TEM: Transmission electron microscopy

SiGe for QCLs

http://www.microscopy.ethz.ch/

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 Basic principles, first TEM
Wave length of electrons: 200kV: λ= 0.00251 nm
(v/c= 0.6953, m/m0= 1.3914)

Additional correction for relativistic

effects, since the electron's velocity
approaches the speed of light, c
Electrons are deflected by both
electrostatic and magnetic fields

Force from an electrostatic field F=

-e E

Force from a magnetic field

F= -e (v x B)

Electrons are accelerated by

an electric potential (measured
in volts) and focused by
electrostatic and electromagnetic
lenses onto the sample. The
transmitted beam contains
information about electron a) The first electron microscope built by Knoll
Ernst Ruska: Nobel
density, phase and periodicity; this and Ruska in 1933, b) The first commercial
Prize in physics
beam is used to form an image. electron microscope built by Siemens in 1939.
1986

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A transmission Electron Microscope is anologous to a slide projector as indicated by
Philips below

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 (SEM) and TEM
1) The stream of the electron from the
electron gun is then focused to a
small, thin, coherent beam by the use
of condenser lenses. The first lens
determines the “spot size”; the
general size range of the final spot
that strikes the sample. The second
lens actually changes the size of the
spot on the sample.
2) the electron-sample interaction takes
place in three different ways. One is
unscattered electrons (transmitted
beam), elastically scattered electrons
(diffracted beam) and inelastically
scattered electrons.
3) The main function of the objective
lens is to focuses the transmitted
Projector lens electron from the sample into an
image.
4) Objective aperture enhances the
contrast by blocking out high-angle
diffracted electrons
5) The projector lens are used to expand
the beam onto the phosphor screen.

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TEM BASICS

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TEM BASICS
The objective lens forms a diffraction pattern in
the back focal plane with electrons scattered by
the sample and combines them to generate an
image in the image plane (1. intermediate image).
Thus, diffraction pattern and image are
simultaneously present in the TEM. It depends on
the intermediate lens which of them appears in the
plane of the second intermediate image and
magnified by the projective lens on the viewing
screen. Switching from real space (image) to
reciprocal space (diffraction pattern) is easily
achieved by changing the strength of the
intermediate lens.
In imaging mode, an objective aperture can be
inserted in the back focal plane to select one or
more beams that contribute to the final image
(BF, DF, HRTEM). Selected area electron
diffraction (SAED) aperture is an aperture in the
plane of the first intermediate image defines the
region of which the diffraction is obtained.

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 TEM: Magnetic lenses

Magnetic lenses influence electrons in a similar way as convex glass lenses do with light. Thus,
very similar diagrams can be drawn to describe the respective ray paths. Consequently, the
imaginary line through the centers of the lenses in an electron microscopes is called optical
axis as well. Furthermore, the lens equation of light optics is also valid in electron optics, and the
magnification is defined accordingly:
1/u + 1/v = 1/f
Magnification M = v/u

f: focal length; u: object distance; v: image distance

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 TEM Diffraction
Use Bragg's law -  = 2d sin 

But much smaller

(0.0251Å at 200kV)

if d = 2.5Å,  = 0.288°
->  = 2d sin  ≈ 2 d

Electron diffraction is a collective scattering phenomenon with electrons being (nearly elastically) scattered by atoms in
a regular array (crystal). This can be understood in analogy to the Huygens principle for the diffraction of light. The
incoming plane electron wave interacts with the atoms, and secondary waves are generated which interfere with each
other. This occurs either constructively (reinforcement at certain scattering angles generating diffracted beams) or
destructively (extinguishing of beams).
As in X-ray diffraction (XRD), the scattering event can be described as a reflection of the beams at planes of atoms
(lattice planes). The Bragg law gives the relation between interplanar distance d and diffraction angle Θ which is the
distance between the reflection and the origin of the reciprocal lattice:
nλ = 2dsinΘ
Each set of parallel lattice planes, which correspond to planes decorated with atoms in the structure, generates a pair of
spots in the electron diffraction pattern with the direct beam in their center.
Since the wavelength λ of the electrons is known, interplanar distances can be calculated from ED patterns.
Furthermore, information about crystal symmetry can be obtained. Consequently, electron diffraction represents a
valuable tool in crystallography.

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 TEM Diffraction
Diffraction

2 ≈ tan 2 = R/L
𝜆𝐿
𝑅= =
 = 2d sin  ≈ d (2) 𝑑
𝐶𝑎𝑚𝑒𝑟𝑎 𝐶𝑜𝑛𝑠𝑡𝑎𝑛𝑡
R = L /d 𝑑

L is "camera length"
L is "camera constant"

For small scattering angles, Bragg's law becomes from nλ=2dsinθ (for n=1) to λ=~2dθ
tan2θ can also be approximated as ~2θ (again, small angles) which can be described as R/L, where R is the
distance of the diffracted beam from the central, non-diffracted beam on the image plane (i.e. phosphorescent
screen, plate camera etc.) and L is the distance between the image plane and the sample.
Altogether 2θ = ~λ/d = R/L
Rearranging we'd get Rd = λL, or d = λL/R
This expression is useful as it directly (and simply) relates the d-spacing and the distance between diffraction
spots. λL is constant and it is called the camera length.
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 Indici di Miller

Each vector in the reciprocal space will be a

combination of the basic vector a*, b* and c*

r* = d*hkl = ha* + kb* + lc*

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 TEM Diffraction
(i) the reflecting lattice planes are almost parallel to the direct beam (left figure),
(ii) There are many reflection planes (mid fig)
(iii) The incident electron beam is the zone axis of the reflecting sets of lattice
planes (right figure).

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 TEM Diffraction

Diffraction, which mathematically corresponds to a Fourier

transform, results in spots (reflections) at well-defined
positions. Each set of parallel lattice planes is represented by
spots which have a distance of 1/d (d: interplanar spacing)
from the origin and which are perpendicular to the reflecting
set of lattice plane. The two basic lattice planes (blue lines)
of the two-dimensional rectangular lattice shown below are
transformed into two sets of spots (blue). The diagonals of
the basic lattice (green lines) have a smaller interplanar
distance and therefore cause spots that are farther away
from the origin than those of the basic lattice. The complete
set of all possible reflections of a crystal constitutes its
reciprocal lattice.

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TEM BASICS
The objective lens forms a diffraction pattern in
the back focal plane with electrons scattered by
the sample and combines them to generate an
image in the image plane (1. intermediate image).
Thus, diffraction pattern and image are
simultaneously present in the TEM. It depends on
the intermediate lens which of them appears in the
plane of the second intermediate image and
magnified by the projective lens on the viewing
screen. Switching from real space (image) to
reciprocal space (diffraction pattern) is easily
achieved by changing the strength of the
intermediate lens.
In imaging mode, an objective aperture can be
inserted in the back focal plane to select one or
more beams that contribute to the final image
(BF, DF, HRTEM). Selected area electron
diffraction (SAED) aperture is an aperture in the
plane of the first intermediate image defines the
region of which the diffraction is obtained.

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TEM diffraction examples
Single crystals
Electron diffraction patterns
of Ta97Te60 along two perpendicular
directions. The parameters of the
tetragonal unit cell can be
determined from these SAED
patterns: a = 27.6, c= 20.6 Å.

Electron diffraction pattern of Si viewed with the

diffraction spots indexed.

As a diffraction technique, SAED can be used to identify

crystal structures and examine crystal defects. It is similar
to X-ray diffraction, but unique in that areas as small as
several hundred nanometers in size can be examined,
whereas X-ray diffraction typically samples areas several
centimeters in size

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Electron Diffraction in TEM: Applications

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Applications- amorphous vs crystalline materials

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Applications- Study of local ordering in Pb2ScNbO6
complex perovskite

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Applications- Study of defects

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TEM Image
Simplified representation of the
ray path leading to the first
intermediate image in the image
plane of the objective lens.
Electrons, which come from the
condenser system of the TEM, are
scattered by the sample, situated
in the object plane of the objective
lens. Electrons scattered in the
same direction are focused in the
back focal plane, and, as a result, a
diffraction pattern is formed there.
Electrons coming from the same
point of the object are focused in
the image plane. In the TEM, the
first intermediate image is
magnified by further lenses
(projective system).

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Conventional TEM: Contrast

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TEM Image: Bright field

In the bright field (BF) mode of the

TEM, an aperture is placed in the back
focal plane of the objective lens which
allows only the direct beam to pass. In
this case, the image results from a
weakening of the direct beam by its
interaction with the sample. Therefore,
mass-thickness and
diffraction contrast contribute to image
formation: thick areas, areas in which
heavy atoms are enriched, and
crystalline areas appear with dark
contrast. It should be mentioned that the
interpretation of images is often
impeded by the simultaneous occurence
of the contrast-forming phenomena.

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Conventional TEM: Bright Field Contrast

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TEM Image: Dark Field

In dark field (DF) images, the direct

beam is blocked by the aperture
while one or more diffracted beams
are allowed to pass the objective
aperture. Since diffracted beams
have strongly interacted with the
specimen, very useful information is
present in DF images, e.g., about
planar defects, stacking faults or
particle size.

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Conventional TEM: Dark Field Contrast

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 TEM Image: BF vs DF
BF DF

TEM BF and DF images of the same area of microcrystalline

Electron diffraction pattern: the spots indicate
Zirconium Oxide (ZrO2). In the BF image (left), some
the presence of single microcrystals. The
crystals appear with dark contrast since they are oriented
apertures (red circles) are localized around the
(almost) parallel to a zone axis (Bragg contrast). In addition,
direct beam for recording the bright field (BF)
thickness contrast occurs: areas close to the edge are thinner
image and around a few diffracted beams for
and thus appear brighter (lower right side) than those far of
the dark field (DF) image. The intense direct
the edge (upper left side). In the DF image (right), some of
beam is blocked by a metal rod (black shadow
the microcrystals appear with bright contrast, namely such
on the left center) to avoid overexposure.
whose diffracted beams partly pass the objective aperture

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 Scanning TEM analyses
FIB milling was used to extract a
cross lamellar section of the device.
The millling (on the left ) and the
extraction (on the right) are shown
above. The lamella was thinned to a
final thickness of about 150 nm.

STEM-HAADF image of Sample B

(double step in glovebox), showing
all the layers in the device, labelled
on the
schematic on the left, and associated
EDX elemental maps of the same
area

G. Divitini, S. Cacovich, C. Ducati

Divitini et al. Nature Energy 15012 (2016)
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Inelastic Scattering

Incoming electrons ionize the

atom (coreshell excitation), lose
energy

- The energy loss can be

measured (EELS)

Or

- collect emitted x-rays (XEDS)

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 XEDS Analysis
EDS can be used to determine which chemical
elements are present in a sample, and can be
used to estimate their relative abundance. The
accuracy of this quantitative analysis of sample
composition is affected by various factors

• Many elements will have overlapping X-ray

emission peaks
• The nature of the sample; since X-rays are
generated by any atom in the sample that is
sufficiently excited by the incoming beam,
these X-rays are emitted in all directions
(isotropically), and so they may not all escape
the sample.
• The energy of the X-ray and the
composition, amount, and density of
material.

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 XEDS Analysis
Silicon Drift Dector (SDD)

This drift detector structure:

• has very low capacitance which provides
excellent energy resolution at relatively short
electronic processing times and also allows
operation at very high count rates.
• Has very low leakage current so optimum
performance can be achieved at temperatures
which are readily reached by electronic Peltier
cooling systems, removing the need for liquid
Nitrogen.

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 InP Barriers in InAs

1.5 nm InP

(a) TEM image of a whisker with a diameter of 40 nm. (b) FFT image of (a). (c) Inverse FFT using the
information closest to the InP 200 reflection. (d) Colored superimposed image, using an identical mask over the
InP and InAs 200 reflection, respectively.

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 EELS
(electron energy loss spectroscopy)

The material is exposed to a

beam of electrons with a known,
narrow range of kinetic
energies. Some of the electrons
will undergo inelastic scattering,
which means that they lose
energy and have their paths
slightly and randomly deflected.

DETECTED PHENOMENA:
• Phonon excitations,
• Inter- and intra-band transitions
• Plasmon excitations
• Inner shell ionizations.

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Why EELS?

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 CNTs

CNT filled with CdI nanoparticles

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 Nano Trees
InP Trees

GaAsP trees

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 TEM- sample preparation
Size and thickness of the sample Ion milling: 2KV Ion milling: 100V
Diameter: 3 mm
1) Reduce size of large sample
2) Use 3 mm grid support for small sample

Thickness: between 10 et 200 nm depending on the

material and the kind of observation to be done
1) depend on chemical composition
2) high resolution observation, EELS analysis or not Sample has to be:
• electrically conductive
• stable under vacum
• free of hydrocarbures
contamination
• should not contain
artefacts that could lead
to a wrong analyse

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 TEM- Selection of suitable support grid
Depends on the analysis to be done and the particles size

• Standard carbon coated grid (C thickness 25–40 nm) [1]

• Ultrathin carbon film (4–5 nm) [2]
• Holey carbon film with ultrathin carbon windows (5 nm)
• Holey carbon film [3]
• Lacey carbon film [4]

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 TEM- sample preparation: ion milling
Using electric discharge, Ar+ ions of some kV are generated and focused on
the sample. The goal is the crystal lattice destruction at the surface followed
by ejection of superficial atoms.

DRAWBACK and ARTEFACT:

• Surface roughness
• Creation of amorphous layer on
both surfaces
• Ion implantation
• Creation of dislocations
• Modification of stoichiometry
• Differential thinning rates on
different compounds or phases
• Heating

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 TEM- sample preparation: FIB
Focused ion beam (FIB) etching Advantages
process: it uses a focused beam of ions • FIB allows for rapid production of site specific
(usually Ga+), (within 50 nm) TEM specimen
• FIB has a lower preferential sputtering rate than
any other conventional TEM sampling method
Disadvantages
• The use of high energy Ga+1 ions for milling leads to
the formation of damaged, amorphous layers, and
formation of voids in some materials
• Ga implantation
• Physical and electrical properties can be affected

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