SCHEME FOR PROMOTION OF ACADEMIC AND

RESEARCH COLLABORATION

Thin Film Characterization

Dr. Yogesh Kumar Srivastava

Assistant Professor, Department of Physics,
Ultrafast Terahertz Photonics Laboratory (UTPL)
Indian Institute of Technology, Hyderabad
Email: [Link]@[Link] 1
 Outline
❖ Introduction of Thin Films

❖ Thin Film Characterization Techniques

❖ Thickness Measurements
-- Vibrating Quartz Crystal
-- Thickness Profilometer
-- Optical Methods

❖ Optical Constant Measurements

-- Terahertz Time Domain Spectroscopy

❖ Electron Microscopy
2
 What are the Thin Films?

Bulk Materials Fixed Properties Limited Applications

When thickness is reduced beyond certain limit, the properties change dramatically Size Effects

Bulk Materials

Stand Alone Thin films

❖ In Nanotechnology terms, at least one dimension confined to nano dimensions

❖ Thin films can be compared with the infinite potential square well due to particles confinement along a single
axis.
3
 Thin Films?
❖ Thin films are material deposited on thick substrate (Thickness ~ from fraction to nanometers to micrometers).

4
 Applications?

Optical: Reflective and anti-reflective coatings, Magnetic: Memory disks Electronic: Insulators, conductors, semi conductor
Solar cells, Wave guides and optical detector arrays devices, Integrated circuits and piezoelectric device

Chemical: Resistance to alloying,

Mechanical: Topological coating to protect against Thermal: Insulation layers and heat sinks.
diffusion, corrosion and oxidation, abrasion, increase hardness and adhesion and use of 5
also to make gas and liquid devices micro-mechanical properties
 Properties?
Electrical Properties : Film material + Substrate
(metal, semiconductor, or insulator)
✓ Size effect
✓ Shorter mean free path
✓ Scattering points (Defects and grain boundaries)

Optical Properties: Transmission, Reflection and Absorption

✓ Optical coefficients (refractive index (n) and extinction coefficient (k)).
✓ Electrical conductivity
✓ Depends on film roughness and thickness

Mechanical Properties: Different behavior as compared to their bulk form

✓ Dependence on film’s thickness and microstructure
✓ Microstructures like grain boundaries, dopants, and dislocations in the thin films results in larger hardness
compared to their bulk counterparts
✓ Strength and hardness

Thickness: Most Important Factor

6
Characterization Techniques

7
 IN-SITU AND EX-SITU MEASUREMENTS
Measurements is Important as deposition process.

In -Situ : Measurements during the deposition process.

Ex-Situ: Measurements after unloading the sample

Thin film Characterisation: Depending on the properties under investigation, the

measurements could be categorized as follows

➢ Thickness measurements

➢ Optical constant measurements

➢ Electrical conductivity measurements

➢ Thin film surface and structural characterisation

 Classification of Investigation Techniques?

In-Situ Ex-situ

(a) QCM (Quartz Crystal Microbalance) (a) Stylus Profilometer (Mechanical)

(b) RHEED(Reflective High Energy Electron (b) Ellipsometry ( Optical)
Diffraction)
(c) Interferometry ( Optical)
(d) THz-TDS (Optical)
(e) TEM( Electronic Microscopy)
(f) SEM ( Electronic Microscopy)
(g) STM( Scanning Probe Microscopy)
(h) AFM ( Scanning Probe Microscopy)
(i) XRD( Structural characterization)
9
(j) Neutron Diffraction( Structural characterization)
 Thickness Measurement
✓ Vibrating Piezoelectric Crystals
✓ Stylus Profilometer
✓ Optical Methods

10
 Quartz Crystal Microbalance

𝑽𝒊𝒃𝒓𝒂𝒕𝒊𝒏𝒈 𝑸𝒖𝒂𝒓𝒕𝒛 𝑪𝒓𝒚𝒔𝒕𝒂𝒍: 𝑮𝒓𝒂𝒗𝒊𝒎𝒆𝒕𝒓𝒊𝒄 𝑻𝒆𝒄𝒉𝒏𝒊𝒒𝒖𝒆 Involves Piezoelectric Oscillators

❖ Works based on the change in frequency with the
change in mass

❖ Resonant frequency depends on elastic modulus,

dimensions and density

❖ Additional mass alters the frequency of oscillation

(basically reduces) – f – change on frequency
❖ (Sauerbrey equation)

𝟐𝒇𝟐𝒐 ∆𝒎
∆𝒇 = −
𝑨 𝝆𝒒 𝝁𝒒
Need to use tooling factor as the amount of 𝑓0 = Resonance Frequency of Quartz crystal
deposition not same on quartz and the substrate. A- Piezoelectrically active crystal area,
Δm-change in mass due to deposition,
ρq- density of the Quartz Crystal
11
𝜇𝑞 = Sheer Modulus of Quartz
 Quartz Crystal Microbalance

𝜌𝑞 𝜇𝑞
Z - Factor =
𝜌𝑓 𝜇𝑓
∆𝒎
∆𝒅 =
𝝆𝒇
∆𝒅 - Change in thickness – film thickness

Quartz is used as microbalance since it has very good quality factor of f/f = 106
(very low noise)

For 1 MHz frequency of oscillation, 1 Hz change can be detected

12
 Advantages and Disadvantages

Advantages
• Very good for vacuum evaporation technique
• Rapid measurement with high resolution of about 0.05 nm thickness (change in mass – 10
nanograms)
• Can control the deposition rate – (in-situ)
• Not so expensive, Non Destructive Method
Disadvantages

• Not ideal for angular deposition such as sputtering deposition and PLD
• May need to be water cooled otherwise the heating form the source can change the precession
• Need to clean or replace periodically (if it is coated heavily)

13
Stylus Thickness Profilometer

14
 Stylus Profilometer

Physical Step + Sensitive Probe • Mechanical (contact) profiler.

• Easy to use

• Diamond/sapphire tip of a few micron radius.

• Apply a small force < 10-4 N.

• Feedback loop to construct the surface.

• Lateral resolution may not be accurate due to the large

radius of the tip.

• Sometimes can create scratches on certain surface

Ideal Reality 15
 Stylus Profilometer
YBCO Film on Sapphire Substrate

Depending on the expected thickness height of the step, the following methods could be used
1) Stylus Profilometer
2) Atomic Force Microscopy
3) Scanning Electron Microscopy
4) Focused Ion Beam

16
Optical Methods

17
Optical Microscopy

We can look at the the surface of the thin film but cannot specify any details or
structural information due to diffraction limit.

18
ELLIPSOMETORY ( Brief history)

Film thickness measured 0.3 A 19

 WHAT IS ELLIPSOMETRY

A Method of probing surface with light.

➢ Ellipsometry is a method based on the measurement of the change of the polarisation state of light
after reflection at non-Normal incidence on the surface to study.

▪ Very sensitive

▪ Highly accurate & Reproducible

Why
ellipsometry? ▪ Non- Destructive

▪ Easy and quick measurement

▪ No reference material

20
 MEASUREMENTS THROUGH ELLIPSOMETORY

What ellipsometry measures: What we are interested in:

➢ Film Thickness
➢ Refractive Index
Psi (Ψ) ➢ Extension Coefficient
Delta (∆) ➢ Surface Roughness
➢ Anisotropy
Desired information must
➢ Composition
be extracted through a
model based analysis using ➢ Uniformity
an equation to describe the
interaction of light and
material.
21
PRINCIPLE (POLARISATION OF LIGHT)

The polarization-change is
represented as an amplitude
ratio, Ф, and a phase
difference, Δ. The measured
response is dependent on
optical properties and
thickness of each material.

Fig: Schematic of Polarisation Process

22
 EXPERIMENTAL SETUP

Light source Detector

Ellipsometry measures the complex reflectance

ratio:
Polarizer Analyzer
𝒓𝒑
Compensator ф Compensator Ρ= = tanΨexp(i∆)
(optional) (optional) 𝒓𝒔

Sample

23
 ADVANTAGES AND DISADVANTAGES

ADVANTAGE DISADVANTAGE

Non-Destructive:it does not alter or damage the sample Complexity: Ellipsometry measurements involve complex
during measurement optical principles and data analysis techniques

High Sensitivity:It can detect small variations in thickness, Limited Depth Sensitivity: Ellipsometry is primarily a
refractive index, and surface roughness, making it ideal for surface-sensitive technique, with limited penetration depth
precise characterization of thin film structures. into the sample

Multilayer Analysis: Ellipsometry can analyze multilayered Limited Wavelength Range: The accuracy and sensitivity
structures, providing detailed information about each layer's of ellipsometry measurements depend on the wavelength
optical properties, thickness, and composition. range of the light source used.

Contactless Measurement: it does not require physical Typically requires flat and optically smooth surfaces for
contact with the sample surface. accurate measurements.

24
 Interferometry

In case of transparent films The reflected light will show an interference maximum for a
wavelength λ, when the path difference between successive
beams reflected at each surface

2𝑛1 𝑡𝑐𝑜𝑠𝜃 = mλ
m = integer
If no < n1 > n2

Minimum Intensity (dark band)

2𝑛1 𝑡𝑐𝑜𝑠𝜃 = mλ

If no < n1 > n2
Maximum Intensity (bright band)

2𝑛1 𝑡𝑐𝑜𝑠𝜃 = (m − 1/2)λ

Envolve interferometry to capture reflected and transmitted

light
25
 Interferometry for Transparent Films

Transparent films are highly suited for

interferometry since interference of light occurs
naturally between two surfaces
n1

n2

Film thickness=d

Optical film thickness n1d

For (n1> n2)
Maxima occurs at d= λ/4n1, 3λ/4n1, 5λ/4n1….

26
 Interferometry

Opaque films – not transparent

• If two rays reflected from two surfaces, depending on the path difference –
Inference pattern forms

• Path difference – difference in the path travelled by two rays

• Path difference decides whether you have constructive or destructive interference

forming fringes

• The shift in the fringe spacing – gives us the thickness

• Resolution is good about 1.5 nm

27
 Interferometry

Opaque films – not transparent

When highly reflecting surfaces are brought into close proximity, the interference fringes are
observed when the assembly is viewed in monochromatic light

Commonly employed for thickness measurement (now became standard method)

Optical flats must be highly reflective

The two adjacent fringes are

separated by λ/2

By adjusting the relative positions of

the optical flats to get a wedge-shaped
air gap, the fringes can be observed in
straight line ┴ to the step

28
 Interferometry

Condition for Constructive interference:

𝟐𝜹 𝒏−𝟏
𝟐𝑺 + = 𝒏𝝀; 𝑺= λ
𝟐𝝅 𝟐

The existence of the step now displaces the fringe pattern abruptly by Δ

Δ λ
The thickness of film 𝑑 =
𝑓𝑟𝑖𝑛𝑔𝑒 𝑠𝑝𝑎𝑐𝑖𝑛𝑔 2

Fringe width is 1/40 times the fringe spacing for highly reflective surfaces
Displacement can be easily detected

29
 Optical Constant Extraction

Terahertz Time Domain Spectroscopy (THz-TDS)

30
 Terahertz Radiation?

Electronics Photonics
THz: Where electronics meet Photonics

THz parameters Uniqueness of THz waves Technological gap

o Low photon energy o High power source
Frequency: 0.1 – 10 THz
o Longer Wavelength o Detectors
Wavelength: 3 mm – 30 microns
o Strong molecular absorption o THz optical components
Equivalent temperature: 1- 100 K
o Huge bandwidth (beyond 5G) ✓ Modulator
Energy: 0.41 - 41 meV 31
o Time domain ✓ Integrated systems…..
31
Applications of Terahertz Waves?
Material Characterization Terahertz Sensing
• Complex permittivity • Remote gas detection
• Complex conductivity • Molecule detection
• Carrier density • Hydration monitoring
• Mobility/Diffusion length • Phonon mode
• Ultrafast dynamics

Terahertz Imaging 6G Communication

• Security scanning • 6G communication

• Pharmaceutical /Food (~ Tbps speed)
• Medical diagnostics • Massive IoT
• HD imaging • Huge bandwidth
• LIDAR • Low latency (~ 0.1 ms)
32
 THz-TDS Setup

THz Pulse

THz Spectrum
Optical pump

ZnTe based THz-TDS system

Laser: Ti Sapphire laser
Wavelength: 800 nm light
Repetition rate: 1 KHz (1 ms)
33
Thin Film Characterization

ΔA ~ Re (σ)

ETHz
Δt ~ Im(σ)

34
Non-equilibrium Properties

ETHz Etotal ETHz + E1THz

J(t) – E1THz
𝑑𝐽(𝑡)
E1THz ~ ൗ𝑑𝑡
35
 Optical Constant Extraction

ΔA ~ Re (σ)
✓ Complex conductivity

✓ Complex refractive index Fourier Transform

✓ Complex permittivity
Δt ~ Im(σ)
✓ Mobility

✓ Scattering time
Complex THz conductivity of solid
✓ Number density
𝜀0 𝜔𝑝2 𝜔
𝜎 𝜔 = −𝑖𝜀0 ω(𝜀∞ − 1) +
𝑖 𝜔02 − 𝜔 2 + 𝜔Г1

Equilibrium and non-equilibrium optical constants / Dispersion 36

 Analytical Form of Transmission

~ ~  id ( n
~ − 1) 
2n ( nsub + 1) exp 
  (Through minimum error
Ta ( ) =
c T ( ) − Ta ( ) = 0
~ ~ ~ ~  2idn~ method)
(1 + n )(n + nsub ) + ( n − 1) exp 
 c 

T(ω) is the experimentally measured THz transmission.

d = thickness of the film
ω = angular frequency
n~sub = Terahertz complex refractive index of substrate
~ = n + ik = Complex refractive index of the film
n
Complex conductivity Dielectric constant
𝜎෤ 𝜔 = 𝑖𝜔𝜀𝑜 (1 − 𝑛෤ 2 ) 𝜀ǁ = 𝑛෤ 2
𝜎෤ 𝜔 = 𝜎𝑟𝑒𝑎𝑙 𝜔 + 𝑖𝜎𝑖𝑚𝑔 (𝜔) 𝜀1 = 𝑛2 − 𝑘 2 𝜀2 = 2𝑛𝑘
37
 Conti…

By processing conductivity and permittivity with appropriate model, more material

characteristics could be extracted
𝜎𝐷𝐶 𝑖Γ 𝜀0 𝜔𝑝 2
Drude Model 𝜎= =𝑖
(𝜔 + 𝑖Γ) (𝜔+𝑖Γ)

Complex conductivity
𝑛𝑒 2
Plasma frequency is given by 𝜔𝑝 2 = ∗
𝑚 𝜀0

n = Carrier density ꞷp = Plasma frequency

m* = Effective mass Γ = damping rate

38
 Mandatory Requirement

❖ Dry nitrogen or vacuum environment 39

Example: THz-TDS of Superconductor Thin Film

40
 Electrodynamics of Superconductors

➢ Conductivity
σ(ɷ, T) =σn(ɷ, T) +σs(ɷ, T)

T and ɷ are the key players

Where, σn(ɷ, T) – normal component of conductivity

σs(ɷ, T)- superconducting component of conductivity

➢Contribution due to normal carriers by Drude model

Where nn = normal carrier density

e = electron charge
τ = Momentum relaxation time 41
 Electrodynamics of Superconductors
➢ Contribution due to superconducting carriers by London equations (in low frequency
regime)

➢Complete frequency dependent conductivity is given by

➢Where λL is penetration depth and is given by

𝑛𝑒 2 𝑓𝑛 (𝑇)𝜏 𝑛𝑒 2 𝑓𝑛 𝑇 𝜔𝜏 2 𝑓𝑠 𝜔
𝜎𝑟𝑒 =
𝑚∗ 1 + 𝜔 2 𝜏 2 𝜎𝑖𝑚𝑔 = + Dramatic tunability
𝑚∗ 1 + 𝜔2𝜏 2 𝜏
42
 Superconductors at Terahertz
❖ Superconductor : Macroscopic coherent quantum system

Binding energy : 2
Phase

Amplitude

Superconducting gap 2 ~ few meV~ THz range

h

Superconductor Normal Metal

Physics and time scale behind Cooper pair dissociation and formation 43 and
Robert A. Kaindl, et. al. Terahertz Spectroscopy: Principles
Applications, 2017, 119 (Chap. 4)
Superconductors at Terahertz

Two fluid model of conductivity

nN (T) = Normal carrier density (/m3)

nS (T) = Cooper pair density (/m3)
e = electronic charge
m* = mass of the carrier
 = Angular frequency
τ = Scattering time
L = London penetration length
Robert A. Kaindl, et. al. Terahertz Spectroscopy: 44
Lkin = kinetic inductance Principles and Applications, 2017, 119 (Chap. 4)
 Conductivity of 25 nm YBCO Thin Film
7K
10 K Real part of conductivity
6
20 K 4x10 Imaginary part of conductivity
0.6 30 K
Transmission Amplitude

40 K

Conductivity (S/m)
50 K
3x106
55 K
60 K
0.4 65 K
70 K 2x106
72 K
74 K
76 K
78 K 1x106
0.2 80 K
82 K
84 K 0
90 K
100 K
0.0 120 K 0 50 100 150 200 250 300
0.3 0.6 0.9 1.2 150 K Temperature (K)
295 K
Frequency (THz)

✓ 54 % Broad band transmission change at 0.6 THz on changing temperature from 7 K to 295 K

✓ Very large imaginary part of the Conductivity in comparison to the real part at lower temperature

45
 Charge Carrier Density

1.0
1.5x1027 nn (Normal Carrier) fn (Normal Carrier)
ns (Cooper Pair) fs (Cooper Pair)
0.8
Carrier Density (/m3)

Carrier Fraction
1.0x1027 0.6

0.4
5.0x1026

0.2

0.0 0.0
0 10 20 30 40 50 60 70 80 90 0 10 20 30 40 50 60 70 80 90
Temperature (K) Temperature (K)

✓ Large increase in the Cooper pair fraction below transition temperature

46
✓ Cross over at about 40 K~ Large error in normal carrier density ~ Crossover within the error bar
Scattering Time and Kinetic Inductance

Scattering Time 100 Thin Film_25 nm

70

60
80

Kinetic Inductance (pH)

Scattering Time t (fs)

50
60 Kinetic inductance
40

30
Scattering time 40

20
20

10
0
0 10 20 30 40 50 60 70 80 0 10 20 30 40 50 60 70 80 90
Temperature (K) Temperature (K)

✓ Large variation of the scattering time

47
✓ Expected variation of the kinetic inductance
 Much More…..Transition Temperature

The transition temperature of the Superconductor films could be obtained by measuring THz Pulses
0.06 0.06
295 K 5K
6K
66 nm Thick NbTiN 0.04 0.04
7K
8K
0.02 TMax 0.02 9K
10 K

THz Field (V)

THz Field (V)

0.00 0.00 12 K

Peak to Peak THz

13 K
-0.02 -0.02
15 K
TMin 25 K
-0.04 50 K
-0.04
Measured TC = 10 K 100 K
200 K
-0.06 -0.06 250 K
295 K
-0.08 -0.08
192 195 198 201 204 190 192 194 196 198 200 202 204

Time Delay (ps) Time Delay (ps)

1st Derivative of Peak-to-Peak THz Pulse

0.025
0.12 1st Derivative of THz Pulse
Peak to Peak THz Pulse (V)

0.020 10 K
0.10
0.015
Peak to Peak THz Pulse
0.08
0.010
10 K
0.06
0.005

0.04 0.000

10 100
10 100
Temperature (K) 48
Temperature (K)
 Much More…..Microwave Properties

❖ Square parallel plate capacitors using a thin film

Complex reflection coefficient S11 of the varactors could be measured through VNA

Admittance, Y, could be expressed as

where G and C are the conductance and capacitance of the varactor and Z0 = 50 Ω

𝐺 𝐶𝑡
The effective loss tangent 𝑡𝑎𝑛𝛿 = , and the dielectric constant 𝜀𝑟 =
𝜀0 𝐴
𝜔𝐶 49
 Much More…..Thickness Measurement
Terahertz pulses passing through 500 micrometres thick sapphire substrate

2𝑛𝑑
0.1
Time delay =
𝑐

d = thickness
0.0
Terahertz Signal (mV)

If one know the refractive index, then can

calculate the thickness of the film
-0.1
11 ps 11 ps
11 ps

-0.2

-0.3
150 160 170 180 190 200
Time Delay (ps) 50
ELECTRON MICROSCOPY (EM)

51
 ELECTRON MICROSCOPY:

TRANSMISSION ELECTRON MICROSCOPY

Form Images using electrons that are transmitted
through a specimen.

Types of Electron Microscopy

SCANNING ELECTRON MICROSCOPY

Utilizing electron that are bounced off the surface of
the specimen.

52
TRANSMISSION ELECTRON SPECTROSCOPY (TEM)

53
 INTRODUCTION:
➢ The technology was first discovered by German
scientist Max Knoll and Ernst Ruska in 1931.
➢ In this, a beam of electrons is transmitted through an
ultra-thin specimen, interacting with the specimen as
it passes through.
➢ An image is formed from the interaction of the
electrons transmitted through the specimen; the image
is magnified and focused onto an imaging device, Ernst Ruska (Right) and Max knoll (Left)
pictured with their Invention, the first
such as a fluorescent screen, on the layer of magnetic electron microscope, Berlin,
1932.
photographic film.
54
 MAIN COMPONANTS

TEM has four main parts:

1. Electron gun: To produce the electron.

2. Condenser System: To focus the electrons bean to the specimen

3. Image producing system:

▪ It is made up of the objective lens, a movable stage holding the specimen, and intermediate and projector
lenses.

▪ They focus electrons passing through the specimen, forming a highly magnified image.

4. Image recording system:

▪ It is made up of a fluorescent screen used to view images.

▪ It also has a digital camera that permanently records the images captured after viewing.
55
 COMPONANTS OF TEM:

Electron source
electron beam
Secondary
electron

Condenser lens
Auger electron
Backscattered Condenser
electron Aperture
Photon
Sample

Objective
Selected aperture
area
Absorbed aperture Intermediate
Elastically electron lens
Scattered Projection
electron lens
Unscattered electron
Fluorescent Screen

Fig: signals generated when electron beam Fig: components of TEM

strikes the sample 56
 TEM ( Transmission Electron Microscope):
Principle:
➢ A heated tungsten filament in the electron gun produces electrons that get focused on the specimen by
the condenser lenses.

➢ Magnetic lenses are used to focus the beam of electrons on the specimen.

➢ Column tube of the condenser lens in a vacuum helps to create a clear image

➢ The vacuum allows electrons to produce a clear image without collision with any air molecule which
may deflect them.

➢ When the electron reaches the specimen, the specimen scatters the electrons which are focused by the
magnetic lenses

➢ Once the electrons reach a florescent screen, it form a polychromatic image.

57
How TEM Images looks?

Fig: Transmission electron micrograph of SARS-CoV-2

58
Image: By Microbe Notes
 ADVANTAGES & DISADVANTAGES

ADVANTAGE DISADVANTAGE
High Resolution: TEM offers incredibly high resolution, Sample Preparation: One of the major drawbacks of TEM is
allowing visualization of structures at the atomic level. the extensive and often challenging sample preparation
required.

Magnification: This enables detailed examination of small Thin sample: Specimens must be extremely thin (typically
features and structures. less than 100 nm) and electron-transparent, which necessitates
specialized techniques such as thin sectioning, ion milling, or
freeze-fracture.

Elemental Analysis: With the use of techniques such as High Vacuum Requirement: TEM operates under high
energy-dispersive X-ray spectroscopy (EDS), TEM allows vacuum conditions to prevent electron scattering, which can
for elemental analysis of specimens. affect image quality.

Beam Damage: The high-energy electron beam used in TEM

can cause radiation damage to specimens, leading to
structural alterations or sample degradation.

59
SCANNING ELECTRON MICROSCOPY (SEM)

60
 INTRODUCTION

➢ Electron microscope is, that images the sample surface by scanning it with a high-energy
beam of electrons in a raster scan pattern.

➢ The electrons interact with the atoms that make up the sample producing signals that contain
information about the sample's surface topography, composition , and other properties.

➢ Magnification in a SEM can be controlled over a range of up to 6 orders of magnitude from

about 19X to 300,000X.

61
 Basic component of SEM

➢ Electron Gun

➢ Condenser Lenses

➢ Objective Aperture

➢ Scan Coil

➢ Chamber

➢ Detector

➢ Computer Hardware
and software
Figure: Basic SEM Setup and Electron path
62
[Link]
SEM ( Scanning Electron Microscope)

Incident Beam

Primary Backscattered Electron

X-Rays Atomic no and topographical
Through Thickness information
Composition Information

Cathodoluminescence
Electrical information

Auger Electron
Surface sensitive Secondary Electron
Compositional information Topographical Information

Sample

The signals generated when electron beam strikes the sample 63

 SEM ( Scanning Electron Microscope)

Principle:

➢ The basic principle is that the beam of the electrons is generated by a suitable source, typically
a tungsten filament or a field emission gun.

➢ The electron beam is accelerated through a high voltage (e.g. 20kV) and passes through a
system of apertures and electromagnetic lenses to produce a thin beam of electrons.

➢ Then the beam scans the surface of the specimen. Electrons are emitted from the specimen by
the action of a scanning beam and collected by a suitably positioned detector.
64
 CHARACTERISTIC INFORMATION

➢ Topography :
The surface features of an object or “ how it looks “, its texture; direct relation between these
features and material properties.

➢ Morphology:
The shape and size of the particles making up the object ; direct relation between these
structure and material properties.

➢ Compositions;
The elements and compounds that the object is composed of and the relative amounts of
them; direct relation between composition and material properties.

➢ Crystallographic Information;
How the atoms are arranged in the object; direct relation between these arrangement and
material properties. 65
 VACUUM CHAMBER

➢ SEM requires a vacuum to operate.

➢ Without a vacuum, the electron generated by the electron gun would encounter constant
interference from air particles in the atmosphere.

➢ Not only would these particles block the path of the electron beam, but electrons would also be
knocked out of the air and onto the specimen, which would distort the surface of the specimen.

66
 How SEM Images looks?

Award-winning SEM image of an Image of pollen grains taken on a A gold-coated spider, prepared for
Ant was taken by Stefan Eberhard SEM shows the characteristic depth viewing with an SEM
of Complex Carbohydrate Research of field of SEM micrographs Image courtesy: Toby Hudson
Ctr, Univ of Georgia.

67
[Link]
 ADVANTAGES & DISADVANTAGES
ADVANTAGE DISADVANTAGE

High Resolution SEM system are expensive to purchase, operate and

maintain.
SEM is highly sensitive to surface features and can While SEM typically requires less sample preparation
provide detailed information about surface topography, compared to techniques like transmission electron
texture, and composition. microscopy (TEM), Some specimens may still require
special preparation techniques such as coating with a
conducting layer to prevent charging effect.

SEM can be used to analyse a wide range of material, The high energy electron beam used in SEM can cause
including Metals, ceramics polymers, and biological damage to sensitive samples, such as biological
specimens. specimens or polymer, leading to change the
morphology or composition.

Some advanced SEM system allow for real-time

imaging and analysis.
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 Conclusion

❖ The measurements of thin film characteristics are extremely important

❖ The choice of characterization technique depends on the property under investigation and
the desired accuracy

❖ In-situ and non-destructive techniques could be preferred tool to measure thin film
properties

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Thank You

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