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Electron Microscpy

The document provides an overview of basic types of electron microscopes, specifically Transmission Electron Microscopes (TEM) and Scanning Electron Microscopes (SEM), detailing their operational principles, electron interactions with matter, and the types of signals generated. It discusses the components of SEM, including electron guns, lenses, and detectors, as well as the characteristics of secondary and backscattered electrons. Additionally, it highlights the importance of various techniques like Energy Dispersive X-ray Spectroscopy (EDX) for material analysis and emphasizes the versatility of SEM in different applications.

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0% found this document useful (0 votes)
5 views24 pages

Electron Microscpy

The document provides an overview of basic types of electron microscopes, specifically Transmission Electron Microscopes (TEM) and Scanning Electron Microscopes (SEM), detailing their operational principles, electron interactions with matter, and the types of signals generated. It discusses the components of SEM, including electron guns, lenses, and detectors, as well as the characteristics of secondary and backscattered electrons. Additionally, it highlights the importance of various techniques like Energy Dispersive X-ray Spectroscopy (EDX) for material analysis and emphasizes the versatility of SEM in different applications.

Uploaded by

pranilbanoth12
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Basic types of electron microscopes

Transmission electron microscope (TEM) Scanning electron microscope (SEM)


Basic types of electron microscopes

Transmission electron microscope (TEM) Scanning electron microscope (SEM)


Electron beam Electron beam

sample 60-100nm

Projection Surface

Typical electron energies: 60 – 300 keV ≤30 keV


Electrons
-10
0.1 nm 10
• Rest mass m=0 9.1× 10−31 kg nonrelativistic
• Charge Q =−e =−1.602 × 10−19 C relativistic correction
• Rest energy E0 m=
= 0c
2
511 keV

• Planck constant =h 6.6256 × 10−34 Nms


-11
0.01 nm 10
• A non-relativistic approach:
1
E eU
= = m 0v 2

wavelength [m]
• Energy SEM
2
• Momentum p m=
= 0v 2m0E
h h h TEM
• de Broglie wavelength λ= = =
p m 0v 2m0E 1 pm 10
-12

h 1
• Wavelength including relativistic λ=
correction 2m0E E
1+
2m0c 2

-13
10 3 4 5 6
10 10 10 10
accelerating voltage [V]
How do electrons interact with matter
• Unscattered electrons (no
E0 E0 collision)
• Elastic scattering on nuclei of
atoms of the matter
ATOM • primary electron changes
mainly its direction by an angle
Θel
electron
orbits • often backscattered electrons
∆E>0 • Inelastic scattering
(e.g. SE electron, X-ray, etc.) • primary electron slightly
nucleus
changes its direction by the
angle Θin and loses part of its
energy ΔE
• inner-shell ionization
• secondary electrons (SE)
• continuum X-rays
(Bremsstrahlung)
• phonons (lattice vibrations -
Elastic scattering Inelastic scattering heat)
Eel = E0 Ein = E0 − ∆E • plasmons (oscillations of loosely
bound electrons)
〈Θel〉 >> 〈Θin〉 • cathodeluminiscence
• …
Usually multiple scatter occurs

• Scattering occurs depending on the material


of the sample and the energy of the electron
• The path of the primary electron can be
emission of SE/photon reversed during the interaction with the
energy loss
sample (backscattered).
• Secondary electrons (SE) have very little
energy and therefore only those at the surface
emission of SE/photon get out of the sample
Mean free path Λ: energy loss • Due to the loss of energy during inelastic
Λel: elastic scattering scattering, the primary electron can be
emission of SE/photon absorbed in the sample (electron range)
Λin: inelastic scattering energy loss
Λtot: total scattering
emission of SE/photon
energy loss

emission of SE/photon
energy loss

emission of SE/photon
sample
energy loss

inelastic scattering elastic scattering


Electron scattering: atomic number and energy

Λ increases with decreasing Z


Λ increases with increasing E
Interaction volume Monte Carlo simulations of electron scattering
Electron energy

Interaction volume
Atomic number
Spectrum of signal electrons

Schematic energy spectrum of emitted


electrons consisting of
• secondary electrons (SE; ESE ≤ 50 eV)
• backscattered electrons (BSE; EBSE > 50 eV)
• and more signals like Auger electrons (AE)
or low-loss electrons (LLE) used mainly for
material science

Origin and information depth of


• secondary electrons (SE)
• backscattered electrons (BSE)
• Auger electrons (AE)
• X-ray quanta (X)
in the diffusion cloud of electron range R for
normal incidence of the primary electrons
(PE)
X-rays: Energy dispersive X-ray spectroscopy (EDX)

Characteristic X-rays Values for individual elements are well known

E = ∆E-Ex

Vacuum

Conduction band

Valence band

EL3 L3
E0 EL2 L2
EL1 L1
Ex = EK-EL3
EK

Energy is characteristic of a given element


E = E0 -∆E
X-rays: Energy dispersive X-ray spectroscopy (EDX)
X-rays: Energy dispersive X-ray spectroscopy (EDX)

EDX spectrum recorded from an area or point = all elements in one place

Color representation of selected elements in the sample = one element in all pixels
Si Fe C

WDX/WDS: wavelength dispersive X-ray spectroscopy (much better energy resolution, but slow)
Scanning electron microscope (main parts)

• Electron gun is source of electrons


with required parameters
• Condenser lens converge the electron
beam emitted from electron gun into
finer beam
• Deflection coils are used to scan the
electron beam in X and Y directions
and change size of the area to be
scanned (magnification)
• Objective lens converges electron
beam into a fine beam and focus it on
the sample surface.
• Detectors for capturing signal for each
pixel
• Synchronization of data acquisition
and scanning system to receive an 2D
image
Kinds of electron guns
Tungsten LaB6 Cold field-emission Schottky

Tungsten LaB6 CFE Schottky


Material Tungsten hairpin Lanthanum Tungsten single Tungsten single
hexaboride single crystal crystal/ zirc.
crystal oxide
Cathode temp ~2300 °C ~1500 °C RT °C ~1500 °C
Brightness 106 A/cm2·sr 107 A/cm2·sr 109 A/cm2·sr 108 A/cm2·sr
Energy width ~2 eV ~1.5 eV 0.2-0.3 eV 0.3-1 eV
Max. probe current ~100 nA ~100 nA ~10 μA ~100 nA
Working pressure 10-4 Pa 10-5 Pa 10-8 Pa 10-7 Pa
Lifetime 50-100 h 200-1000 h 2-4 y 2-3 y
Electron lenses
Condenser lens Objective lens Standard type
• generally used in low-end
SEM
• WD can be high (longer
depth of focus)
• optionally can be set also
in snorkel type

In-lens type
• best resolution SEM
• only short WD
• limited sample size

Electron lenses in SEM: magnetic/electrostatic


lenses to focus the accelerated virtual electron
source from electron gun into a fine probe Semi in-lens (snorkel) type
• high-end SEM
onto the sample surface.
• virtual lens close to
Condenser lens: “shaping” electron beam sample (sample in EM
(responsible for its intensity) field)
Objective lens: focusing the electron beam
into a fine probe
Depth of focus in SEM
Light Microscope SEM

25µm Radiolarian

Magnific Depth of focus (example)


ation
Light microscope SEM
10 60 µm 1000 µm
100 8 µm 100 µm
1,000 0.2 µm 10 µm
10,000 --- 1 µm

Effect of aperture
diameter (D) and working
distance (WD) of depth
of focus
(Light bulb coil) D=600μm, WD=10mm D=200μm, WD=10mm D=200μm, WD=38mm
Detector of secondary electrons (SE)

Everhart-Thornley (ET) detector


• SE electrons (very low energy <50 eV) are accelerated towards 10 kV electric
field and hit against the scintillator for conversion into the light signal which
leads to the photomultiplier tube (PMT) through a light pipe
Signals in SEM and their detection

SE detector:
ET detector, in-lens (TLD) detector
X-ray detector detector:
EDX, WDX detectors BSE detector:
retractable BSE detector,
in-lens detektor
CL detector

STEM detector:
bright-field, dark-field detectors,
2D-STEM detector
Secondary electrons (SE)

SE signal:
• is formed by very low energy of secondary electrons (≤ 50 eV) generated from the collision
between the primary electrons and loosely bound outer electrons
• gives mainly information about topography (topographic
contrast), less about composition Edge effect
• increases with decreasing electron energy
many SE
• weaker dependence on atomic number Z
• is strongly dependent on tilt of the sample (edge effect)
some SE
some SE

sample
SE signal

SE signal

atomic number electron energy


Secondary electrons (SE)

• SE detector type • Artefacts


• upper “in lens” detector • charging • In non-conducting
samples the electron
probe current remains
in sample 
accumulation of charge
 artefacts mainly for
SE (reducing probe
current, lowering E0,
imaging with BSE,
metal coating,…)
• lower “ET” detector • contamination • Result of interaction of
electron beam with
residual gasses and
hydrocarbons on the
sample surface
(ensure cleanliness,
decrease probe current,
use plasma cleaner,…)
Secondary electrons (SE)

• Effect of penetration depth • Enhancement of contrast by metal coating to reduce


• Interaction volume
5 kV • Charging effect
• Beam damage

No coating Gold

20 kV

Gold/Palladium Iridium

Bar: 1 µm (Sample: Diatom)


Backscattered electrons (BSE)

BSE signal:
• is formed by primary electrons which are backscattered (all electrons in the energy range from
50 eV to E0)
• in general number of BSEs is much lower than SEs
• gives mainly information about material (material contrast), less about topography
• increases with increasing atomic number Z up to E0~30 keV
• increases with increasing tilt of the sample
• is almost independent on energy for E0 >10 keV

for higher electron energy


atomic number
BSE signal

BSE signal

atomic number electron energy


Backscattered electrons (BSE)

• BSE detector type


• retractable BSE detector (standard BSE like ET for SE)
• annular active area (well defined)
• very effective
• basic types
• scintillator based (usually YAG detector)
• usually 1 segment
• semiconductor detector
• usually multi-segment

• in-lens detector (only for snorchel type objective)


• various possibilities depending on SEM producer
and SEM type
SE vs. BSE imaging

• Immunogold labeling of surface proteins (rubber nanoparticles isolated from


Taraxacum)

SE BSE

SE: sample surface information (topography)


BSE: due to targeted immunolabeling (gold nanoparticles bound to immunoglobulin) the
possibility to identify specific parts on the sample (bright Au nanoparticles)
Conclusions

• SEM is a versatile instrument that can be used for many purposes and can be
equipped with various accessories
• Secondary electrons (SE): mainly topography
• Backscattered electrons (BSE): mainly material contrast
• Transmitted electrons (STEM): mass-density contrast
• X-ray: chemistry (composition)
• Use the full power of your SEM - play around with the settings (modern
SEMs offer many options)

• EM manufactures:

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