.
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 Specimen
stage
In-column motion
of specimen: Z-Y-Z
shift, rotation/ tilt
around a common
axis by
coresponding
mechanism.

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Sample tilt in single obj. lens
 A major problem with TEM
lens design is the fact that
there is very little space
between the pole pieces of
the objective lens to
accommodate the specimen
and objective aperture.
 This also puts severe
constraints on how far the
specimen can be tilted
within the lens.
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Twin/double objective lens
 A clever solution to this
problem came in the invention
of the double objective or “twin”
lens.
 In this lens design the
specimen actually lies between
two separate lens fields
allowing for tilt angles as large
a 60o from perpendicular to
the optical axis.

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Focus Wobbler shifts the image back and
forth, and when the movement is stable
the image is focused.

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 Specimen
preparation

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 Wedge sample
-”windows” technique

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 Electropolishing

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 Sample sections after
electropolishing and sample grids

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Cutting thin sample
by microtomy

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 Replica foils

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 Instrumentation
TEM grids

3 mm
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 Sample holders

Sample positions

Cooling

Standard

Heating

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 Applications

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 Dislocation structure
(diffraction contrast)

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 Contrast image
and
microdiffraction
pattern of two
screw dislocation
groups with
different Burgers
vectors

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 BF and DF
images of
dispersive
precipitates
in Al-Cr-Zr
alloy

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 Lattice
image of
(111)
planes in
Ga-As

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HR image
of σ
phase in
Al alloys

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 HR contrast
image of
metal atom
arrangement
in 1,97 nm
thick
specimen
of Nb-W-O
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