Do Minh Nghiep

Materials Science Center

Electron Microscopy
and Diffraction
1. Introduction
 Contact

ƒ Lecturer: Đỗ Minh Nghiệp

Room No: 303-C10
303 C10 ĐHBKHN
Tel. 38691332
e-mail: nghiep@mail.hut.edu.vn
g p@
ƒ Class time: Mon 14:50-17:20
ƒ Class room: D6-106

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 C
Course outcomes
t
ƒ U
Understanding
d t di off image
i f
formation
ti b glass
by l andd
electromagnetic lenses.
ƒ Understanding of the physics of scattering.
scattering
ƒ Understanding of the construction of various types of
electron microscopes, the function of the various
parts and methods of image formation.
ƒ Understanding of methods of sample preparation for
SEM and TEM.
TEM
ƒ Ability to utilize EDS and WDS results for elemental
(microchemical) analysis.

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 C t t
Content
• Introduction to EM
• Electron optics
• Electron source and vacuum system
• Electron-matter interaction
• SEM
• TEM
• Electron diffraction
• EDS and WDS
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 Lab works

1. Preparation of an alloy specimen to observe

its microstructure by SEM
2. Determination and imaging of chemical
composition of the alloy specimen by SEM
and EDS
3 Preparation
3. P ti off an TEM specimen
i t image
to i
its microstructure and to analyze ED pattern

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R di
Reading
ƒ Textbook: Handouts
ƒ References:
1. D. B. Williams and C. B. Carter, Transmission electron microscopy, Books
1 to 4, Plenum Press, 1996
2. P. Hirsch, et al.; Electron microscopy of thin crystals; Huntington, N. Y., R.
E Krieger Pub.
E. Pub Co.,
Co 1977
3. Elizabeth M. Slayter, Henry S. Slayter; Light and electron microscopy;
Cambridge (England), New York, Cambridge University Press, 1992
4 Ludwig Reimer; Transmission electron microscopy: physics of image
4.
formation and microanalysis; Berlin, New York, Springer-Verlag, 1993
5. John M. Cowley; Diffraction physics; Amsterdam, New York: North-Holland
Pub. Co., New York: Sole distributors for the U.S.A. and Canada, Elsevier
North-Holland, 1981
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 G di
Grading

The weighting factors used to determine

th fi
the finall grade:
d

ƒ Attendance and seminar grading: 10 %

ƒ Lab work and reports: 20 %
ƒ Mid-term test and final exam: 70 %

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 Lecture schedule
ƒ Week 1 Whyy electron microscope p - a brief historyy
ƒ Week 2 Electron sources, Vacuum
ƒ Week 3 Electron optics, Electromagnetic lenses, Resolution limits
ƒ Week 4 Electron beam -specimen interactions
ƒ Week 5 Mid-term test
ƒ Week 6 SEM: Scanning system, Detectors, SE image,
Backscattered image, Resolution
ƒ Week 7 TEM: System configuration
configuration, Image formation (Mass- thickness,
thickness
Diffraction, Phase)
ƒ Week 8 Microprobe analysis: Detection systems (EDS, WDS), Qualitative
and quantitative analysis
ƒ Week 9 Practical lab for SEM, EDS
ƒ Week 10 Electron diffraction, Diffraction patterns
ƒ Week 11 Practical lab for TEM, ED
ƒ W k 12
Week Fi
Finall exam

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 Introduction

• M t i l characterization
Materials h t i ti
• History
• Why EM ?
• Classification of EMs
• Overview of SEM and TEM

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 What does materials
characterization mean?
ƒ Character: a sum of qualities that make a person / thing different from
others
ƒ Characterize: to indicate / describe / investigate / express the character
of a person / thing (action)
ƒ Characterization: the act / process / activities of characterizing
ƒ Materials characterization:
- in specifying
p y g the internal microstructure of an engineering
g g materials
including the chemistry, the crystallography, the structural morphology
- in terms of engineering properties of materials, and reflects the need to
know the p physical,
y chemical and mechanical p properties
p of the materials
before we can design an engineering system or manufacture its components
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 Why materials
characterization is important?

It is believed that optimization of material properties through control of

microstructure is the most disciplinal.
disciplinal

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 Five levels of materials
structure and properties

• Sub atomic level: Physics

Sub-atomic
• Atomic level: Physics and Chemistry
• Molecular level: Chemistry
• Microscopic level: Chemistry and Materials Sci.
and Eng
Eng.
• Macroscopic level: Mechanical and Materials Eng.

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 Macroscopic properties
of materials
ƒ Mechanical properties
ƒ Chemical
Ch i l properties ti
ƒ Physical properties
- Thermal property
- Optical property
- Electrical property
- Magnetic property

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 Equipments
for composition
analysis
(atomic &
molecular levels)

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 Equipments
for structural
analysis
(microscopic
levels)

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 History
y

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 Milestones
Optical/light microscope (OM): visible light limits magnification of max
1000-2000X and resolution of 0,2 mm. Electron microscope (EM) is
developed for overcoming these limitations.
ƒ 1932 - 1938:
- The first TEM (1932, idea of EM, Max Knoll and Ernst Ruska,
Germany)
- The first SEM (1938, later STEM - TEM with scanning coil, Knoll and
von Ardenne),
Ardenne) thin sample
ƒ 1940 -1952:
- The first SEM for thick sample (1942, Zworykin et al., RCA
L b t i U.S.A),
Laboratories U S A) resolution
l ti 1 mm.
- The first Field Emission electron source (1942, FE Gun)
- The SEM with resolution of 50 nm (1952, Oatley and McMullan,
E l d)
England)
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 Milestones

ƒ 1959-1967:
- SEM withi h stereoscan (Wells)
(W ll )
- Performance of SE detector (1960, Everhart and
Thornley)
- The first commercial EM (1965)
- Electron-channeling contrast for crystal orientations
(
(1967))
[Oatley (1982), J. Appl. Phys. 53, R1]

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 Contributors

Antonie van Leeuwenhoek,

1932 theory of EM
15th cent.,
cent single lens microscope
1986 Nobel Prize winners
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 Contributors

James Hillier

1939: First Toronto EM

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 Contributors

EM
1938 - First SEM is produced
by von Ardenne
1940

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 Contributors
The prototype of the
first Stereoscan
supplied by the
Cambridge Instrument
Company to the
duPont Company,
U.S.A. (Stewart and
Snelling1965)

McMullan’s original
microscope

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 Why
y EM ?

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 D fi iti
Definition
ƒ Microscope - A device with a lens or series of lenses
that enlarge (magnify) the appearance of an object
(not applied to SEM).
SEM)
ƒ Image - Perception of an object using your eyes (vision).
One can sense an object j without vision ((touch, etc..).
)
Requires visible light.
ƒ Lens - A lens is an optical component which is used to
focus beams of radiation.
radiation Lenses for light are usually
made of a glassy material, whereas non-uniform
electromagnetic fields are used as lens for electrons.

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 Definition
ƒ Magnification
g - The ratio between imageg size to the
object size. Can be varied by changing the distance
between the object and the final lens (of the eye) or by
inserting a second lens between the two.
two
ƒ Wavelength - Distance between peaks of the waveform.

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 Definition

ƒ Resolution
- RP is the smallest
distance between two
points at which two or more
objects can be
distinguished
g as separate.
p
- Resolution is the ability of
a lens to distinguish
between two point sources
at infinity, when they are
viewed in the image plane.

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 Abbe’s
Abbe s formula RP ≈ (1/2)λ

ƒ In 1870, Ernst Abbe (1840-1905) derived mathematical

expression for resolution of microscope: Resolution is
limited to ≈ 0.5 the wavelength of illuminating source.

61 λ
0,61
0
RP = ----------------
NA = n.sinα
n sinα - numerical aperture
RP- resolution power NA = n.sin
RP
n - index of refraction α - half angle of illumination

ƒ In the microscopy the resolution of a lens can be increased by a)

increasing the half angle of illumination, b) increasing the refractive
index of the lens by using Crown glass, and c) decreasing the
wavelength of illumination.
illumination

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 How to increase NA ?
ƒ Increase sin α ( decr. working
g distance,, incr. size of the lens):
)
↓ ↑

ƒ Increase refractive index n (oil refractive index is

higher than air)

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How to decrease wavelength ?

Replacing visible light

by electron beam

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 Viewing scales

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 Resolution limits

The smallest
Th ll t di
distance
t b
between
t ttwo points
i t th
thatt can be
b
resolved by
ƒ Human eye: 0
0.1-0.2
1 0 2 mm
ƒ Light microscope: 0.2 μm
ƒ SEM: 1-2 nm
ƒ TEM: 2Å
This high resolution is achieved by TEM thanks to the
use of a high energy electron beam (small wavelength).

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 Vi i
Viewing options
ti
Resolution Sample Sample
Instrument Magnification
[µm] environment thickness
E
Eye 1 200 Ai
Air Thi k
Thick
Magnifying
2-10 15-100 Air Thick
glass
Optical
200-1300 0.2 Air or Oil Thick
microscope
SEM 10-10
10 105 0 01
0.01 Vacuum Thick

TEM 103-1.5X106 0.00014 Vacuum Thin

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 Electron- dual ((wave-
Electron- (wave-particle)) character:
Light particles - Matter waves
Antone de Broglie (1924): Theory of wave nature of electrons
Hermann Busch (1924): Axial magnetic fields refract electrons

h - Planck constant (6.624 X 10-27 erg/s)

v - electron velocity (p = mv: momentum)
V- accelerating voltage
mo - rest electron mass
m - relativistic electron mass (9
(9.11
11 x 10-28 gram = 1/1837 of proton)
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 Resolution of microscopes
D B
De Broigle
i l relationship
l ti hi

λe≈ ( 150 / V )1/2 Angstroms (Å)

ƒ Resolution limit of light microscope:
- λ can decrease
d tto 470 nm
- n.sinα is limited to ≈ 1.6
- Thus the maximum resolution is about 200 nm
ƒ Cannot go beyond this even with better optics.
Solution ? Use illumination of shorter wavelength

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 R
Resolution
l ti off microscopes
i

ƒ Resolution of electron microscope:

- λ can decrease to ≈ 10-3 nm
- n.sinα is very small, because n ≈ 1 and α ≈ 0.1 radians
- Thus,
Thus for a beam of 100 keV we get a wavelength
of 0.0389 Å and a theoretical resolution of 0.0195 Å !
- But in p
practice most TEMs will only
y have an actual
resolution 2.4 Å at 100 kV

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 Electron ƒ Refractive index n is dependent
on a ray of illumination entering a
refraction/bending medium of differing density causing
the beam to bend.
bend

ƒ In the vacuum environment of

an electron microscope p the index
of refraction is 1.0 and therefore
NA depends solely on the half
angle α of illumination.

ƒ In electron microscopy the

refractive index cannot exceed
1 0 the
1.0, th half
h lf angle
l is
i very small,ll
and thus the only thing that can be
Refractive index:
n = tanαi/tanαr adjusted is decreasing the
wavelength of illumination
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 B di
Bending by
b lenses
l
ƒ Converging (convex/positive) lens: bends
rays toward the axis. It has a positive focal
length. Forms a real inverted image of an
object placed to the left of the first focal point
and an erect virtual image of an object placed
between the first focal point and the lens.

ƒ Diverging (concave/negative) lens: bends

the light rays away from the axis. It has a
negative focal length. An object placed
anywhere to the left of a diverging lens results
in an erect virtual image. It is not possible to
construct a negative magnetic lens although
negative electrostatic lenses can be made.

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 Types of lenses

Glass lenses (curved glass

or mirror) for visible light

concave convex

Electromagnetic lenses
(solenoid/coil) for
subatomic particles
(electron, protons,
positrons)

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 Classification
of EMs

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 Equipments for structural analysis
(microscopic
( i i levels)
l l )

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 Two groups of EMs

ƒ Scanning Electron Microscopes - SEM

Versions: Environmental (ESEM) / Low Voltage (LVSEM) /
V i d Pressure
Varied P (VPSEM) / Elevated
El t d Pressure
P (EPSEM)
(EPSEM),
Field Emission (FESEM)
ƒ Transmission Electron Microscope - TEM
Versions: High Resolution (HRTEM), Scanning- (STEM),
Field Emission (FETEM), Energy Filtering (EFTEM)
ƒ Analytical Electron Microscope - AEM
Versions: SEM-EDS/WDS, STEM-EDS-EELS

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 Overview of EMs

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 Scanning Electron
Microscope - SEM
ƒ SEM is an instrument using electron light to image and
control the material sample in very fine scale.
ƒ What is imaged and controlled:
– Surface topography (SE: microstructure roughness)
– Surface morphology (SE (SE, BSE: microstructure shape
and size)
– Composition contrast (BSE)
– Elemental composition (EDS/WDS: qualitative and
quantitative analysis)
– Crystallite orientation (BSED)
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 SEM versus OM and TEM (imaging)
ƒ The SEM is a distinctly
different instrument in terms of
image formation than is an
optical microscope and a TEM.
ƒ In the SEM, the probe
examines the object one spot at
a time, then gives out an array
(in 2-D)
2 D) of the results from
many spots.
ƒ The optical microscope, (also
TEM) conversely, takes the
signals from simultaneously-
examined spots, and gives
th
them b k allll att once.
back
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 SEM versus TEM (signals used)

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 Construction of SEM

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 Construction of SEM

JEOL SEM 6335F

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 F
Functions
ti off SEM main
i parts
t
ƒ Electron gun (filament/cathode, Wehnelt
cylinder, anode): generating/ emitting
electron beam
ƒ Lens system (condense and objective
lenses): focusing/linking electron beam
ƒ Scanning coil: scanning electron beam
over specimen surface
ƒ Detectors: collecting electrons and/
x-rays
ƒ Mearurement system (Cathode Ray
Tube-CRT, electronic devices): data
amplifying, acquisition and processing

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 What processes happen in SEM

ƒ F
Formation
ti off accelerated
l t d electron
l t b
beam t
toward
d
specimen by a positive voltage (kV)
ƒ Condensing electrons into a monochromatic and
narrow beam with electromagnetic lenses and
metallic diaphragms/apertures
ƒ Focusing and scanning electron beam into
specimen surface through electromagnetic
lenses and scanning g coil
ƒ Beam-specimen interaction
ƒ Data acquisition and imaging

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 In environmental SEM
ƒ Ionizing of rest gas to eliminate electric charge on
the surface of non-conductive samples
samples, because:
- A low vacuum is used
- Non
Non-conductive
conductive specimens without coating are
avaiable
- Hydrated specimens are allowed
- Chemical composition is analyzed for only
specimen (without coating)

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 SEM capabilities
Backscattered Imaging S
Secondary
d El
Electron
t IImaging
i
(BSI) (SEI)
ƒ Compositional contrast ƒ Surface topography,
Morphology Particle sizes
Morphology,

Scanning
g Electron
Microscope
Transmitted Electron Imaging (SEM) Electron Backscattered
(TEI) Diffraction (EBSD)

ƒ Internal ultrastructure Energy-Dispersive X-ray ƒ Crystallographic info

Spectrometry (EDS)

ƒ Elemental composition, mapping and linescans

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 Pros and cons of SEM
ƒ Pros
P (
(strengths):
h )
- Higher resolution and depth of field than that of OM (the surface of
materials can be studied to about 2 nm resolution on good HRSEMs)
- Allows for direct observation of surface morphology
- In-situ environmental studies are possible (e.g. catalysts in an
atmosphere)
- Microanalysis (composition of small areas)
- Typically a low power technique, so organic material can be studied
- Very good at looking at an average of sizes and arrangements in a
sample
- Easy operation and maintenance
- Negligible damage of specimen (through coating, heating during
radiation))

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 Pros and cons of SEM

ƒ Cons (weaknesses/limitations)
(weaknesses/limitations)::
- Specimens must be suitable in vacuum
- False/artificial outputs through sample preparation
- Coating non-conductive samples is required
- The crystallinity cannot be determined
- Resolution is often not sufficient to tell all of the surface features
- Scanning gpprocess is slow and so sample p may y move leadingg to
distorted images

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 Transmission Electron
Microscope - TEM

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 A modern TEM

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 TEM vs OM (imaging)

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 Construction of TEM

Electrons path in TEM:

electron source →
condenser lens(es) and
aperture → sample →
objective lens(es) and
aperture → projector
( ) → screen
lens(es)

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 Imaging in TEM

ƒ TEM is designed to project a

magnified image of specimen
onto screen (we see only the
shadow of the specimen).
ƒ It’s thanks to contrast
(intensity difference) of
t
transmitted
itt d unscattered
tt d and d
forward diffracted / scattered
beam.

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 3D--object → 2D
3D 2D--image

Each particle image represents a 2D

projection of the 3D object

A single projection image is

plainly insufficient to infer the
structure of an object.
j

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 3D--object → 2D
3D 2D--image

Watch out!
A cover slide!

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 High Resolution
TEM - HRTEM
Contrast ((intensity
y difference)) on image
g pplane:
ƒ Mass-thickness contrast (BF imaging)
ƒ Diffraction contrast (BF, DF imaging)
ƒ Phase contrast / HREM and Moire’ HREM image

fringes (HR imaging) Interference pattern

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 HRTEM:
HRTEM:
comparison of parameters

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 TEM capabilities
p
Bright- and Dark-Field Imaging Electron Diffraction
(BF/DF imaging)
i i ) (ED)

ƒ Internal ultrastructure ƒ Crystallographic info

ƒ Nanostructure dispersion
ƒ Defect identification

Transmission Electron
High-Resolution Microscope
Transmission Electron (TEM) Electron Energy Loss
Microscopy (HR-TEM) Spectroscopy (EELS)

ƒ Interface structure Energy-Dispersive ƒ Chemical composition

ƒ Defect structure X-ray Spectrometry ƒ Other bonding info
(EDS)

Elemental composition, mapping and linescans

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 Pros and cons of TEM
ƒ Pros
- Very high resolution is possible
- Images can be obtained directly
ƒ Cons
- Expensive
p machine for high
g resolution
- Extreme heating of the sample can destroy it
- Only thin samples can be studied
- Sample must be in a good (10-6 Torr) vacuum

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 Comparison of SEM and TEM

SEM TEM
ƒ High resolution for thick bulk ƒ High resolution (1,2-1,5 Å)
samples: 20-50 Å (most for very thin samples (most
commercial SEM) and < 10 Ao commercial TEM)
(research SEM) ƒ 3D
3D-imaging
imaging impossible
ƒ 3D-imaging due to large ƒ Information about crystal
depth of field structure (crystal lattice
ƒ Small magnification avaiable and orientation,
orientation
as for light microscope dislocation, twinning,…)

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