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Electron Microscopy Basics

The document discusses electron microscopy techniques including electron diffraction, energy dispersive X-ray spectroscopy, electron energy loss spectroscopy, and scanning transmission electron microscopy. It covers the basic principles, instrumentation, and applications of these techniques.

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Nithiesh Naik
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13 views

Electron Microscopy Basics

The document discusses electron microscopy techniques including electron diffraction, energy dispersive X-ray spectroscopy, electron energy loss spectroscopy, and scanning transmission electron microscopy. It covers the basic principles, instrumentation, and applications of these techniques.

Uploaded by

Nithiesh Naik
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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Electron Microscopy

Dr. Priyabrat Dash


NIT Rourkela, India 1
Dr. Priyabrat Dash
NIT Rourkela, India 2
Dr. Priyabrat Dash
NIT Rourkela, India 3
Dr. Priyabrat Dash
NIT Rourkela, India 4
Dr. Priyabrat Dash
NIT Rourkela, India 5
Dr. Priyabrat Dash
NIT Rourkela, India 6
Dr. Priyabrat Dash
NIT Rourkela, India 7
Dr. Priyabrat Dash
NIT Rourkela, India 8
Dr. Priyabrat Dash
NIT Rourkela, India 9
Dr. Priyabrat Dash
NIT Rourkela, India 10
Single electron outer shell
excitation
Zero Loss Peak

Elastic scattering: Inelastic scattering:


Coulomb attraction by nucleus Coulomb repulsion (outer shell electrons)
Dr. Priyabrat Dash
NIT Rourkela, India 12
Dr. Priyabrat Dash
NIT Rourkela, India 13
Dr. Priyabrat Dash
NIT Rourkela, India 14
Dr. Priyabrat Dash
NIT Rourkela, India 15
Dr. Priyabrat Dash
NIT Rourkela, India 16
Dr. Priyabrat Dash
NIT Rourkela, India 17
Dr. Priyabrat Dash
NIT Rourkela, India 18
Dr. Priyabrat Dash
NIT Rourkela, India 19
Dr. Priyabrat Dash
NIT Rourkela, India 20
Dr. Priyabrat Dash
NIT Rourkela, India 21
Dr. Priyabrat Dash
NIT Rourkela, India 22
Dr. Priyabrat Dash
NIT Rourkela, India 23
Dr. Priyabrat Dash
NIT Rourkela, India 24
Dr. Priyabrat Dash
NIT Rourkela, India 25
Dr. Priyabrat Dash
NIT Rourkela, India 26
Electron matter interactions
Coherent incident
high-kV beam

Second electrons
sample Incoherent elastic From within the specimen (SEM
backscattered electrons (SEM)
Characteristic
X-rays (EDS)
Auger electrons (XPS)
Visible light
Sample
Incoherent inelastic
Bremsstrahlung scattered electrons
X-rays (EDS) (EELS)
Direct beam
Incoherent elastic
(imaging, diffraction,
Coherent elastic forward scattered
EELS)
scattered electrons (STEM, Electrons (STEM,
Diffraction, EELS) diffraction,EELS)
Energy Dispersive X-ray
Spectroscopy
(EDS)
EDS spectrum
EDS spectrum
EDS: Energy Dispersive Spectroscopy
EDXS: Energy Dispersive X-ray
Spectroscopy
X-EDS: X-ray Energy Dispersive
Spectroscopy
EDX: Energy Dispersive X-ray analysis
Quantification
Peak intensities are proportional to concentration and specimen thickness.

They removed the effects of variable specimen thickness by taking ratios of


intensities for elemental peaks and introduced a “k-factor” to relate the intensity
ratio to concentration ratio:

𝐶𝐴 𝐼𝐴
= 𝐾𝐴𝐵
𝐶𝐵 𝐼𝐵

Each pair of elements requires a different k-factor, which depends on detector


efficiency, ionization cross-section and fluorescence yield of the two elements
concerned.
The Detector

Crystal (Si(Li)): Absorbs the energy of incoming x-rays by ionization, yielding free
electrons in the crystal that become conductive and produce an electrical charge
bias. The x-ray absorption thus converts the energy of individual x-rays into
electrical voltages of proportional size; the electrical pulses correspond to the
characteristic x-rays of the element.
Detection Mechanism

When X-rays deposit energy in a semiconductor, electrons are transferred from the
valence band to the conduction band, creating electron-hole pairs. The energy required
for this transfer in Si is 3.8 eV at liquid-N2 temperature. (This energy is a statistical
quantity, so don’t try to link it directly to the band gap.) Since characteristic X-rays
typically have energies well above 1 keV, thousands of electron-hole pairs can be
generated by a single X-ray. The number of electrons or holes created is directly
proportional to the energy of the X-ray photon. Even though all the X-ray energy is not,
in fact, converted to electron-hole pairs, enough are created for us to collect sufficient
signal to distinguish most elements in the periodic table, with good statistical precision.
EELS

Electron energy loss spectrometry (EELS) analyzes transmitted electrons to


determine the amount of energy they have lost in interactions with the sample.

It provides information about the interacting atoms, including elemental identity,


chemical bonding, valence and conduction band electronic properties, surface
properties, and element-specific pair distance distribution functions.
EDS vs. EELS
Applications
Scanning transmission electron microscopy (STEM) combines the principles
of transmission electron microscopy and scanning electron microscopy and
can be performed on either type of instrument. Like TEM, STEM requires
very thin samples and looks primarily at beam electrons transmitted by the
sample. One of its principal advantages over TEM is in enabling the use of
other of signals that cannot be spatially correlated in TEM, including
secondary electrons, scattered beam electrons, characteristic X-rays, and
electron energy loss.

Like SEM, the STEM technique scans a very finely focused beam of
electrons across the sample in a raster pattern. Interactions between the
beam electrons and sample atoms generate a serial signal stream, which is
correlated with beam position to build a virtual image in which the signal
level at any location in the sample is represented by the gray level at the
corresponding location in the image. Its primary advantage over
conventional SEM imaging is the improvement in spatial resolution.
CY 524 (Nanoscience and Nanotechnology)
Dr. Priyabrat Dash 38
NIT Rourkela, India
CY 524 (Nanoscience and Nanotechnology)
Dr. Priyabrat Dash 39
NIT Rourkela, India
Electron Diffraction

• Elastic Scattering Events


– Bragg diffraction
• nl=2d sinq
Electron Diffraction

• Four conditions in Back Focal Plane (BFP) of the


objective lens:

– No sample No reflections (only transmitted beam)


– Amorphous Transmitted beam + random scattering
– Polycrystal Transmitted beam + rings
– Single crystal Transmitted beam + spots
Electron Diffraction
Angle of incidence ~1/20 to even come close to
satisfying the Bragg condition.

Therefore only the lattice planes close to parallel to the


beam are involved in diffraction.
Electron Diffraction
• Think of TEM as a
diffraction camera

Rd=lL
R is measured
Transmitted Beam
d is the unknown
L
l is the electron wavelength
L is the camera length Diffracted Beam
(lL is the camera constant)

Reciprocal relationship between


lattice spacing and distance from R
the transmitted spot.
Electron Diffraction
• Au (111) ring [2.35 Å d-spacing]

With 200KV and L=65cm the (111)


ring should be at about 7.5mm from
the transmitted beam

Rd=lL
R=0.027A*650mm/2.35A

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