Transmission Electron Microscopy

Chapter 1
Introduction of TEM

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 Outline

• Why We Need Electron Microscope?

• History of EM

• The Interactions of Electrons and Matters

• Applications

• Limitations

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 What is Electron Microscopy ?
Definition from Wikipedia
• Microscopy is the technical field of using microscopes to view objects and
areas of objects that cannot be seen with the naked eye.

• Transmission electron microscopy (TEM) is a microscopy technique in which

a beam of electrons is transmitted through an ultra-thin specimen,
interacting with the specimen as it passes through it.

Optical (light) Microscope Scanning Electron Microscope Transmission Electron Microscope

(OM) (SEM) (TEM)

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 Why we need microscope ?
To view objects and areas of objects that cannot be seen with the naked eye.

Source : Optical microscope Electron microscope

visible light Electrons
(400 nm to 700 nm)

Lens Class lens with different reflect index Electromagentic Lens

To deflect the light into the focus mode To deflect the electron beam into the focus mode

Lens Maker's formula 1/d0+1/di=1/f

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 What is Electron Microscopy ?
• The electron microscopy is the use of specialized microscopes that
interact a high energy electron beam with samples as a mean to probe
the structure of a material.

• Electron microscopes have a greater resolving power than light

microscopes, allowing us to see much smaller objects in finer detail (sub
nanometer resolution).

• TEM is the expensive and large

instrument, generally standing along in
the small and specially-designed room
and requiring the trained personnel to
operate it.

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 Why We Need TEM?
• Among the analysis technologies, TEM is one of few that can look into the
materials and has the atomic scale resolution.

InGaN Multi-nanodisks ADF HR-STEM

@ GaN Nanorod (Atomic Image)

1 m TEM HR-TEM 50 nm
(Lattice Image)
SEM STEM
HR: high resolution, STEM: Scanning Transmission Electron Microscopy, ADF: Annular Dark Field

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 Why We Need TEM?
A
• Defect Investigation (Stacking Fault) B
C-axis
A
B
Crystal 1
Crystal 2 ADF HR STEM Ga N

Shift
A
B
GaN Nanorod A
B
Stacking
TEM Perfect A Fault
B
Crystal C
B
C
B

Distortion HR: high resolution, STEM: Scanning Transmission Electron Microscopy, ADF: Annular Dark Field

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 Why We Use Electrons
Resolving Power: the ability to distinguish two points (Rayleigh
Criterion)
Unresolved Well Resolved Just Resolved
• Rayleigh limit (Resolution)

0.61
=

:
:
:
: of lens

• The resolution of OM is about 300 nm (if is 550 nm).

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 Resolving Power

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 History

• The Discovery of the Electrons

Joseph J. Thomson
The Nobel Prize in Physics 1906

" in recognition of the great merits of his theoretical and experimental

investigations on the conduction of electricity by gases "

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 History

• Wave Nature of the Electrons Theoretical Basis

Louis de Broglie
The Nobel Prize in Physics 1929

"for his discovery of the wave nature of electrons"

de Broglie hypothesis (1924): wave-particle duality

Energy of the particle =

= =
Wave-energy relation = =
de Broglie wavelength
: , : , : , : , :
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 History

• Wave Nature of the Electrons

Experimental Evidence

• Davisson-Germer Experiment (1927)

Clinton J. Davisson George P. Thomson

(1/2) (1/2)
The Nobel Prize in Physics 1937

"for their experimental discovery of the

diffraction of electrons by crystals"

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 Why We Use Electrons
• The wavelength of electron beam can be tuned by changing the
accelerating voltage (energy) of the electron source.

1.22 : ( )
= = : :
(2 ) e: charge
V: accelarating voltage (V)
E: energy eV

• When the energy > 100 keV, the =

relativistic effect counts. The
2 (1 + )
equation should be modified. 2
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 History

• The Design of the EM

Ernst Ruska Gerd Binnig Heinrich Rohrer

(1/2) (1/4) (1/4)
The Nobel Prize in Physics 1986
"for his fundamental work in electron optics,
and for the design of the first electron The first EM built by Ruska and Knoll.
microscope” to E. Ruska
"for their design of the scanning tunneling
microscope“ to G. Binnig and H. Rohrer
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 Timeline of TEM Developments
1932
1929 1st TEM
Quantum -Knoll and Ruska
1980s
Mechanics
- Schrödinger and Heisenberg
High Voltage TEM

1950s 1970
1927 The Observation Development
Davisson-Germer of Dislocations in of STEM
1897 Experiment Stainless Steel -A. Crewe

Discovery of -Davisson and Germer

the Electron 1964
-J. J. Thomson 1939 1st Commercial 2000s
1924 1st Commercial SEM Cs-Corrected TEM
de Broglie TEM
Hypothesis -Ruska
-L. de Broglie

1900 1920 1940 1960 1980 2000

10 nm 0.2 nm < 0.1 nm
Resolution
of TEM 0.05 nm
1 nm

Nobel Prize Laureate

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 Analytical TEM

Requirements:

1. Double-tilting holder
2. EDS or EELS

JEOL JEM 2010

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 in-situ UHV TEM
• Heating

Evaporator
Pre-chamber

CCD Camera
S. C. Wang et al., Nano Lett. 14, 3241-3246 (2014)

• Current Injection

EELS

Vacuum: < 5x10-10 torr

K. C. Chen et al., Science 321, 1066 (2008)

JEOL JEM 2000 V
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 High Voltage TEM

JEM 1.25 MeV HVEM

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 Spherical Aberration (Cs)
Electron Beam

• One of the main defects in optical

system.

• The focal point of the light far from

the axis doesn’t meet that of the light
close to the axis.

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Spherical Aberration (Cs)
w/o Cs correction

w/ Cs correction

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 Spherical Aberration (Cs)

Probe Correction Image Correction

Specimen

CM: mini condenser lens

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 Cs-corrected TEM

Nion SuperSTEM FEI Titan

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 Cs-corrected TEM
Tsing-Hua

Name: JEM-ARM200FTH
Accelerate Voltage: 80/200 kV
Electron Source: Cold type Field Emission Gun
(CFEG) with EDS detector (Oxford X-Max) and
CEOS aberration corrector(CESCOR)

Zone axis: [110]

2 nm
Si Dumbbell Structure

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 Cs-corrected TEM

• Without Cs corrector
- d is 0.2-0.3 nm (depending on the
accelerate voltage) (cross-over point !)
• With Cs corrector - d is 0.06-0.08 nm

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The Interactions of Electrons and Matters

Spatial Distribution Angular Distribution

the contrast in image diffraction pattern

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 The Interactions of Electrons and Matters

• Elastically Scattered Electron • Inelastically Scattered Electron

1. Coherent ( electrons are in phase) 1. Incoherent
Bragg diffracted electrons Electron energy loss Spectroscopy
Selected area electron diffraction (EELS)
(SAED)
Bright-field TEM image
Dark-field TEM image
Two beam condition
Weak beam • Secondary Signals
Phase contrast imaging (HRTEM)
1. Characteristic X-ray
2. Incoherent 2. Bremsstrahlung X-ray
Mass-thickness contrast imaging 3. Visible Light
Z-contrast imaging (HAADF STEM) 4. Secondary Electrons
Backscattered electrons

EDS: Energy Dispersive Spectroscopy; EELS: Electron Energy Loss Spectroscopy; CL: Cathodoluminescence; DP: Diffraction Pattern; BF: Bright Field; DF: Dark Field

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 The Interactions of Electrons and Matters
Backscattered Secondary CL
Electrons Electrons
Characteristic
X-ray

Electrons
Visible Light

Incident
EDS DP
Specimen
Bremsstrahlung
Elastically Scattered
X-ray
Electrons
(Diffracted Electrons)

STEM
Inelastically BF TEM DF TEM
Scattered Electrons
Transmitted
Electrons
EELS
EDS: Energy Dispersive Spectroscopy; EELS: Electron Energy Loss Spectroscopy; CL: Cathodoluminescence; DP: Diffraction Pattern; BF: Bright Field; DF: Dark Field

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The Interactions of Electrons and Matters

• The information provided by TEM

-- Crystal structure CS

-- Microstructure MS

-- Chemical composition CC

-- Chemical bonding CB

-- Electronic structure ES

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Advantages of Using Electrons as the Source
1. Easy to produce high brightness electron beams
• High coherence beams allow us to generate diffraction patterns
and high spatial resolution images .

2. Easily manipulated
• Electron lenses and deflectors are used to easily change focal
lengths and beam directions , which is a necessary operating
condition for flexible imaging devices.

3. High energy electrons have a short wavelength

• Shorter wavelengths means better spatial resolution (Raleigh
Criterion).

4. Electrons interact strongly with matter

• Secondary signals have information specific to the material.
• Elastically scattered electrons –structure, orientation, phase
distribution, and defect content, etc.

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 Morphological and Structural Analysis
• Morphology • Crystal structure
(0001)
(-1100)

InGaN
Diffraction Pattern (DP)

GaN

SEM BF-TEM ADF-STEM

TEM/STEM is the 2D projection imaging ,

However, it provides the information inside High Resolution (HR) TEM Image
the materials. Lattice Image

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 Compositional Analysis
• Energy Dispersive Spectroscopy (EDS)
Indium
22.8 % Gallium
Nitrogen
14.2 %

Intensity (a.u. )
7.1 %

7.3 %

0 50 100 150
Distance (nm)

Quantitative Analysis Linescan

Spectrum
Mapping
(Qualitative Analysis)
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 Compositional Analysis
• Electron Energy Loss Spectroscopy (EELS)

Spectrum
(Qualitative and Quantitative Analysis)

Elemental Mapping
Chemical State Determination
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 Variety of Materials
• Metals

Au@Ag Nanoparticles CrMnFeCoNi High Entropy Alloy

S. Gomez-Grana et al. Z. Zhang et al. Nat Commun. 2015, 6, 10143

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 Variety of Materials
• Semiconductors

InGaN/GaN
NiGe

AlGaN/GaN
[110] Ge

ABF STEM ADF STEM

Multi-Quantum Well Structure Ge Film

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 Variety of Materials
• Low-Dimensional Materials

Graphene MoS2

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 Variety of Materials
• Polymers

PS- b -PDMS nanostructures

Organic-Inorganic Hybrid Structure
S. Ren et al. C. J. Chu et al. Macromol

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 Variety of Materials
• Biological Tissues

E. coli Conornavirus-19, TEM image

T. Kim and J. I. Han J. Environ. Manage.

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 Property Characterization
• Cathodoluminescence (CL) Conduction Band
Light or e-beam
Generation of electron-hole pairs
Bandgap (Eg)
Recombination
Valence Band

S. K. Lim et al. Nano Lett.

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 Applications
• in-situ Study (Heating)

ZnO NW In

Diffusion Behavior Thermal Expansion (Nano-thermometer)

S. C. Wang, M. Y. Lu, * et al. Nano Lett. 2014, 14, 3241-3246 N. W. Gong et al. Appl. Phys. Lett. 2008, 92, 073101

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 Applications
• in-situ Study (Biasing)

Observation of Atomic Diffusion at Twin-modified Grain Boundaries in Copper

K. C. Chen et al. Science 2008, 321, 1066

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 Applications
• in-situ Compression Study (Mechanical Property)

Sample

Compression Study of Nanocrystalline Cu

3-axis indenter

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 Applications
• in-situ Tensile Study (Mechanical Property)
Fixed End
Force

Tensile Study of gold Nanowire

Yang Lu et al. Adv. Funct. Mater. 21, 3982–3989 (2011)

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 Limitations
• Sampling
• High spatial resolution of TEM TEM can only view the small part of the
specimen at one time.

The higher the resolution, the worse the sampling ability

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 Limitations
• Sampling
• Before TEM analysis, you must have examined the specimen with techniques
that offer poorer resolution but better sampling.

Know the forest before you start looking into the veins in the
leaves on the trees

Eye OM SEM TEM

Magnification 1000 x 100 kx 1 Mx
Resolution 0.1 mm 200 nm 0.5 nm <0.1 nm
Chemical Information EDS EDS, EELS

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 Limitations
• Interpreting Transmission Images
• The TEM presents the transmitted image in 2-D, but the specimen is 3-D.

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 Limitations
• Interpreting Transmission Images
• The TEM presents the transmitted and projected image in 2-D, but the specimen
is 3-D.

Beware of artifacts, which abounds in TEM images

Electron Beam

Specimen

Screen

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 Limitations
• Interpreting Transmission Images
• 3-D Tomography

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 Limitations
• Interpreting Transmission Images
• 3-D Tomography

(a) (b)

2D TEM images of Ag/NaY at a tilt angle of 0°

(a) and –71° (b). Silver particles are 10-40 nm.

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 Limitations
• Electron Beam Damage
• Ionized radiations of high voltage e-beam will damage the specimen, especially
polymers, biological tissues, ceramics, carbon materials. The effect is significant
if the intense beam is used (Cs correction).

• e-beam damage can be reduced

by,

1. low accelerating voltage.

resolution is worse.

2. low-dose image technique.

Beam damage in quartz after bombardment with 125 keV electrons. With
increasing time, the bubble-like regions (damaged area) increase in size

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 TEMs in DMSE

JEOL JEOL JEOL JEOL JEOL

Model Name
JEM-2010 JEM-3000F JEM-2000V JEM-200FTH JEM-F200
Accelerating
200 KV 300 KV 200 KV 80 KV/200 KV 80 KV/200 KV
Voltage
Cold-Type Cold-Type
Gun LaB6 Field-Emission LaB6
Field-Emission Field-Emission
Image Mode TEM TEM/STEM TEM TEM/STEM TEM/STEM
Cs corrector/EDS/
Function EDS/in-situ EDS/EELS EELS/in-situ EDS/EELS
in-situ
PhD Student w/ Master Student/ Not Open to PhD Student w/
Requirements PhD Student
TEM License PhD Student Public TEM License
Advisor M.Y. Lu S.Y. Chang M.Y. Lu M.Y. Lu Y.L. Chueh

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