HAC714C: INTRODUCTION TO TRANSMISSION

ELECTRON MICROSCOPY (TEM) TABLE OF CONTENTS

Angélique Letrouit-Lebranchu angelique.lebranchu@umontpellier.fr

 General introduction to Transmission Electron Microscopy

 Electron Diffraction

 Exercise: indexation of Diffraction pattern

 Exam: Wednesday, December 15, 9.45am

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WHAT IS A MICROSCOPE? EARLY DEVELOPMENT OF ELECTRON MICROSCOPE

 Electron microscopes are scientific instruments

that use a beam of energetic electrons to
examine objects on a very fine scale.

 Micro= small/tiny + Scope= to view/to observe  Electron microscopes were developed due to the
limitations of Light Microscopes which are limited
by the physics of light.
 1928-1931: Knoll and Ruska, in Berlin began
development of electron lenses and built a prototype
of Electron Microscope
 An instrument used for viewing very small objects, such as mineral samples or
animal or plant cells, typically magnified several hundred times.
 1986: Nobel Prize in physics for Ernst Ruska
(TEM), Gerd Binnig & Heinrich Rohrer (STEM)

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LIGHT MICROSCOPE VS TEM LIGHT MICROSCOPE VS TEM

FEI titan cubed ultimate Jeol 2200 FS

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LIGHT MICROSCOPE VS TEM SCALE AND MICROSCOPY TECHNIQUES

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WHAT DO WE KNOW ABOUT ELECTRONS? WHAT DO WE KNOW ABOUT ELECTRONS?

 Wave Characteristics of electron gives rise to coherent scattering  Particle characteristics gives rise to
(diffraction) characterise X-Rays

 Negatively charged particules We can apply an electric field to accelerate it!

 Electron Duality:
 Behave as waves Diffraction patterns when passing by crystals
 Behave as particles excitation of inner shell électrons: X-Ray chemical Analysis

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WHAT DO WE KNOW ABOUT ELECTRONS? WHY ELECTRONS?

 Wavelenght of electrons as a fonction of acceleration voltage

 λ (100kv)=3,7.10-3nm
 λ (200kV)=2,5.10-3nm
 λ (300kv)=2,0.10-3nm

 Green light: around λ =500 nm

  λ e- five orders of magnitude smaller than visible light!!!

For electron microscopist, relativistic effect cannot be ignored at energies >= 100keV
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INTERACTIONS ELECTRONS-MATTER
Multitude of signals resulting from the electron matter interaction
TEM TECHNIQUES
 Crystallographic informations:
 Electron diffraction
 Selected Area Diffraction (SAD)
 Convergent beam electron diffraction (CBED)
 Imaging
EDX  Low magnification mode
 Dark field / Bright field imaging
 High resolution (transmission) electron microscopy (HRTEM or HREM)

 Chemical analysis:
 X-rays
 Energy dispersive X-ray spectroscopy (EDS or EDX)
 Electrons
 Electron energy loss spectroscopy (EELS)
EELS
Electron Diffraction
STEM/HAADF
High Resolution Electron Microscopy
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Electron diffraction Imaging

 Low magnification
 SAD

A1.5+xSb+5−2xAl5O11.5 (A = Sr, Ba) phases A. Letrouit et al., Solid State Sciences, V10, 2008, P982-990
Homogeneous precipitation of δ-Ni2Si (orthorhombic)
A1.5+xSb+5−2xAl5O11.5 (A = Sr, Ba) phases in Cu [T. EPICIER, Z. SUN, MATEIS (2007)]
 Lattice parameters, reflections condition, possible space(s) group(s) A. Letrouit et al., Solid State Sciences, V10, 2008, P982-990

control of the sample: good sample preparation, homogeneity, number of characteristic phases
Imaging
 High Resolution TEM
A1.5+xSb+5−2xAl5O11.5 (A = Sr, Ba) phases
b
a
A. Letrouit et al., Solid State Sciences, V10, 2008, P982-990
The contrast between two adjacent areas in a TEM image can be defined as the difference in
the electron densities in image plane. Comparison between calculated and recorded images
confirmation of the atomic structure, stacking fault…
Chemical Analysis
 Electron Energy-Loss Spectroscopy (EELS)
Some of the electrons will undergo inelastic scattering, which means that
they lose energy and have their paths slightly and randomly deflected
The Electron Energy Loss (EEL) spectrum can be
roughly split into two different regions: the low-
loss spectrum (up until about 50eV in energy
loss) and the high-loss spectrum. The low-loss
spectrum contains the zero-loss peak as well as
the plasmon(quantum of plasmon oscillation)
peaks (quantum of plasmon oscillation) and
contains information about the band structure
and dielectric properties of the sample. The
high-loss spectrum contains the ionisation
edges that arise due to inner shell ionisations in
the sample. These are characteristic to the
species present in the sample, and as such can
be used to obtain accurate information about
the chemistry of a sample.
Chemical Analysis
 Energy Dispersive Spectroscopy (EDS)
AlK SiK
MgK
CuL CuK
The incident beam may excite an electron in an inner shell, ejecting it from the shell while creating
an electron-hole where the electron was. An electron from an outer, higher-energy shell then fills the
hole, and the difference in energy between the higher-energy shell and the lower energy shell may
be released in the form of an X-ray.
determination of the elemental composition of the sample
INSTRUMENTATION
 Basic requirements:
 Voltage: 200-300kV
 Brillant source: W, LaB6, FEG
 Essential extras
 Diffraction and image simulation software
 Image processing software
 Possible extras:
 Scanning transmission electron microscope (STEM)
 Energy dispersive X-Ray detector (EDS)
 Electron Energy Spectrometer (EELS)
 X-Ray and EELS mapping software
 Cold stage, tensile stage, heating stage…
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INSTRUMENTATION

TEM TECHNIQUES
1: electron gun
2: anode
3: condenser(s) system
4: condenser diaphragm
5: thin object
6: objective lenses
7:objective diaphragm
8: image plan of the
objective
9: projection lenses
10: fluorenscent screen
11: vacuum pump

Specimen : Ø < 3 mm
thin thickness ≈ 10 - 100 nm

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INSTRUMENTATION INSTRUMENTATION

 Illumination system: Focuses the electron beam

and directs it to the specimen
 Objective Lens and stage: The electrons exiting the
specimen are recombined to create a first image
and diffraction pattern (DP) in a reproducible
manner (most important part of the lens system
as it defines the quality of the final image)
 Imaging system: Complicated system magnifying
and projecting the DP (diffraction mode) or image
(image mode) onto the viewing screen

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INSTRUMENTATION

ELECTRON SOURCES

There are strict requirements to produce an electron beam with the necessary properties.
There are two types of source:

 thermionic: tungsten (W) filaments or lanthanum hexaboride (LaB6) crystal

produces electrons when the source is heated. Materials used has to be refractory materials (high melting
point, they should not melt or vaporise) or materials with low work fonction.

 field-emission sources (or ‘guns’ as they are often called): fine tungsten (W) needle : W monocrystal
<310>//W<310> covered by a monolayer of ZrO
 produces electrons when a large electric potential is applied between the thin W needle and an anode

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ELECTRON SOURCES: THERMIONIC SOURCES ELECTRON SOURCES: FIELD EMISSION

 Tungsten filament:
needle radius= 50 µm; T ≈ 1700°-2400°C

 LaB6 crystal:  Cold needle: very thin W needle (T=20°C)

pyramid-shaped with 4 natural sides, the electron are produced from the top of
the pyramid <110>, T ≈ 1500°C
 Thanks to the geometry of the needle (« needle
effect»)(r< 0.1 μm), there is an important field at the end
of the needle (107 Vcm-1) : Electrons are extracted by
This material is chosen for its good emission quality, its lifetime is longer than for a W tunneling effect.
filament.
 If the local field is very intense (107 Vcm-1), even without
 Emission of the electrons: Based on Joule effect
enough thermal energy (needle at room temperature),
 Electrons need to acquire enought energy to overcome the potential barrier that
keep them in the solid. For this the filament is heated to an appropriate electrons get over the energy barrier by tunneling effect. It
temperature and the emission is then due to thermal agitation.
is called cold emission, only possible with very thin needle.
 Electrons are going out in the vacuum and then they are accelerated by an electric
field

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ELECTRON SOURCES: COMPARISON BETWEEN THE MOST COMMON
SOURCES LENSES
Emission Thermionic Field emission In general:
Source W LaB6 Froide (W) Schottky (W/ZrO)
 Lenses control basic operational functions in electron microscopes
Operating temperature (K) 2800 1400-2000 300 1800
 Used to focus and magnify the electron beam and the images
Vacuum (Pa) 10-2 10-3 10-3.10-4 10-7 10-8 <10-6  Electromagnetic lenses are still very imperfect and cause errors
Needle radius 50 μm 10 μm 100 nm 100 nm
 Very complex structure and way of working

Current density (A/cm2) 1-3 30 104 106 500 → Understanding the lens system is crucial in order to understand the basic structure of electron microscopes
Work Fonction (eV) 4.5 2.7 4.5 2.7 and being able to properly operate them.

Brightness (A/cm2.sr-1) 104-106 106-107 108-109 107-108

Energy spread (eV) 2-5 1.5-2 0.3-0.5 0.4-0.7

Lifetime 30-100 1000 >1000 >5000

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LENSES LENSES
 All rays from a point in the object are brought back to a point
in the image and all parallel rays (whether parallel to the optic
 Simple reminder of light optics and Link between axis or not) are brought to a focus in a plane at a position
optical construct and diffraction pattern: depending on their angle to the axis.
 Convex lens magnifies, focuses parallel rays to one point  3 important distances:
 Electron lenses act as combination of convex glass lenses
1. the distance from the object plane to the lens (the object
(approx.)
distance do),
2. the distance from the lens to the image plane (the image
distance di),
 A fundamental principle of how a lens works is that
an electron passing through the middle of the lens is 3. the distance from the lens to the back-focal plane (the
unaffected so we can draw its path as a straight line. focal length f)
All other electron paths are bent when they pass
through the lens.
Newton’s lens equation:

1/f= 1/d0+1/di
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 OBJECTIVE LENS
CONDENSER LENS
 Same structure as the condenser lenses, but producing a very strong field with a small
TEM lens systems usually consist of two or three condenser lenses and one objective lens. focal length

 Performance of this lens determines the image quality (resolution, contrast, etc)

 When running a current through → bore and gap should be as tight as

the copper coil, an inhomogenous possible in order to get small
(strong on the sides, weakest on aberration coefficients, but are limited
axis) magnetic field inside of the by the side-entry-type specimen
bore is created through the pole holder (standard)
pieces
 Radial and circumferential forces Top-entry-type holders: Specimen is
cause the electrons to spiral surrounded by the objective lens
towards the centre of the lens → complicated construction,
and bring the beam to focus restricted analytical possibilities

33 34
Image: Williams, Carter: Transmission electron microscopy, 1996 Image: www.jeol.co.jp/en/words/emterms/glossary_file/file/objective_lens.jpg

ELECTRON PATH THROUGH THE MAGNETIC FIELD ELECTRON PATH THROUGH THE MAGNETIC FIELD

 Electromagnetic lenses works like the light optics in principle.

 Electrons are used instead of photons.
 Electrons leave the object and focused into an image.
 When an electron with charge q (= –e) enters a magnetic field with a
strength B (Tesla) and an electric field of strength E, it experiences a  e- -path parallel to optical- axis Z: spiraling all the
force F, known as the Lorentz force, which depends on the velocity of the way through the lens
electron, v. All these factors are related through the equation:

F = q(E+ v B)=-e(E+ vB)

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APERTURES APERTURES

 An aperture is often inserted into a lens. The aperture limits the  Diaphragms come in several forms
collection angle (β) of the lens as shown schematically in Figure 9 , depending on their function and
and such an aperture in the objective lens allows us to control the the particular microscope. They can
resolution of the image formed by the lens, the depth of field and the be either individual disks, each
depth of focus, the image contrast, the collection angle of the with a particular aperture diameter,
electron energy-loss spectrometer, the angular resolution of the or they can be a series of different
DP…. apertures in a single metal strip.
 Physically, the aperture may reside above, in, or below the plane of
the lens.
 The diameter can be as small as
 Usually the apertures are circular holes in metal disks and the disks 10 μm, which is about the smallest
are made of either Pt or Mo, which are both refractory metals. circular aperture we can make
consistently or up to ≈ 0.3mm (300
μm).
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SPHERICAL ABERRATION CS
SPHERICAL ABERRATION CS

 This is the principal defect of the objective

lens.
 This defect occurs when the lens field
behaves differently for off-axis rays. For
our electromagnetic lenses, the further off
axis the electron is, the more strongly it is
bent back toward the axis.
Gaussian image plane Gaussian image plane
 As a result, a point object is imaged as a disk of
finite size, which limits our ability to magnify detail
because the detail is degraded by the imaging
process. We can now correct this aberration, but it
Plane of least confusion still limits the resolution of most TEM’s so we need Plane of least confusion
to examine it carefully.

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CHROMATIC ABERRATION CC
CHROMATIC ABERRATION CC

 We assumed that the electrons are monochromatic, but they are not really. However, we can make very good
high-voltage supplies and the variation of the electron energy due to the power supplies is usually smaller  The objective lens bends electrons of lower
than one part in 106, which is 0.1 eV for a 100-keV beam. energy more strongly and thus electrons
from a point in the object once again are
 As we already discussed before, depending on the electron source the actual energy spread in the beam may blurred to form a disk in the Gaussian
vary from 0.3 eV (cold FEG) to 1 eV(LaB6). This range is still so small that we generally do not have to worry image plane (and a smaller disk in the
about chromatic aberration affecting the image resolution. The exception is if you happen to have a Cs plane of least confusion).
corrector, in which case, after compensating for Cs, Cc is the next most-persistent aberration. Lens elements
that can correct for Cc are being developed (monochromator)

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ASTIGMATISM
ASTIGMATISM

 In image mode a point will appear as an

ellipse.

 It appears because objective lense doesn’t

have a perfect revolution symetry. The focal
length differs in 2 axial perpendicular planes
to the electron trajectories.

1. Distortion before or behind the focal plane

Fig 12: Astigmatism

ASTIGMATISM
SAMPLE PREPARATION
 The TEM specimen, when you made it, must be electron transparent (usually) and representative of the
material you want to study. In most cases (but not all) you would like your specimen to be uniformly thin,
stable under the electron beam and in the laboratory environment, conducting, and non-magnetic.
 Few specimens approach the ideal and usually you have to makecompromise. In general, we can divide
specimens into two groups: self-supporting specimens and specimens resting on a support grid or thin
washer; the grid or washer is usually Cu but could be Au, Ni, Be, C, Pt, etc
 Which method you choose would depend on what you want to learn about your material.
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SAMPLE PREPARATION
 There are many ways to produce a TEM specimen; the one you choose will depend on the
information you need, time constraints, availability of equipment, your skill, and the
material…
 One important point to keep in mind is that your technique must not affect what
you see or measure, or if it does, then you must know how. Specimen preparation
artifacts may be interesting, but they are not usually what you want to study.
SAMPLE PREPARATION
 The type of TEM specimen you prepare depends on what you are looking for so you need
to think about the experiment that you are going to do before you start your preparation.
 For example, is mechanical damage to be avoided at all costs, or can it be
tolerated so long as chemical changes don’t occur—or vice versa?
Is the specimen at all susceptible to heat or radiation?
Depending on the answers to these questions, some of the following methods will
be inappropriate.
SAMPLE PREPARATION REFERENCES

 scienceportfolio1.weebly.com

 http://www.nanoscience.gatech.edu/zlwang/image/research/tem/fig1.jpg

 Transmission electron microscopy by William and Carter

 A diagram summarizing the different preparation philosophies is shown in Figure 1:
 Rsscience.com

 Physical Principle of Electron Microscopy, An Introduction to TEM, SEM and AEM, Second Edition, Egerton,
R.F. (2016), p.34
 www.globalsino.com/EM/
 PPT - Electron Microscopy: Lecture 1: Introduction to the Transmission Electron Microscope (TEM) PowerPoint
Figure 1: Summary of different preparation philosophies Presentation - ID:5955069 (slideserve.com)

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