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Electron Microscopy: Instruments & Alignment

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7 views40 pages

Electron Microscopy: Instruments & Alignment

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陳楷翔
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd

MSE7015 Electron Microscopy

A Journey into Materials Inner Space

Chapter 2 Instrument & Alignment

Hung-Wei (Homer) Yen


Department of Materials Science & Engineering
National Taiwan University

Homer Yen | Electron Microscopy Ch. 1 1

Check Point
• Instrument
• Overall Configuration
• Electron Source
• Illumination, Image Formation and Magnification
• Recording
• Quality of Electron Microscopy
• Coherence
• Aberration & Resolution Power
• Alignment and Focus
• Illumination Optimization (Alignment)
• Image Focus

Homer Yen | Electron Microscopy Ch. 1 2


Overall Configuration

Source………………………………………………………..

Illumination………………………………………………

Specimen (interaction)………………………………
Focus………………………………………………………..

Magnification……………………………………………

Imaging…………………………………………………….

Homer Yen | Electron Microscopy Ch. 1 3

Overall Configuration (TECNAI)

Homer Yen | Electron Microscopy Ch. 1 4


Electron Source
• Thermal Emission Gun
• Tungsten Hairpin
• LaB6 Gun (Single Crystal)

• Field Emission Gun (FEG)


• Schottky FEG
• Cold FEG

100 μm

Homer Yen | Electron Microscopy Ch. 1 5

Electron Emission
• Thermal Emission
• Richardson Law for the current
density (j):
𝜑
𝑗 A𝑇 exp
𝑘𝑇
T: temperature
A: Richardson’s constant
φ: work function
k: Boltzmann constant

Homer Yen | Electron Microscopy Ch. 1 6


Electron Emission
• Schottky Effect
• Schottky effect gives a field
suppression:

∆𝜑 𝑒 𝐸/4𝜋𝜖 𝑐𝐸,
𝑐~1.44 10 𝑒𝑉 𝑉/𝑚
• The emission current is
𝜑 ∆𝜑
𝑗 A𝑇 exp
𝑘𝑇
when using a Schottky emitter
(Field-Assisted Thermal Emission)

Homer Yen | Electron Microscopy Ch. 1 7

Electron Emission
• Uncertainty Principle & Tunneling (ΔpΔx ≈ ħ/2): The more precisely the position is
determined, the less precisely the momentum is known in this instant, and vice
versa.

• Werner Karl Heisenberg’s uncertainty paper (1927): Uncertainty in momentum


corresponds to the barrier height (φ, work function): (2mφ)1/2.

• If uncertainty in position: Δx ≈ ħ/2(2mφ)1/2 is approximately the barrier width w =


φ/fe (fe = applied field), then electrons will have a high probability of existing on
either side.

Homer Yen | Electron Microscopy Ch. 1 8


Electron Emission
• Fowler-Nordheim Equation:
.
B 𝜑 ∆𝜑
𝑗 A 𝜑 ∆𝜑 𝐸 exp
𝐸

A ~ 1.541 x 10-10 A/m2eV(V/m)-2


B ~ 6.831 x 109 (eV)-1.5V/m
• Field Emission is called Fowler-
Nordheim tunneling
• The total emission current is lower
than that of thermal emission.
BUT cold FEG has higher current
density than that Schottky FEG has.

Homer Yen | Electron Microscopy Ch. 1 9

Desired Electron Source


• Brightness
• Emission current (ie): current (A)
• Current density (j): current per unit area (A/m2)
• Brightness (B): current per unit area per unit solid angle (A/m2 sr)
𝛼
𝑖 4𝑖 𝑗
𝐵
𝜋 𝑑 ⁄2 𝜋 𝛼 𝜋𝑑 𝛼 𝜋 𝛼 d

• Optimized Brightness
• Decreasing gun cross-over (d0)
• Increasing emission current (ie)
• Decreasing divergence angle (α0)

10
Field Emission Gun (Schottky Emitter)
• Characteristics
• Gun cross-over (d0)
• Emission current (ie)
• Divergence angle (α0)

• Control parameters
• Filament current (usually fixed)
• Extraction voltage
• Acceleration voltage

11

Field Emission Gun (Schottky Emitter)

Source: [Link]

12
Characteristics of Electron Gun

13

Overall Configuration (TECNAI)

Homer Yen | Electron Microscopy Ch. 1 14


Convergent Illumination Parallel Illumination

Illumination
Illumination

16
15
Image Formation & Magnification
• Objective Lens
• Gaussian Plane: Morphology
• Back Focal Plane: Diffraction

• Intermediate Lens
• strong for image
• weak for diffraction

• Projection Lens
• magnification

Homer Yen | Electron Microscopy Ch. 1 17

Lens
• Electromagnetic Lens
• Focal Length: 𝑓 𝐾
• K = constant based on the number of turns of lens coil wire and the geometry of the lens.
• V = acceleration voltage
• i = milliamps of current put through the coil

Homer Yen | Electron Microscopy Ch. 1 18


Lens - Lens Equation

∆𝐼 ↔ ∆𝑓

1 1 1
𝑑 𝑑 𝑓

𝑑
𝑀
𝑑

19

Lens - Spiral Electron Path


• Electrons travel in spiral path

𝑟 =

• For electrons with higher keV, we must use


stronger lens (larger B) to get similar ray paths.

One will see this effect as he/she operates the TEM because
the image or DP rotates on the display screen as trying to
focus or if changing magnification.

20
Lens - Focus & Defocus

21

Lens - Focus & Defocus (Fresnel Fringes)

Focus (A) and defocus -4,748 nm (under) in (B )and + 4,031 (over) nm in C) low-
resolution TEM images of a partially ordered area for a bulk PCMO sample (x = 0.32)
at 90 K, acquired in a JEM-2100F with a magnetic field free focal lens.

Ref: Jooss et al. 10.1073/pnas.0702748104.

22
Aperture
• General aperture is applied for
• Reducing the β angle
• Shielding the off-axis electrons.

Pt or Mo

Homer Yen | Electron Microscopy Ch. 1 23

Aperture: C2 Aperture

Misalignment

24
Aperture: Objective & SAD Apertures
• Objective Aperture
• Back Focal Plane
• Choose diffraction for morphology
(image)

• Selective Area Diffraction (SAD)


Aperture
• Gaussian Plane
• Select area for diffraction

Homer Yen | Electron Microscopy Ch. 1 25

Objective Aperture
• Single beam for diffraction contrast image and Multiple beams for phase
contrast image.

26
SAD Aperture

Homer Yen | Electron Microscopy Ch. 1 27

Overall Configuration (TECNAI)

Homer Yen | Electron Microscopy Ch. 1 28


Deflector
• Deflectors control translation and tilting
of electron beam. It is the most frequently
used function in practical operation.
• Gun deflector
• Gun tilt: straight and symmetrical illumination
• Gun shift: axial illumination
• Beam deflector
• Beam tilt: alignment/dark field
• Beam shift: alignment/position beam
• Image deflector
• Image shift: movement of image of diffraction
pattern

29

Deflector in STEM Mode

30
Stigmatism

Example of C2 Lens

31

Overall Configuration (TECNAI)

Homer Yen | Electron Microscopy Ch. 1 32


Screen: Survey
• Screen is pasted with ZnS powder.
• The screen will decay under strong light or UV.
• You must notice to
• cover it when light on, and
• prevent from long exposure under diffraction mode.

33

Detection: Charge-Coupled Device


• CCDs are metal-insulator-silicon devices that store charge generated by light or
electron beams.

34
Resolution Limited by CCD Detector
• Rayleigh Limit: 𝑟 0.61λ/sin𝛼

• Nyquist Limit: 𝐿 0.30λ/sin𝛼


• Example
• CCD with pixel size of 10 x 10 μm2
• In 200 kV TEM, the point-to-point resolution is
~0.25nm
• Under the magnification of 20,000X, the point-to-
point distance is magnified into ~ 5 μm (< 10 μm).
• What is the solution?
• CCD with finer pixel size
• zoom to 100,000X

Homer Yen | Electron Microscopy Ch. 1 35

Check Point
• Instrument
• Overall Configuration
• Electron Source
• Illumination, Image Formation and Magnification
• Recording
• Quality of Electron Microscopy
• Coherence
• Aberration & Resolution Power
• Alignment and Focus
• Illumination Optimization (Alignment)
• Image Focus

Homer Yen | Electron Microscopy Ch. 1 36


Quality of Electron Microscopy

• The ability to achieve tiny spot with high brightness and high coherence.

• The ability to achieve extremely high resolution.

• The ability to interpret more and direct information.

37

Coherence
• Temporal incoherence results from the
energy spreading of the electron source:
∆𝜆

• Spatial incoherence results from the size of


the electron source. The effective size of
coherent illumination is defined as 𝑑

Homer Yen | Electron Microscopy Ch. 1 38


Coherence

Schottky FEG

LaB6

Cold FEG

Homer Yen | Electron Microscopy Ch. 1 39

Coherence: Cold FEG

Ref: Hitachi EM

40
Resolution
• Resolution of microscope is intuitively known to be its ability to see the details of
one object.

• Resolution is defined by the minimum distance between two points that are
distinguishable under the microscope.

• Magnification doesn’t improve resolution.

• Besides the diffraction limit, there are aberrations in electron microscopes due to
gun, lens, aperture, and misalignment.

41

Resolution: Chromatic Aberration


• This term is related to the ‘color’ (i.e., frequency,
wavelength, or energy) of the electrons.

• It results from
• The nature of gun
• The electron-specimen interaction

• The chromatic aberration is defined by

∆𝐸
𝛿 𝐶 𝛽
𝐸

Homer Yen | Electron Microscopy Ch. 1 42


Resolution: Spherical Aberration
• Electrons near the edge of the lens are bent
more than those near the center because the
magnetic field between the lens pole pieces is
not uniform.

• The spherical aberration is defined by:

𝛿 𝐶𝛽

• How can we move the image of least confusion


to the image plane? Answer: under-focus
(counter-clockwise)

Homer Yen | Electron Microscopy Ch. 1 43

Cs Corrector

Homer Yen | Electron Microscopy Ch. 1 44


Cs Corrector

Homer Yen | Electron Microscopy Ch. 1 45

Cs Corrector

Homer Yen | Electron Microscopy Ch. 1 46


Astigmatism
• Astigmatism occurs when the electrons
sense a non-uniform magnetic field as
they spiral round the optic axis:
• Imperfect design in lens system
• Defects of aperture

• These effects in general described by:


𝛿 ∆𝑓𝛽

• This can be corrected by stigmators.

Homer Yen | Electron Microscopy Ch. 1 47

Diffraction Limit
• All lens aberration quickly increase with β.
• In fact, β decreases with increasing
magnification from lens to lens.
• The largest angles β occur in the region of the
objective lens. Obj Lens Determine the quality of
the microscope!
• Choosing the smallest aperture improves
resolution. NO!!!
• There is diffraction limit:
0.61𝜆
𝛿 𝛿
𝛽

Homer Yen | Electron Microscopy Ch. 1 48


Resolution Power
• That is, aberration limits the resolution by:

𝛿 𝛿 𝛿 𝛿 𝛿

if chromatic aberration and astigmatism is neglected.

• Optimum aperture: 𝛽 ∗ ~0.77 𝜆/𝐶 /

/
• Optimum resolution: 𝛿 ∗ ~0.91𝐶 𝜆 /
. This is called “Resolution Power”.

49

Check Point
• Instrument
• Overall Configuration
• Electron Source
• Illumination, Image Formation and Magnification
• Recording
• Quality of Electron Microscopy
• Coherence
• Aberration & Resolution Power
• Alignment and Focus
• Illumination Optimization (Alignment)
• Image Focus

Homer Yen | Electron Microscopy Ch. 1 50


Overall: Top-Down and Top-Down

Homer Yen | Electron Microscopy Ch. 1 51

Homer’s Note
• The e-beam is less defective when the lens is strongly activated (short focus).
• Illumination
• High Brightness
• Parallel/Convergent, Centralized and Concentric Beam/Probe
• Well Controllable Rays
• Image/Diffraction
• Clear Image and Diffraction Pattern
• Accurate Size
• Correct Morphology
• Interpretation (Ch4 – Ch6)

Homer Yen | Electron Microscopy Ch. 1 52


Gun Alignment
• Confirm that the electron beam enters the microscope (that is, the C1 lens)
parallel to the optical axis by means of the gun tilt and that the beam goes
through the center of the C1 lens by means of the gun shift.
• Gun Tilt
• symmetrical filament image
• highest brightness (shortest exposure
time)
• Gun Shift
• No shifting when changing the strength
of C1 lens.
• Tecnai F20: spot size 3 & 9
Tecnai F30: spot size 2 & 7

53

Gun Tilt: Filament Image

Not aligned Aligned Aligned


(FEG)

Homer Yen | Electron Microscopy Ch. 1 54


Gun Shift Alignment

C1 Lens & C1 Aperture


• C1 lens de-magnifies the source
crossover into a smaller electron
source (~x10): Spot Size.

• C1 aperture is usually fixed to maintain


the instrument stability.

• In TEM, increasing the # of spot size


will reduce the crossover.

• In SEM, increasing the # of spot size


will enlarge the crossover.

Homer Yen | Electron Microscopy Ch. 1 56


Spot Size in SEM
• C1 lens in SEM is designed by electrostatic lens,
which has a weaker strength in focus.

• The crossover of C1 lens exactly locates at the


entrance of Obj/C2 aperture, when Spot Size # is
7(max).

• There are Spot Size # 1, 2…and 7. Spot size 7 gives


the highest current.

• Spot Size # ↑, strongly activated, and then large


spot size.

Homer Yen | Electron Microscopy Ch. 1 57

C2 Lens & C2 Aperture


• C2 creates a parallel illumination onto the
specimen in TEM, or a convergent illumination in
SEM/STEM: Condenser
• Question: How can we confirm that the parallel
illumination has bee

Homer Yen | Electron Microscopy Ch. 1 58


Illumination
Parallel Illumination Convergent Illumination

59

Illumination (C3 Lens)


• Without a c/o lens, underfocus
gives a more parallel beam at the C2
plane of the specimen than
overfocus.

• The convergent effect of the c/o


lens can be offset by forming a C/O or C3
strong
crossover at the FFP of the
objective lens. FFP
Mini lens
or
Upper Obj
• The parallel beam condition is
met in the overfocus condition in
the c/o lens.
Homer Yen | Electron Microscopy Ch. 1 60
Illumination (C3 Lens)

Homer Yen | Electron Microscopy Ch. 1 61

C2 Aperture & Stigmator


• Adjust C2 stigmator to obtain a circular beam.

• Centralized the C2 aperture to prevent from non-concentric focus when changing


C2 strength.

62
C2 Aperture Alignment

Beam Deflector Coils


• Beam deflector
• Beam tilt: alignment/dark field
• Beam shift: alignment/position beam

• Alignment: Pivot Point


• No tilting in diff mode when shifting
• No shifting in image mode when tilting

• Pivot point of beam deflector are available for


general users. Pivot point of gun deflector are
available only for TEM managers.

Homer Yen | Electron Microscopy Ch. 1 64


Parallel and Centralized Illumination
• Check whether the beam is along the optical
axis of the objective lens by Rotation
Center/Current Center/HV wobbler.

• When the beam is inclined, one see image


movement when Rotation Center is on.

• Using beam tilt to minimize the movement of


the image.

Homer Yen | Electron Microscopy Ch. 1 65

Parallel and Centralized Illumination


• Comma free

tilted Non-tilted

66
Homer’s Note
• The e-beam is less defective when the lens is strongly activated (short focus).
• Illumination
• High Brightness
• Parallel/Convergent, Centralized and Concentric Beam/Probe
• Well Controllable Rays
• Image/Diffraction
• Clear Image and Diffraction Pattern
• Accurate Size
• Correct Morphology
• Interpretation (Ch4 – Ch6)

Homer Yen | Electron Microscopy Ch. 1 67

Image Focus
• Objective Lens
• Gaussian Plane: Morphology
• Back Focal Plane: Diffraction

• Intermediate Lens
• strong for image
• weak for diffraction

• Projection Lens
• magnification

Homer Yen | Electron Microscopy Ch. 1 68


Image Focus

Image Focus: Fresnel Fringes

Bright Edge Dark Edge

Image shows minimum contrast when just focused.

Ref: Portland University


Astigmatism: Fresnel Fringes

Under-Focus Focus Over-Focus


With Astigmatism
W/O Astigmatism

Ref: [Link]

Astigmatism: Image Quality


Under-Focus Focus Over-Focus
With Astigmatism
W/O Astigmatism

Ref: [Link]
Astigmatism: Image Transfer Function

Under-Focus Focus Over-Focus


With Astigmatism
W/O Astigmatism

Image Focus & Specimen Position

d0 x, f ↓, di ↓ d0 ↑, f x, di ↓ d0 ↑, f ↑, di x
1 1 1
𝑑 𝑑 𝑓 Pattern is not well focused.
Eucentric Height

Diffraction Focus
• What if the diffraction pattern is not
well focused into a point?
• Check eucentric height and sample
position
• Check intermediate lens (insert obj
aperture)
• Check beam parallelism

Homer Yen | Electron Microscopy Ch. 1 76


Depth of Field & Depth of Focus
• The depth of field is defined as the range of object distances that are imaged in
focus.

- Why it is possible to image the entire thickness of a TEM sample.

• The depth of focus is the range of distances over which the image appears in
focus in the image plane of a lens.

- Why the same lens settings provide a crisp image on the viewing screen, CCD
camera, which may be separated by several centimeters.

77

Depth of Field & Depth of Focus

Limitation of
our eyes/detector

78
Depth of Focus in SEM
• Larger depth of focus increases the ability to focus objects from different depths.
• How to increase the depth of focus in SEM?

79

Any Question?
(homeryen@[Link])

Homer Yen | Electron Microscopy Ch. 1 80

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