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Transmission Electron Microscopy

Chapter 2
Electron Optics

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Outline

• The Structure of TEM

• Aberration and Resolution

• Depth of Field and Depth of Focus

• Calibration

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OM VS TEM
Optical Microscope (OM) Transmission Electron Microscope (TEM)

Light
Source
Condenser
Lens
Specimen
Objective
Lens

Projector
Lens
EYE

1000x BETTER
http://nptel.ac.in/courses/102103047/35
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Geometric optics Three principles elements

Object plane
Back focus plane
Image plane

Object and image planes


are called conjugate planes

Object distance
Image distance
Focus length
Modification

Lens Maker's formula


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Structure of TEM

E-gun

Condenser Lens Condenser Condenser Lens


Aperture
Specimen
Objective Objective Aperture
Holder
Aperture
Field Limiting Objective Lens
Aperture
Intermediate
Projector Lens Projector Lens
lens

Viewing Screen

http://www.nsf.gov/news/special_reports/scivis/popup/tem.jsp

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Structure of TEM

E-gun

(A) Illumination System


Condenser Lens

Specimen
(B) Stage Holder
Objective Lens
Intermediate
(C) Imaging System Lens Projector Lens

Viewing Screen
(D) Image Detection
/ Recording System
http://www.nsf.gov/news/special_reports/scivis/popup/tem.jsp

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Structure of TEM

E-gun

(A) Illumination System


Condenser Lens

• Electron Gun Specimen


Holder
Thermionic Gun Objective Lens
Intermediate
Field-Emission Gun Lens Projector Lens

• Condenser Lens
Viewing Screen

http://www.nsf.gov/news/special_reports/scivis/popup/tem.jsp

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Illumination System
• W filament or LaB6
Thermionic Gun
• Thermionic Emission Theory

Cathode • Follows Richardson’s Law

=
Filament J: Current density
A: Richardson’s constant
Wehnelt k: Boltzmann’s constant
cap T: Temperature in Kelvin
Anode : Work function
plate LaB6 : lanthanum hexaboride

The image of three major parts of


a thermionic gun.

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Thermionic Guns
W Filament LaB6 Gun

LaB6 : lanthanum hexaboride

Indirect Heating
Direct Heating
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Thermionic Guns
• The Wehnelt cap acts
Characteristics as the electrostatic
lens to focus the
electrons.

• The electrons are


accelerated by the
voltage difference
between the source
and the anode plate.

• If the accelerating
voltage of 100 kV is
used, the electrons
will gain the energy of
100 keV after
Schematic diagram of a LaB6
thermionic gun. accelerating process.

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Work function
Electrons on the surface of the metals can be escaped through the energy barrier after
the heating process. This energy barrier calls work function.

Polarization effect: For a P- polarization state, the fixed


(negative) surface charge will act to reduce the work function,
defined as the vacuum level with respect to the Fermi level.
Thus, the more negative the polarization, the smaller

Surface
the effective work function. However, the electrons inside the
materials need to overcome polarization state to the surface
of the metal. (Need more energy to escape the surface of the
metal)

Image effect: A positive charge can be inducted to pull back


the electron once the electron has been escaped out of the
surface of the metal.

Both effects need the energy


, called “work”.

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Electron Guns

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Brightness

• The brightness is defined as,

Emission Current
=
First Area of the Solid Angle
Cross-over Cross-Over Point of the Beam

4
= =
2
Current Density : =
2
Schematic diagram of a LaB6
thermionic gun. : Diameter of the cross-over point
: Divergence angle
: Emission current

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Cross-Over

radius of filament radius of crossover


Diameter W wire
of different
sources (d) LaB6
FEG

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Thermionic Guns

Characteristics

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Thermionic Guns

Operating Conditions
Saturation Condition: ie reaches a
maximum such that a further
increase in if doesn’t increase ie.

Operating Condition: if is at or
just below the saturation.

Advantage:
1. Prolonging the lifetime of the
gun.
The relationship between the current emitted by
the electron source and the source heating 2. Optimizing the brightness.
current for a self-biasing gun.

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When the current of electrons emitted from the electron gun is increased,
Coulomb interactions between the electrons make an increase of the energy
spread of the electrons. This phenomenon is termed "Boersch effect," which
gives rise to the increase of the chromatic aberration.

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Importance of high brightness
High brightness can generate strong the 2nd electrons, X-ray and inelastic
electrons
In STEM mode, It needs the high brightness to reduce the exposure time of
taking an image.

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Illumination System

Field-Emission Gun (FEG)


• Because the tip must be free of
contaminations and oxides, the
operation in UHV environment
is required.

Thermal FEG Tip Radius: < 0.1 m


UHV: ultra-high vacuum ( < 10-9 torr)
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Field-Emission Gun

Working Principle

Anode 1: Provides the


Cathode
extraction voltage (few
KV). Enables electrons to
tunnel out of the tip.

Anode 2: Provides the


accelerating voltage.
Accelerate electrons to
high speed.

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Schottky Field Gun

The electric field on the tip of SFE is applied to decrease the material working
function . For this reason such field emitters are coated with low working
function materials such as ZrO2 . Even if SFE is a thermoinoic emitter, the
brightness and the current density are comparable with that ones of CFE. The
electron gun of a SFE is quite similar to that one of CFE. SFE guns include a
suppressor grid to eliminate unwanted thermionic emission from regions outside
the tip.

Schottky emitters - operated typically at high temperatures of 1,700K - are a good


choice for general applications focused on analytical work using large, very stable
probe currents.
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Illumination System

E-Gun (Electron Source) 1 : 10 : 103


Thermionic Source FEG

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Coherency and Energy spread
Coherency and Energy spread of beam are determined by

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Spatial and Temporal Coherency
Coherency is the measurement of the correlation between the phases measured
at different (temporal and spatial) points on a wave.

Temporal coherency is a measurement of the correlation of light wave’s phase at


different points along the direction of propagation – it tells us how monochromatic
a source is.

Spatial coherency is a measurement of the correlation of a light wave’s phase at


different points transversed to the direction of propagation - it tells us how uniform
the phase of a wavefront is.

No way to create a monochromatic electron beam: There is 0.1 ~0.3 eV


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Temporal and Spatial Coherency of beam in TEM

Temporal Coherency
Monochromatic source
Energy dispersion still happens in TEM (0.1~0.3 eV) for
each electron in electron beam

Spatial Coherency
Effective beam irradiated on the surface of
the specimen can be defined as

(convergence angle)
Control condenser lens to control the C1 cross over
(spot size) and condenser lens aperture to control
the angle. (convergence angle) Aperture to
Small parallel beam with much better spatial reduce the
angle
coherency.
Disadvantage: reduce the brightness of beam
through the aperture.
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Fresnel Fringe
• Fresnel fringe can be used to gauge the coherency
of the electron beam.

Fresnel fringe from thermionic gun Fresnel fringe from FEG

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FEI (thermal
fisher, 2017)
Field Electron and
Ion Company

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Condenser Lenses

Parallel Beam

Condenser
Aperture

< 10-4 rads (0.0057o)


• When operating at conventional
TEM mode.
• The lens is underfocused to provide
more parallel beam.
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Condenser Lenses
Convergent Beam Strong C1 Weak C1

• Convergent beam with greater


illumination intensity, can be used
for analyzing thicker specimen.
• Probe-like beam is used to localize
the signals in STEM mode.
STEM: Scanning Transmission Electron Microscope

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Stability
In addition to highly stable in high bias, the beam current should be stable
after the emission.
-Get stable under the longer exposure time
-More stable information on chemical results, including EELS, CL and
EDS.

Unstable condition occurs in thermionic guns when the new gun materials
were replaced or the guns are broken.

In normal case, 1%/per hr unstable behavior is trustable.

For the cold guns, it is more difficult to maintain the stable operation of the
guns.

Ultra high vacuum is necessary for the stable operation.

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How to confine (focus) the beam ?

1. Change the current to modify the magnetic field to change focus


ability
2. Use aperture to control the coverage angle

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Magnetic Lens

• Electrostatic Lens
Wehnelt Cap
• Magnetic Lenses
Most of Lenses in TEM

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Magnetic Lens

• A selection of different lenses; (A) a split polepiece objective lens, (B) a top-
entry immersion lens, (C) a snorkel lens, and (D) a quadrupole lens.
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Force induced by magnetic field

Angle between optical axis and


direction of electron traveling
Direction of electron traveling is parallel with the direction of the
magnetic field. No magnetic force can be induced. No deflection
of electron
Maximum occurs
magnetic force occurs

• If we change B, the helix trajectory of electrons differs and the electrons with
higher energy must use stronger magnetic field to get similar ray path.
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Magnification and Rotation of Image

Rotation of Image • The force generated when electrons travel


through the magnetic field, thus, the electrons
travel in the helical manner as they pass
through the lens.
• If we change B, the helix trajectory of electrons
differs. Also, the electrons with higher energy
must use stronger lenses to get similar ray
path.
• The image or DP rotate if you change the
magnification,
=

-- The rotation has been removed by the


addition of a compensating projective lens,
in this case, the image and DP have the
= + × = + × identical orientation.

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Magnification and Rotation of Image

Magnification • The focal length (f) of the lens

1 1 1
= +

• The magnification (M)

• Strengthening the lens shortens the


focal length f.

1
=

-- A weaker lens (f1) produces a higher


M of the object.
E: energy; B: magnetic field

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Focus Conditions

The Strength of Magnetic Field

Object Object

Image
Plane

Overfocused Focused Underfocused


Lens Lens Lens
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Focus Conditions
• It is better to take an image at slightly underfocused condition
because the edge of the image is clearly seen at the underfocus.

Underfocused Focused Overfocused

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Remarks
1. There are two types of the electron guns.
Thermionic gun and field-emission gun.

2. The working principle of thermionic gun is based on


the thermionic emission theory , while the electrons of
field-emission gun are pulled out by strong electric field .

3. The parallel beam is used in TEM mode , and it can be obtained


if the condenser lens is underfocused or the condenser aperture
is inserted into TEM.

4. The convergent beam is used when analyzing the thicker specimen


in TEM mode or the probe-scan in STEM mode . The convergent
beam is formed if the lens is at focused condition .

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Structure of TEM

Specimen
(B) Stage Holder

• Top-Entry Holder

• Side-Entry Holder

http://www.nsf.gov/news/special_reports/scivis/popup/tem.jsp

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Specimen Holders

Top-Entry Holders
Loading
System

Pros:
1. Less drift.
Cons:
1. Difficult design.
2. EDS detector is not
accessible.
Cross-section and top-view
illustrations of top-entry holder 3. Resolution is limited.

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Specimen Holders

Side-Entry Holders
3 mm

Clamp or Screw O-ring

Vacuum

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Specimen Holders

Side-Entry Holders Heating Holder: The


most popular holder for
in-situ studies of
material diffusion,
thermal expansion and
crystallization.
Cooling Holder: this is for
in-situ studies of
superconducting materials,
polymer and biological
tissue.
Double-Tilt Holder: The
essential holder for
imaging and diffraction
analysis of crystalline
specimens.

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Structure of TEM

Objective Lens
Intermediate
(C) Imaging System Lens Projector Lens

http://www.nsf.gov/news/special_reports/scivis/popup/tem.jsp

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Imaging System

Objective Lens : The most


important lens in a TEM. It
Intermediate Lens : Electron Beam determines the quality of all
This lens has dual the information (image and
function. DP) about the specimen.

1. Determining the Specimen Objective Lens


magnification
Intermediate
Lens
2. Selecting image
Projector Lens
or DP is
projected onto Projector Lens : The final
the viewing lens. It projects the final
screen. image or DP onto the
viewing screen.

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Imaging System

The Lens Equation


1 1 1
Specimen Object Plane
= +

f: the focal length of the lens

Objective Diffraction Pattern (DP)


Lens

Back Focal Plane


Image

Image Plane

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Imaging System

Diffraction mode: The back


focal plane of objective lens
acts as the object of
intermediate lens. The DP is
projected onto the viewing
screen.

Image mode: Adjusting the


intermediate lens so that its
object plane is at the image
plane of the objective lens. The
image is projected onto the
viewing screen.
Diffraction mode Image mode
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Structure of TEM

Viewing Screen
(D) Image Detection
/ Recording System
http://www.nsf.gov/news/special_reports/scivis/popup/tem.jsp

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Image Detection/Recording

• Viewing Screen: The fluorescent


screen coated with doped-ZnS emits
light of 550 nm (green light).

Binoculars

Viewing
Screen

CCD Camera

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Image Detection/Recording

• Photographic Film: The oldest recording


medium. Complicated to have the data.
Brightness of beam, exposure time,
develop conditions….etc.

• Charge-Coupled Device (CCD): The


digital device to record static images
and videos.
-- pros
1. low noise
2. linear response
-- cons
1. expensive
• Ultrahigh speed CCD costs
several millions Photographic Film CCD

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Image Detection/Recording

• Semiconductor Detector: a Si-based p-n junction plate for detecting the


electrons.

1. e-h pairs generated by the energy


transfer from incident electrons.

2. The incident electron signal is


converted to a current in the
external circuit.

3. STEM detector in ring shape (annular


detector).

ADF/HAADF STEM Detector

BF/ABF STEM Detector


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Outline

• The Structure of TEM

• Aberration and Resolution

• Depth of Field and Depth of Focus

• Calibration

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Aberrations

A. Astigmatism

B. Chromatic Aberration

C. Spherical Aberration

D. Diffraction Aberration

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Astigmatism

• Astigmatism occurs when


1. The polepiece is inhomogeneous.
2. Apertures are not precisely centered.
3. The aperture is not clean.

• The distortion of image,

=
f: The maximum difference in focus
induced by the astigmatism.
: The maximum angle of collection

Astigmatism is easily corrected !!


a quadrupole lens
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Astigmatism

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Chromatic Aberration

• Chromatic aberration arises from • The aberration,


the energy spread of electron
beam. The energy spread varies =
from 0.3 eV (cold FEG) to 1 eV
(LaB6).
• It becomes significant after
coming through the specimen.
• The chromatic aberration is
minimized, if

1. The specimen is thin enough.


2. Energy-filtered TEM is used.

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Chromatic Aberration

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Spherical Aberration

• The spherical aberration occurs


when the lens field behaves
differently for off-axis rays

• The radius of the aberration disk is


given by

=
: Spherical aberration coefficient
: The maximum angle of collection

• Cs is typically few mm, it can be


reduced by the Cs corrector.

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Spherical Aberration

Negative Cs Cs = 0 Positive Cs

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Cs Corrector →

confinee - beam

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Cs Corrector

TEM Mode
W/O Cs W/ Cs

The grain boundary in SrTiO3 imaged without and with Cs corrector.

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Cs Corrector

STEM Mode • Interface of ZnO and In


• The Dumbbell Structure of Ge

ABF STEM

• Polarity Determination of GaN


ADF STEM

[110] Ge

ABF image: Annular Bright Field


ADF image: Annular Dark Field
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Diffraction Aberration

• In ideal lens system, the resolution is generally defined by Rayleigh


Criterion.

Just
Resolved Un resolved
Resolved

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Diffraction Aberration

• The theoretical resolution of


the lens is given by

= .

Image
: The wavelength of light source Plane
: The maximum angle of collection Lens

Objects
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Resolving Power

A. Astigmatism

fields. operation.
B. Chromatic Aberration
-beam.
specimen.
C. Spherical Aberration

is used.
D. Diffraction Aberration
.

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Resolving Power

• The resolution is given

= + = + .

• The best resolution is

(Cs corrector) Higher resolution


Lower or
(smaller )
(High voltage)

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Remarks
1. There are two types of specimen holders.
Top-Entry and Side-Entry.

2. The intermediate lens not only determines the magnification, but


also selects the image or diffraction pattern .
3. Besides astigmatism and chromatic aberration, the image
resolution of TEM is affected much by spherical aberration and
diffraction aberration.
4. Lowering Cs or can improve the image resolution of TEM, which
can be achieved by installation the Cs corrector or increasing the
operating voltage, respectively.

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Outline

• The Structure of TEM Ch. 5, 6, 7, 8, 9

• Aberration and Resolution Ch. 6

• Depth of Field and Depth of Focus Ch. 1, 6

• Calibration Ch. 9

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Depth of Focus and Depth of Field

• Depth of Field (Dob): The distance


Object along the axis on both sides of
the object plane within which we
can detect without loss of focus.

• Depth of Focus (Dim): The


distance along the axis on
both sides of the image plane
Image within which the image is
focused.

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Depth of Focus and Depth of Field

• and refer to the smallest distance which we can resolve in the


object and image, respectively.

• and are very small, thus

~ = 2 2
~ =
2 2

• = Typically,
1
=
• =

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Depth of Focus and Depth of Field

• Depth of Focus is given by

• Depth of Field is given by

• If we want to see detail at the 0.2 nm level, we need to use a


magnification of ~500,000x, in this condition, the depth of focus
will be 5 km. If we want to see 2 nm, we can use the magnification
of 50,000x and the depth of focus is 500 m. ~ 0.01

The TEM image would be in focus on the floor under the microscope.

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Outline

• The Structure of TEM Ch. 5, 6, 7, 8, 9

• Aberration and Resolution Ch. 6

• Depth of Field and Depth of Focus Ch. 1, 6

• Calibration Ch. 9

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Calibration

• The TEM should be calibrated when it is first installed or the


instrument (lens coil, gun…etc) is modified.

1. Magnification Calibration

2. Camera-Length Calibration

3. Rotation of the Image

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Magnification Calibration

• We use the standard specimens to calibrate the magnification. The


thin carbon-film replica of an optical-diffraction grating of known
spacing.

• The typical linear density of lines of the replica is 2160/mm.

• This replica enables the calibration up to 200000 x.

0.463 um

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Magnification Calibration

• The lattice fringes (phase contrast images) of known crystal ,


can be used for the calibration at higher magnification (the
magnification for high resolution image)

0.344 nm

1300

1200

1100

1000

900

800

700

600
0.0 0.5 1.0 1.5 2.0 2.5 3.0
nm

Graphite

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Camera-Length Calibration

• Camera length (L) is an important factor


for structural analysis using diffraction
pattern.

• The magnification of DP (R) increases


with the increased camera length.
Camera
Length 2 ~ =

R: the distance of the diffracted


spot and the direct beam

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Rotation of the Image

• We have to determine the direction or plane of the crystalline


materials in most cases, so, it is crucial to know the angle between
orientations in image and in the DP.

• If you record the images at different magnifications, the images will


rotate by an angle with respect to the DP.

[001]
(001)

The superposition of the image


MoO3 crystal and the DP of MoO3

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Rotation of the Image

• There is no angle rotation between the image and DP, that we can
simply know the growth direction/plane by putting the image and DP
together.
(0001)AlN
(0001)InN

Direct beam

InN
[0001]InN

AlN
[0001]AlN

Si

InN film on buffered AlN/(111)Si substrate

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Remarks
1. Carbon-film replica and a known crystal (e.g. graphite) are used
to calibrate the magnification for low-magnification and high
resolution TEM image, respectively.

2. Camera Length is a crucial factor for analyzing the DPs, R increases


with the increased camera length.

3. The rotation of image differs at different magnifications, please


make sure that before you analyze your specimen, although the
rotation has been removed in most TEMs.

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Any Questions?

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