Optical & Electron Microscopy

Tech. of Microstructural Analysis

Wahyuaji NP
 Optical Microscopy

• Introduction
• Lens formula, Image formation and
Magnification
• Resolution and lens defects
• Basic components and their functions
• Common modes of analysis
• Specialized Microscopy Techniques
• Typical examples of applications
 Diffraction of Light
Diffraction of light occurs when a
light wave passes by a corner
(or a barrier) or through an
opening (or a slit) that is
physically the approximate size
of, or even smaller than that
light's wavelength.

Sin=/d
/d

1st 2nd 3rd

film
 Resolution of a Microscope (lateral)
The smallest distance between two specimen points
that can still be distinguished as two separate entities

dmin = 0.61/NA NA=nsin()

 – illumination wavelength (light)

NA – numerical aperture
-one half of the objective angular aperture
n-imaging medium refractive index

dmin ~ 0.3m for a midspectrum  of 0.55m

 Wavelength vs
Resolution

Wavelength of the visible light

Smaller
wavelength able to
separate two small
dots
 Axial resolution – Depth of Field
Depth of focus (F mm) Depth of Field Ranges
(F (F
m)m)

NA F F
0.1 0.13 55.5
0.4 3.8 5.8
.95 80.0 0.19

The distance above and below The axial range through which
geometric image plane within an object can be focused without
which the image is in focus any appreciable change in image
sharpness
M NA F F
F is determined by NA.
M NA F F
Basic components and their functions
 Old and Modern
Light Microscopes
Anatomy of a modern LM

Illumination System
 Functions of the Major Parts of a
Optical Microscope
 Lamp and Condenser: project a parallel
beam of light onto the sample for illumination
 Sample stage with X-Y movement: sample is
placed on the stage and different part of the
sample can be viewed due to the X-Y
movement capability
 Focusing knobs: since the distance between
objective and eyepiece is fixed, focusing is
achieved by moving the sample relative to the
objective lens
Light Sources
 Condenser

Light from the microscope light source

Condenser gathers light and concentrates it into a
cone of light that illuminates the specimen with
uniform intensity over the entire viewfield
 Condenser-2
(NA)

NA: 1.2 0.6 0.3 0.15

It is critical that the condenser aperture be properly adjusted to

optimize the quality of light entering the objective front lens.
Specimen Stage
 Functions of the Major Parts of a
Optical Microscope
 Objective: does the main part of
magnification and resolves the fine
details on the samples (mo ~ 10 – 100)
 Eyepiece: forms a further magnified
virtual image which can be observed
directly with eyes (me ~ 10)
 Beam splitter and camera: allow a
permanent record of the real image
from the objective be made on film
 Microscope Objectives
dmin = 0.61/NA
Objective specifications Anatomy of an objective

rical
ture

Objectives are the most important components of a

light microscope: image formation, magnification, the
quality of images and the resolution of the microscope
 Eyepiece

(Diaphragm)

M=(L/fo)(25/fe)
Eyepieces (Oculars) work in combination with microscope
objectives to further magnify the intermediate image
camera

Beam Olympus
splitter
BX51
Research
Microscope
Cutaway
Diagram
 Common Modes of Analysis
Depending on the nature of samples, different illumination
methods must be used
• Transmitted OM - transparent specimens
thin section of rocks, minerals and single crystals
• Reflected OM - opaque specimens
most metals, ceramics, semiconductors
Specialized Microscopy Techniques
• Polarized OM - specimens with anisotropic optical
character
Characteristics of materials can be determined
morphology (shape and size), phase distribution
(amorphous or crystalline), transparency or opacity,
color, refractive indices, dispersion of refractive
indices, crystal system, birefringence, degree of
crystallinity, polymorphism and etc.
Anatomy of a modern LM

Illumination System
 Polarization of Light

When the electric field vectors of light are restricted to a

single plane by filtration, then the the light is said to be
polarized with respect to the direction of propagation and
all waves vibrate in the same plane.
Polarized Light Microscope Configuration
Typical examples of
applications
 1200C/30min
Grain Size Examination
Thermal Etching

a
1200C/2h

b 20m

A grain boundary intersecting a polished surface is not in

equilibrium (a). At elevated temperatures (b), surface
diffusion forms a grain-boundary groove in order to
balance the surface tension forces.
 Grain Growth - Reflected OM

5m 30m

Polycrystalline CaF2 Large grains in polycrystalline

illustrating normal grain spinel (MgAl2O4) growing by
growth. Better grain size secondary recrystallization
distribution. from a fine-grained matrix
Liquid Phase Sintering – Reflective OM

Amorphous
phase

40m

Microstructure of MgO-2% kaolin body resulting

from reactive-liquid phase sintering.
 Polarized Optical Microscopy (POM)

Reflected POM Transmitted POM

(a)Surface features of a microprocessor integrated circuit

(b)Apollo 14 Moon rock
 Phase Identification by Reflected
Polarized Optical Microscopy

YBa2Cu307-x superconductor material: (a) tetragonal phase and

(b) orthorhombic phase with multiple twinning (arrowed) (100 x).
 Specialized LM Techniques
• Enhancement of Contrast
Darkfield Microscopy
Phase contrast microscopy
Differential interference contrast microscopy
Fluorescence microscopy-mainly organic materials
• Confocal scanning optical microscopy (new)
Three-Dimensional Optical Microscopy
inspect and measure submicrometer features in
semiconductors and other materials
• Hot- and cold-stage microscopy
melting, freezing points and eutectics, polymorphs, twin
and domain dynamics, phase diagram
• In situ microscopy
E-field, stress, etc.
• Special environmental stages-vacuum or gases
 Contrast
Contrast is defined as the difference in light intensity
between the specimen and the adjacent background
relative to the overall background intensity.

Image contrast, C is defined by

Sspecimen-Sbackgroud S
C= =
Sspecimen SA

Sspecimen and Sbackgroud are

intensities measured from
specimen and backgroud, e.g., A
and B, in the scanned area.
 Angle of Illumination
 Bright filed illumination – The normal method of illumination,
light comes from above (for reflected OM)
 Oblique illumination – light is not projected along the optical
axis of the objective lens; better contrast for detail features
 Dark field illumination – The light is projected onto specimen
surface through a special mirror block and attachment in the
objective – the most effective way to improve contrast.

Light stop

Imax-Imin
Imax C=
Imin Imax

C-contrast
Reflected Darkfield Illumination
 Contrast Enhancement

OM images of the green alga Micrasterias

Crystals Growth-Interference
contrast microscopy

Growth spiral on
cadmium iodide
crystals growing
From water
solution (1025x).
Confocal Scanning Optical Microscopy
Three-Dimensional Optical Microscopy
Critical dimension measurements
in semiconductor metrology
w
Cross-sectional image with line scan
at PR/Si interface of a sample
containing 0.6m-wide lines and
1.0m-thick photoresist on silicon.

The bottom width, w, determining

the area of the circuit that is
protected from further processing,
can be measured accurately by
using CSOP.

Measurement of the patterned

photoresist is important because it
allows the process engineer to
simultaneously monitor for defects,
misalignment, or other artifacts that
may affect the manufacturing line.
Hot-stage POM of Phase Transformations
in Pb(Mg1/3Nb2/3)O3-PbTiO3 Crystals

(a) and (b) at 20oC, strongly

birefringent domains with extinction
n directions along <100>cub,
indicating a tetragonal symmetry;
(c) at 240oC, phase transition from
the tetragonal into cubic phase with
increasing isotropic areas at the
T(oC) expense of vanishing strip domains.
 E-field Induced Phase Transition in
Pb(Zn1/3Nb2/3)O3-PbTiO3 Crystals

a b c
Single domain

Schematic diagram for Domain structures of PZN-PT

in situ domain observa- crystals as a function of E-field;
tions. (a)E=20kV/cm, (b) e=23.5kV/cm
(c) E=27kV/cm
Rhombohedral at E=0 and
Tetragonal was induced at E>20kV/cm
 Limits of Optical Microscopy
• Small depth of field <15.5m
Rough surface
• Low resolution ~0.2m
• Shape of specimen
Thin section or polished surface
Cover glass
specimen
Glass slide
resin

20m

• Lack of compositional and

crystallographic information
 Optical Microscopy vs Scanning
Electron Microscopy

25m
radiolarian
OM SEM
Small depth of field Large depth of field
Low resolution High resolution
Scanning Electron Microscopy (SEM)
•What is SEM?
•Working principles of SEM
•Major components and their functions
•Electron beam - specimen interactions
•Interaction volume and escape volume
•Magnification, resolution, depth of field and
image contrast
•Energy Dispersive X-ray Spectroscopy (EDS)
•Wavelength Dispersive X-ray Spectroscopy
(WDS)
•Orientation Imaging Microscopy (OIM)
•X-ray Fluorescence (XRF)
 What is SEM

The SEM is
designed for
direct studying
of the surfaces
of solid objects

Cost: $0.8-2.4M

Scanning electron microscope (SEM) is a microscope that

uses electrons rather than light to form an image. There
are many advantages to using the SEM instead of a OM.
 Advantages of Using SEM over OM
Magnification Depth of Field Resolution
OM 4x – 1000x 15.5m – 0.19m ~ 0.2m
SEM 10x – 3000000x 4mm – 0.4m 1-10nm

The SEM has a large depth of field, which allows a large

amount of the sample to be in focus at one time and
produces an image that is a good representation of the
three-dimensional sample. The SEM also produces
images of high resolution, which means that closely
features can be examined at a high magnification.

The combination of higher magnification, larger depth of

field, greater resolution and compositional and
crystallographic information makes the SEM one of the
most heavily used instruments in research areas and
industries, especially in semiconductor industry.
 Scanning Electron Microscope
– a Totally Different Imaging Concept

• Instead of using the full-field image, a point-to-

point measurement strategy is used.
• High energy electron beam is used to excite
the specimen and the signals are collected and
analyzed so that an image can be constructed.
• The signals carry topological, chemical and
crystallographic information, respectively, of the
samples surface.
 Main Applications
• Topography
The surface features of an object and its texture
(hardness, reflectivity… etc.)
• Morphology
The shape and size of the particles making up the
object (strength, defects in IC and chips...etc.)
• Composition
The elements and compounds that the object is
composed of and the relative amounts of them
(melting point, reactivity, hardness...etc.)
• Crystallographic Information
How the grains are arranged in the object
(conductivity, electrical properties, strength...etc.)
A Look Inside the Column
Column
 Electron Gun

A More e- beam

Detaile
d Look 
Inside

Source: L. Reimer,
“Scanning Electron
Microscope”, 2nd Ed.,
Springer-Verlag, 1998, p.2
 Image Formation in SEM

M = c/x
A 10cm
e-
beam
Detector

10cm
Amplifier

A c-length of CRT scan

x-length of e- beam scan
Beam is scanned over specimen in a raster pattern in
synchronization with beam in CRT. Intensity at A on CRT
is proportional to signal detected from A on specimen and
signal is modulated by amplifier.
 Image Magnification

Example of a series of increasing magnification (spherical lead

particles imaged in SE mode)
 Comparison of OM,TEM and SEM
Source of
Light source electrons
Condenser
Magnetic
lenses
Specimen
Objective

Specimen
Eyepiece
Projector CRT
Cathode
Ray Tube

detector

OM TEM SEM

Principal features of an optical microscope, a transmission

electron microscope and a scanning electron microscope,
drawn to emphasize the similarities of overall design.
How an Electron Beam is Produced?

• Electron guns are used to produce a

fine, controlled beam of electrons
which are then focused at the
specimen surface.
• The electron guns may either be
thermionic gun or field-emission gun
 Electron beam Source

W or LaB6 Filament
Thermionic or Field Emission Gun
Thermionic Emission Gun
• A tungsten filament
heated by DC to
approximately 2700K or
LaB6 rod heated to around
2000K
• A vacuum of 10-3 Pa (10-4
Pa for LaB6) is needed to
prevent oxidation of the
filament
• Electrons “boil off” from
the tip of the filament
• Electrons are accelerated
by an acceleration voltage
of 1-50kV
 Field Emission Gun
• The tip of a tungsten needle is
made very sharp (radius < 0.1
m)
• The electric field at the tip is
very strong (> 107 V/cm) due
to the sharp point effect
• Electrons are pulled out from
the tip by the strong electric
field
• Ultra-high vacuum (better than
10-6 Pa) is needed to avoid ion
bombardment to the tip from
the residual gas.
• Electron probe diameter < 1
nm is possible
 Source of Electrons
Thermionic Gun E: >10MV/cm
T: ~1500oC
W

Filament
(5-50m)

(5nm)

W and LaB6 Cold- and thermal FEG

Electron Gun Properties

Source Brightness Stability(%) Size Energy spread Vacuum
W 3X105 ~1 50m 3.0(eV) 10-5 (t )
LaB6 3x106 ~2 5m 1.5 10-6
C-FEG 109 ~5 5nm 0.3 10-10
T-FEG 109 <1 20nm 0.7 10-9
 Magnetic Lenses
• Condenser lens – focusing
determines the beam current
which impinges on the sample.
• Objective lens – final probe
forming
determines the final spot size of
the electron beam, i.e., the
resolution of a SEM.
 Why Need a Vacuum?
When a SEM is used, the electron-optical
column and sample chamber must always
be at a vacuum.

1. If the column is in a gas filled environment,

electrons will be scattered by gas molecules which
would lead to reduction of the beam intensity and
stability.

2. Other gas molecules, which could come from the

sample or the microscope itself, could form
compounds and condense on the sample. This
would lower the contrast and obscure detail in the
image.
 The Condenser Lens
• For a thermionic gun, the diameter of
the first cross-over point ~20-50µm
• If we want to focus the beam to a size
< 10 nm on the specimen surface, the
magnification should be ~1/5000, which
is not easily attained with one lens
(say, the objective lens) only.
• Therefore, condenser lenses are added
to demagnify the cross-over points.
 How Is Electron Beam Focused?
A magnetic lens is a solenoid designed to produce
a specific magnetic flux distribution.
Magnetic lens
(Beam diameter) (solenoid)

F = -e(v x B) p

q
Lens formula: 1/f = 1/p + 1/q

Demagnification: M = q/p

f  Bo2
f can be adjusted by changing Bo, i.e., changing the
current through coil.
The Condenser
Lens

Demagnification:
M = f/L
 The Objective Lens
• The objective lens
controls the final
focus of the electron
beam by changing the
magnetic field strength
• The cross-over image
is finally demagnified
to an ~10nm beam
spot which carries a
beam current of
approximately 10-9-10-
10-12 A.
 The Objective Lens - Focusing
• By changing the Objective
current in the lens

objective lens,
the magnetic field
strength changes
and therefore the
focal length of
the objective lens
is changed.
Out of focus in focus out of focus
lens current lens current lens current
too strong optimized too weak
 The Objective Lens - Stigmator

• The objective lens is machined to very

high precision and the magnetic field
pattern is very carefully designed.
• However, the precision attainable by
machining cannot match that required
for controlling a beam with Ø10 nm
• The stigmator, which consist of two
pairs of pole-pieces arranged in the X
and Y directions, is added to correct the
minor imperfections in the objective
lens.
 The Objective Lens – The Aperture
• Since the electrons Electron beam
coming from the
electron gun have Objective
spread in kinetic lens
energies and directions
Wide Narrow
of movement, they may aperture aperture
not be focused to the
same plane to form a
sharp spot. Narrow disc
Wide disc of of least
• By inserting an aperture, least confusion confusion
the stray electrons are
Large beam diameter Small beam diameter
blocked and the striking specimen striking specimen
remaining narrow beam
will come to a narrow
“Disc of Least Confusion”
 The Scan Coil and Raster Pattern
• Two sets of coils are
used for scanning X-direction
scanning coil
the electron beam
across the specimen Holizontal line scan
Blanking
surface in a raster
pattern similar to
that on a TV screen.y-direction
• This effectively scanning
coil
samples the
specimen surface
point by point over
Objective
the scanned area. lens
specimen
Electron Detectors and Sample Stage

Objective
lens
Sample stage
Scanning Electron Microscopy (SEM)
•What is SEM?
•Working principles of SEM
•Major components and their functions
•Electron beam - specimen interactions
•Interaction volume and escape volume
•Magnification, resolution, depth of field and
image contrast
•Energy Dispersive X-ray Spectroscopy (EDS)
•Wavelength Dispersive X-ray Spectroscopy
(WDS)
•Orientation Imaging Microscopy (OIM)
•X-ray Fluorescence (XRF)
Electron Beam and Specimen Interactions
Sources of Image Information
Electron/Specimen Interactions

(1-50KeV)

Electron Beam Induced Current (EBIC)

 Secondary Electrons (SE)
Produced by inelastic interactions
of high energy electrons with
Primary
valence (or conduction) electrons of
atoms in the specimen, causing the
ejection of the electrons from the
atoms. These ejected electrons with
energy less than 50eV are termed
"secondary electrons".
Each incident electron can produce
several secondary electrons.
SE yield: d=nSE/nB independent of Z BaTiO3
d decreases with increasing beam
energy and increases with decreasing
glancing angle of incident beam
Production of SE is very topography Growthstep
related. Due to their low energy, only SE
that are very near the surface (<10nm)
can exit the sample and be examined 5m
SE image
(small escape depth).
 Topographical Contrast
Everhart-Thornley
SE Detector

Bright lens polepiece

e-
SE Scintillator
light pipe PMT
Dark
sample Quartz
Faraday window
cage +200V +10kV
Photomultiplier
tube

Topographic contrast arises because SE generation

depend on the angle of incidence between the beam
and sample.
 Backscattered Electrons (BSE)
Primary

BSE image from flat surface of an

Al (Z=13) and Cu (Z=29) alloy
BSE are produced by elastic interactions of beam electrons
with nuclei of atoms in the specimen and they have high
energy and large escape depth.
BSE yield: h=nBS/nB ~ function of atomic number, Z
BSE images show characteristics of atomic number
contrast, i.e., high average Z appear brighter than those of
low average Z. h increases with tilt.
Schematic Electron Spectrum of
Emitted Electrons

0 50eV 2keV E=eV

Electron energy

ESE  50eV and EBSE > 50eV

Effect of Atomic Number, Z, on
BSE and SE Yield
Electron Excitation of Continuum Processes
KE=eV=½(mv2)

Decelerated in Coulombic field

of atom, loss energy, converted
into X-ray photons
 Principles of X-ray Production
(20keV) X-ray are
produced
L Create a vacancy by transitions
K in K shell of electrons
between shells
of atoms

Shells
correspond to
particular
K energy level
for an atom
L
e- in L shell jumps Transition
in to fill vacancy between shells
and energy
K levels are
characteristic
Auger electron
emission of element
L
Process of inner-shell ionization and subsequent deexcitation
 Excitation of K, L, M and N shells and
Formation of K to M Characteristic X-rays
M
 If an incoming electron has K L
sufficient kinetic energy for K2
K1
knocking out an electron of the K
K shell (the inner-most shell),
I
it may excite the atom to an K L II
high-energy state (K state). L III
M
N subshells
 One of the outer electron falls
into the K-shell vacancy, Energy K state
(shell)
emitting the excess energy as K
a x-ray photon. K
 Characteristic x-ray energy: L state
K excitation
Ex-ray=Efinal-Einitial L
M state
EK>EL>EM L excitation M
EK>EK N state
4/10/2018
ground state
Characteristic X-ray Spectrum
Illustrating KLM Lines
Note:
•As Z increases the
Kth shell line energy
increases.
•If K-shell is excited,
then all shells are
excited (Y, Cu, Ba)
but they may not
be detected.
•Severe spectral
overlap may occur
for low energy lines.
 Interaction Volume: I
e-

Monte Carlo simulations of 100 electron trajectories

The incident electrons do not go along a

straight line in the specimen, but a zig-zag
path instead.
 Interaction Volume: II

The penetration or,

more precisely, the
interaction volume
depends on the
acceleration voltage
(energy of electron)
and the atomic
number of the
specimen.
Escape Volume of Various Signals
• The incident electrons interact with specimen
atoms along their path in the specimen and
generate various signals.
• Owing to the difference in energy of these
signals, their ‘penetration depths’ are
different
• Therefore different signal observable on the
specimen surface comes from different parts
of the interaction volume
• The volume responsible for the respective
signal is called the escape volume of that
signal.
 Escape Volumes of Various Signals

If the diameter of primary

electron beam is ~5nm
- Dimensions of escape
zone of
•Secondary electron:
diameter~10nm; depth~10nm
•Backscattered electron:
diameter~1m; depth~1m
•X-ray: from the whole
interaction volume, i.e., ~5m
in diameter and depth
 Electron Interaction Volume

Pear shape

5m

a b

a.Schematic illustration of electron beam interaction in Ni

b.Electron interaction volume in polymethylmethacrylate
(plastic-a low Z matrix) is indirectly revealed by etching
 Image Formation in SEM
M= C/x
A 10cm
e-
beam
Detector

10cm
Amplifier

Beam is scanned over specimen in a raster pattern in

synchronization with beam in CRT.
Intensity at A on CRT is proportional to signal detected
from A on specimen and signal is modulated by amplifier.
 Magnification
e-

x Low M High M
Large x small x
40m 7m

1.2m 15000x
2500x

The magnification is simply the ratio of the length of the

scan C on the Cathode Ray Tube (CRT) to the length of
the scan x on the specimen. For a CRT screen that is 10
cm square:
M= C/x = 10cm/x
Increasing M is achieved by decreasing x.
M x M x
100 1 mm 10000 10 m
1000 100 m 100000 1 m
 How Fine Can We See with SEM?

• If we can scan an area with width 10 nm

(10,000,000×) we may actually see
atoms!! But, can we?
• Image on the CRT consists of spots
called pixels (e.g. your PC screen
displays 1024×768 pixels of ~0.25mm
pitch) which are the basic units in the
image.
• You cannot have details finer than
one pixel!
 Depth of Focus

Depth of Field

4x105W
D= (m)
AM

To increase D
Decrease aperture size, A
Decrease magnification, M
Increase working distance, W (mm)
 SE Images
Image Contrast
Image contrast, C
is defined by

SA-SB S
________
C= = ____
SA SA

SA, SB Represent
signals generated
from two points,
e.g., A and B, in the
scanned area.

In order to detect objects of small size and low contrast

in an SEM it is necessary to use a high beam current and
a slow scan speed (i.e., improve signal to noise ratio).
SE-topographic and BSE-atomic number contrast
 SE Images - Topographic Contrast

1m

Defect in a semiconductor device Molybdenum

The debris shown here is an oxide trioxide crystals
fiber got stuck at a semiconductor
device detected by SEM
BSE Image – Atomic Number Contrast

2m

BSE atomic number contrast image showing a

niobium-rich intermetallic phase (bright contrast)
dispersed in an alumina matrix (dark contrast).

Z (Nb) = 41, Z (Al) = 13 and Z(O) = 8

Alumina-Al2O3