Electron Micros
Electron Micros
Consider light as
EM energy
transmitted as a
wave motion.
We can consider
Resolution is defined by: Intensity light as a series of
ro
↓ ripples impinging
upon an obstacle.
Abbe relationship
d 0.61λ 0.61λ
ro = 1 = = Distance
2 n sin α NA
λ = wavelength of illuminant d1
α = semi-angle
n = index of refraction
NA = numerical aperature B.D. Huey, MMAT322 Lecture Notes, University of Connecticut (2005)
Important Terms
Depth of Field
• Depth of Field
• A measure of how much of the object that we are – Height above and below the plane of focus that an image
looking at remains in focus at the same time. remains sharp.
– DOF is a function of magnification, α, and probe size
• Advantages: BEAM
Scan
α
– You get higher depth of field with (many) electron
microscopy techniques than you do with light.
DOF Plane of focused image
– WHY?
Region of image
in focus
SEM
TEM Other instruments we have or are getting
Adapted from: Scanning and Transmission Electron Microscopy, S. L. Flegler, J.W. Heckman Jr., K.L. Klomparens,
Oxford University Press, New York, 1993.
History of electron microscopes
All of this information is related to
• Developed due to limitations of light optical
properties. microscopes (LOMs)
– LOM: ~1000x magnification; 0.2 µm (200 nm) resolution
properties
• Transmission Electron Microscope (TEM) was
developed first.
– M. Knoll and E. Ruska, 1931
– Patterned “exactly” like a LOM. Uses electrons rather than
structure processing light.
Electron microscopy
provides significant • Use apertures and magnetic lenses to focus the
advantages over light stream into a thin focused monochromatic beam
optical microscopy in 1400X
terms of resolution • Focus the beam onto the sample using another
and depth of field magnetic lens.
accelerated towards –
• Electrons are generated and emitted from a filament an anode
Space charge
10-1000 kV
by thermionic emission (W or LaB6) or from a sharp Electron
Beam
+
Filament
Wehnelt
Made from a high Tmp material
with a low work function (φ) in Operation of thermionic gun
A biased grid with a potential that is order to emit as many electrons
a few hundred volts different than as possible. The work function
the filament (cathode). This helps is the energy needed by an • Apply a positive electrical potential to the anode
to accelerate the electrons and electron to overcome the barrier
causes their paths to cross over. that prevents it from leaking out
of the atom. φW = 4.5 eV, φLaB6 =
W Filament 3.0 eV.
• Heat the cathode (filament) until a stream of electrons is
Bias
produced
Wehnelt cap
(negative potential)
resistor – >2700 K for W
Crossover
The effective source of
illumination for the
microscope. The size
Space charge – • Apply a negative electric potential to the Wehnelt
10-1000 kV
is critical for high Electron + – electrons are repelled by the Wehnelt towards the optic axis
resolution Beam
applications.
Crossover
Anode Plate
• Electrons accumulate within the region between the filament tip
(positive potential) and the Wehnelt. This is known as the space charge.
Ground
Anode • Electrons near the hole exit the gun and move down the column
Positively charged metal plate to the target (in this case the sample) for imaging.
at earth potential with a hole in
it. It accelerates the electron
beam to the high tension
potential.
Other Types of Electron Sources
(i.e., electron guns)
The function of the electron gun is:
Higher brightness than W. More $$$ (~$500K) There are two main types of gun. The
thermionic gun, which is the most
commonly used, and the field emission
gun.
B = jcπβ2
ADVANTAGES
jc = current density
Provide higher current density → Higher brightness β = convergence angle
http://www.matter.org.uk/tem/electron_gun/electron_sources.htm
• Secondary electrons:
– escape from a region slightly larger than the incident beam
~1.0 µm
X-ray
(several µm)
resolution – yield the best spatial resolution
Backscattered electrons are not as numerous as others. However, More abundant than other types of electrons. They are electrons
they generally carry higher energies than other types of electrons. that escape the specimen with energies below ~50eV
Auger Electrons (AE) X-rays
• Formation
– De-energization of the atom after a secondary electron is
• Formation
produced. – Same as AE. Difference is that the electron that fills the
inner shell emits energy to balance the total energy of the
– During SE production, an inner shell electron is emitted from
atom.
the atom leaving a vacancy.
– Higher energy electrons from the same atom can fall into the
lower energy hole. This creates an energy surplus in the • Use
atom which is corrected by emission of an outer shell (low – X-rays will have characteristic energies that are unique to
energy) electron the element(s) from which it originated.
– Collect and sort signals according to energy to yield
• Use compositional information.
– AE have characteristic energies that are unique to each – Energy Dispersive X-ray Spectroscopy (EDS)
element from which they are emitted.
– Collect and sort AE according to energy to determine
composition. Foundation of XPS (X-ray photoelectron spectroscopy). XPS can
– AE have very low energy and are emitted from near surface be used to determine the “state” of an atom and to identify chemical
regions. compounds.
– Accelerating Voltage
• Foundation for Transmission Electron Microscopy (TEM) • higher voltages penetrate further into the specimen and
generate larger interaction volumes
~5–50 nm ~100 Å
Secondary electrons ~1 nm – Auger electrons Secondary electrons 10 Å - 30 Å – Auger electrons
~50 nm ~50 nm
TEM ~300 nm TEM <1µm - 2µm
specimen Backscattered specimen Backscattered
thickness electrons thickness electrons
~1.5 µm ~5 µm
X-rays X-rays
??? ~1.0 µm
X-ray resolution X-ray resolution
Z2 • Variants
– Electron Probe Microanalyzer (EPMA)
Z1 < Z2 < Z3 Z3
– Scanning Transmission Electron Microscope (STEM)
Increasing atomic number (Z)
– Environmental SEM (ESEM)
– High Resolution TEM (HRTEM)
– High Voltage TEM (HVTEM)
• Interaction volume is larger for materials that have – etc...
lower atomic numbers and for higher incident beam
energies!
The TEM is analogous to the transmission LOM
TEM LOM
TEM Electron gun Source Light source
Condenser
Vacuum Apertures
• Patterned after transmission light optical microscopes column
system
z z
y y
+ Tilt & rotation Stage
• Yield Following Information: x x
– Morphology Objective
lens
• Size shape and arrangement of particles, precipitates, etc.
Final imaging
– Crystallographic information system
• Atomic arrangement
Phosphor Eyepiece or TV
screen; film; Observation and screen; film;
digital recording recording system digital recording
– Compositional Information system system
• If proper detector is present
1 in 1020 electrons <1 in 106 photons are
are collected collected
No Force
Electrons
follow a
helical path
Adapted from
B.D. Huey, MMAT322 Lecture Notes, University of Connecticut (2005)
for or calibrated. N N
S S Lower scan
coil
Object
Cu coils
Objective Aperture
Grain structure
Crystallographic information
β′
NiAl-1.0Hf 100 nm
250 nm
1hr 4hr Dislocations imaged in NiAl-0.5Zr single crystals deformed at elevated temperatures.
Precipitate distribution
Defect structures
1
2
Hf rich region
β′ Ni2AlHf
• Modes:
– Bright Field/Dark Field modes for visualization of structure
and defects
– Selected Area Diffraction/Convergent Beam Diffraction
for crystallographic information
Sample
• Part of the beam is transmitted through the sample
Objective Lens
Objective Aperture • Focus transmitted portion using the objective lens to form an image
Selected Area Aperture
First Intermediate Lens • Objective and selected area apertures are used to restrict the beam further
– allows examination of diffraction from specific atoms, crystals, features…
Used to
Second Intermediate Lens
magnify image. – SAD, CBD
Projector Lens
• Enlarge image with intermediate and projector lenses
Phosphor Screen
TEM SEM
SEM
Electron gun Electron gun
• Patterned after reflecting light optical microscopes
Vacuum Condenser system
Condenser lens
column
• Yield Following Information: z
y Scan coils
Time
– Topography Also tilts and rotates
Stage
base
x
• Surface features of an object. Detectable features limited to a
few nanometers depth. Objective lens Probe lens
– Morphology z
y
Signal
amplifier
Final imaging system Stage
• Size shape and arrangement of particles, precipitates, etc x
Also tilts and rotates Detector and
Observation processing
– Compositional Information and recording system
system
• Elements and compounds the sample is composed of
CRT
– Crystallographic information
• Possible using new techniques (OIM/BKD)
In the SEM you use secondary signals to acquire images.
– same as TEM but lower V of the optics in First Condenser Lens (C1)
• Condenser:
Condenser lens
an SEM Condenser Aperture
• Probe Lens:
z Signal
– lens that forms a spot at the y
Stage
amplifier
specimen surface x Objective (probe) Lens
Detector and
tor
Also tilts and rotates Detec
• Detector & Processing System: processing
system
• Second condenser lens is used to form electrons into a thin, tight, coherent beam.
– Use fine probe current knob
• Scan coils raster the beam across the sample, dwelling on the points for a
predetermined period of time (selected using scan speed)
• When beam strikes the sample, interactions occur. We detect what comes out of the
sample.
70 Ni
60
Ni-AD
50 Ni-Annealed
40
40
Substrate IDZ Coating Al-AD Al
30
Al-Annealed
20
Composition (at%)
10
0
40
30 Pt-AD Pt
Pt-Annealed
20
0
1.0
10 µm 0.8
Hf-AD
Hf
0.6 Hf-Annealed
0.4
Could get 0.2
additional 0.0
-15 -10 -5 0 5 10 15 20 25
information in Distance (µm)
backscattered or
mixed mode Figure 4.8. Composition profiles of the major elements
measured by WDS in an EPMA.
X-ray Analysis in the SEM
EDS or WDS Useful things to remember about
Al2O3 + ???
SEM operation
• Change magnification by changing the scan area
???
Ni O O Hf
• The probe current/spot size are controlled by the
Al Hf
Pt Pt Al Ni condenser lens current
• EPMA!
Specimen
Receiving slits
R • Data is collected sequentially. Takes more time but
X-ray Detector
the results are much more precise than EDS.
• Backscatter coefficient:
– η = -0.254 + 0.016Z - 1.86x10-4Z2 + 8.3x10-7Z3
SE image Multiple elements of BSE
detector
“Overlapping shadows” • Atomic number contrast:
Reduced resolution
– C = (η1 - η2)/ η1
Single segment of BSE
detector
TOPOGRAPHIC
CONTRAST
TOPOGRAPHIC
CONTRAST
Signals from 2
detectors