Unit 4 - Characterization of Thin Film Properties

Characterization of Thin Film Properties 18G5B14
Unit 4
Characterization of Thin Film Properties
➢ Film thickness measurement: Quartz crystal thickness monitor and Stylus Profiler methods.
➢ Film composition: X-ray Photoelectron Spectroscopy
➢ Surface morphology and topography: SEM, AFM.
➢ Electrical characterization: Four probe analyzer, Hall effect measurement
➢ Optical characterization: Ellipsometry, Raman Spectroscopy.
➢ Dielectric and Mechanical properties characterization.
Film thickness measurement:

a. Quartz Crystal Microbalances
Quartz crystal microbalances are used within vacuum deposition chambers to measure thin film thickness
on substrates.
Principle: The quartz crystal thickness Monitor or Controller is based on the “piezoelectric effect”
principle that the oscillating frequency of a quartz crystal is changed by the mass of a deposited film on its
upper face. Electronically measuring this effect allows for a determination of the thickness of a deposited
film.
where f is the frequency, m is mass and k is force constant of the cantilever. The optical, semiconductor,
solar cell, and thin film display (OLED) industries etc, use quartz crystal monitoring in their production
processes. Quartz crystals monitor thickness at the Ångström level that is 10 nano meter or 0.0000001
millimeters. This extreme level of precision accuracy is critical because thickness deviations as little as 10
Angstroms can have a major effect on product performance.
The in-situ thickness monitoring system components are
i. the crystal,
ii. the sensor head, (with the electrical connection, water lines, thermocouple and heating elements)
iii. the feedthrough, which connects the internal components with the air side.
iv. cables and fittings from the feedthrough,
v. the oscillator which makes the crystal vibrate and measures this continuously, and
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vi. the monitor or controller which displays and acts upon this information.
vii. An internal microprocessor then converts this frequency into the actual thickness of the film.
i. Quartz Crystals
The two type of quartz crystals used in film thickness measurement are AT and RC types. The AT crystal is
characterized through the molecular tetrahedral quartz crystal structure and single angle cut which allows it
to vibrate when a voltage is applied to it. The frequency that the crystal exhibits naturally is constant until a
few angstroms of material have been deposited onto it, changing that frequency. The disadvantage of the
AT crystal is that the frequency of the crystal is also sensitive to temperature and internal deposited material
stress. The RC Crystal, is not sensitive to internal stress or high temperatures, and predominately responds
to only film accumulation on the surface. This makes the RC crystal more effective in measuring film
thickness
ii. Sensor heads
This is the mechanical assembly where the quartz crystal is placed and electrical contacts connect the crystal
to an oscillator. The sensor head contains water or air lines for cooling, a heater for changing the sensor
head temperature, and a thermocouple to monitor temperature at all times. A sensor head must be
demountable or replaceable this is accomplished by using a cap, or holder for the crystal. The holder will be
mounted into a sensor body.
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iii. Feedthroughs
The feedthrough is the metal assembly that connects the sensor head and its electrical and liquid or airlines
through the vacuum chamber wall.
iv. Oscillator
The oscillator is an electrical circuit that forces the crystal into vibration or “oscillation.” It does this by
finding a natural, or resonance, frequency for the crystal, and tracking it as this frequency changes with the
addition of coating. Oscillators must be placed close to the feedthrough (within 6-10″) because the
crystal connecting cables make up part of the oscillating circuit. If they are too long, they weaken the
strength of the vibration and the crystal measurement becomes erratic.
v. Monitor or Controller
The monitor or controller is a microprocessor based electronic instrument that takes the frequency
information from the oscillator, through a coaxial cable, and uses it to calculate the film thickness or rate of
thickness being deposited. Depositing a thin film on the crystal’s surface will change the mass of the crystal.
The increase in mass from the deposition causes the resonant frequency of the crystal to decrease.
The changes in the oscillation frequency is continuously recorded by monitor and controller, which
then converts the frequency data into (Thin Film Deposition) thickness data by performing
appropriate mathematical functions. The data includes both instantaneous rate and cumulated thickness.
b. Stylus profiler
A stylus profilometer is a basic tool that allows ex-situ measurement of the physical thickness of films. It
uses a diamond tip dragged on a surface with very light pressure to get information about surface
topography.
Profilometry: is an easy-to-understand mechanical technique for measuring film thickness. It works by
monitoring the height of a stylus as it drags across a step in the film (as shown in the figure). The primary
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advantage of profilometry is that it can be used on all solid films, including opaque materials such as
thick metal films.
All profilometers consist of at least two parts – a detector and a sample stage. The detector is what
determines where the points on the sample are and the sample stage is what holds the sample. In some
systems, the sample stage moves to allow for measurement, in others the detector moves and in some both
move.
There are two types of profilometers: stylus and optical. Stylus profilometers use a probe to detect the
surface, physically moving a probe along the surface in order to acquire the surface height. This is done
mechanically with a feedback loop that monitors the force from the sample pushing up against the probe as
it scans along the surface. A feedback system is used to keep the arm with a specific amount of torque on it,
known as the ‘setpoint’. The changes in the Z position of the arm holder can then be used to reconstruct the
surface.
A stylus profilometer involves physical movements in X, Y and Z while maintaining contact with the
surface, it is slower than non-contact techniques. The stylus tip size and shape can influence the
measurements and limit the lateral resolution.
The stylus shaft of a profilometer is typically about 20 mm in length. The stylus tip in contact with the
surface is typically a 45º diamond cone with an end radius of 25 µm. Various sensors may be used to
detect the vertical movement of the stylus, including linear variable differential transformers, three
plate capacitive sensors, and optical levers. The diagram below shows an optical lever configuration
similar to the one used in atomic force microscopy. In operation, as the translation stage drags the
sample under the stylus tip the tip stays in contact with the surface, and as the stylus rotates about the
pivot the laser light reflecting off of a mirror above the pivot tracks this motion across a position
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sensitive photodetector. The amplified photodetector signal is digitized by a computer for graphical
representation of the surface profile and data processing.
Film composition: X-ray Photoelectron Spectroscopy

X-ray photoelectron spectroscopy (XPS), also known as electron spectroscopy for chemical analysis
(ESCA) is primarily used for identifying the chemical species present in the film.
PRINCIPLE: Incident X-rays cause photoemission of electrons from the sample surface. These are
energy analyzed, allowing the binding energy of the emitted electron to be obtained.
XPS or ESCA is a surface-sensitive analytical technique that analyzes the energy of the
photoelectrons (50-2000 eV) that are emitted when a surface is bombarded with X-rays in Vacuum.
The energy of these electrons is characteristic of the atom being bombarded and thus allows identification of
elements [in much the same way as in AES-Auger Electron Spectroscopy].
When X-ray photons are incident on a solid, they eject electrons (photoelectrons) from the valence
band. Electrons can be emitted from any orbital, and photoelectron emission occurs as long as the X-ray
energy exceeds the binding energy of the electrons. The determination of the kinetic energy of the outgoing
electron is the cornerstone of experimental XPS.
The kinetic energy EK of the photoelectron is given by EK = hν - EB - q ϕsp
where hν is the energy of the incident X-ray photon, EB the binding energy of the electron, and q ϕsp is the
work function of the spectrometer.
The electron binding energy (EB) is influenced by its chemical surroundings, and is suitable for determining
the chemical states of the atoms by measuring the energy shifts.
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Instrumentation:
✓ The THREE basic components of XPS are the X-ray source, Spectrometer and a High Vacuum (to
protect the sample from contamination).
✓ Choice of X-ray source will depend on two factors:
• X-ray energy must be high enough to excite an intense photoelectron, and
• X-ray line width should be as narrow as possible; hence typically the K-alpha X-radiation from
Magnesium (1253.6 eV) or Aluminum (1486.6 eV) is used for analysis.
• The XPS electrons are detected with the most common Cylindrical Mirror Analyzer (CMA). A
“double-pass CMA” is generally used to discriminate against small energy shifts.
• Chemical compounds or elements are identified by the location of the energy peaks on the
undifferentiated XPS spectrum. Concentration determination is more difficult.
• “Peak heights and areas” can be used with appropriate correction factors to obtain concentrations, but
the method is primarily used for identification.
Advantages & applications:

1) XPS is a “surface sensitive” method because the emitted photoelectrons originate from the upper 5 – 0.5
nm of the sample.
2) Since X-rays tend to be less destructive when compared with electrons (e -beam), XPS is more suitable
for polymers, oxides and organics than AES.
3) XPS/ESCA is primarily used for identifying chemical species at the sample surface. Since the electron
binding energy (EB) is influenced by its chemical surroundings, EB is suitable for determining chemical
states of the atoms by measuring energy shifts.
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4) XPS is generally used to determine the ratio of chemical states of compounds in the surface.
5) XPS play(s)ed a major role in understanding the chemistry and reaction mechanisms in the development
of plasma etching.
6) XPS avoids the electron damage and heating that is sometimes encountered in AES.
7) XPS is one of the primary techniques for analyzing the Elemental, Chemical and Electronic
Structure of organic materials. For example, it can determine the chemical environment of each of the
carbon atoms in a hydrocarbon polymeric material.
8) Sensitivity of XPS is around 0.1%.
Surface morphology and topography

a. Scanning Electron Microscope
The SEM uses electrons instead of light to form an image. SEM is a powerful and commonly used
instrument, in both academia and industry for imaging the surfaces of almost any material with a
resolution down to about 1 nm. Most of the scanning electron microscopes have magnification
ranges from 20X to 100000X. SEM image gives a characteristic three-dimensional appearance and
useful for adjudging the surface structure of the sample.
Principle: The smallest distance resolved by a microscope is called Limit of resolution (Δx) and the
resolving power of a microscope is the reciprocal of the limit of resolution.
where 2μsinθ is called the numerical aperture of the objective. Thus shorter the wavelength (λ) of the
radiation, greater is the resolving power.
It is this resolving power that sets a limit to the magnification of the microscope, because a mere increase
in the magnifying power without a corresponding increase in the resolving power would only produce
large blurred image. Optical microscope uses a light beam of wavelength ≈ 600 nm so that the
smallest distance resolvable ≈ 300 nm(Assuming numerical aperture = 2). Hence, if instead of light waves
we could use electron beam the resolving power can be increased by more than 106 fold.
The magnification can be calculated making use of de Broglie waves associated with electrons,
accelerated to approximately 75 kV which has a wavelength of 4.48x10-12 m which is roughly 105 times
shorter than visible radiation.
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In optical microscopes, ‘light waves’ produce the image and magnification is obtained by ‘optical lenses’.
An electron microscope generally uses electron waves and the electron beam is focused by suitable
magnetic lenses.
Magnetic lens:
The magnetic fields which are axially symmetric have a focusing effect on the electron beam passing
through them. The axially symmetric magnetic fields are produced by short solenoids. Such solenoids are
called magnetic lens. The focal length of such magnetic lens depends on the quality of coil and current. By
adjusting the current through the coils the intensity of the magnetic field and the focal length can
be adjusted. It is widely used in electron microscopes.
Working Principle of the SEM:
A beam of electrons are produced by heating a thermionic filament. And it is operated with an acceleration
voltage of 1 KV to 40 KV for the electrons. The electron beam follows a vertical path and it makes its way
through a set of magnetic lenses which focuses and directs the beam towards the sample. These electrons
interact with the sample to a depth of ~1μm and generate a number of different types of signals, which are
emitted from the area of the specimen where the electron beam is impinging. The induced signals are
detected and the intensity of one of the signals (at a time)
is amplified and used as the intensity of a pixel on the
image on the computer screen. The electron beam, then
moves to the next position on the sample and the
detected intensity gives the intensity in the second
pixel and so on. This produces an image with depth-of-
field which is usually 300-600 times better than that of an
optical microscope, and also enables a three-dimensional
image to be obtained.
Construction:
A schematic of SEM is shown in the figure. Electrons are
thermionically emitted from a tungsten filament (cathode) are drawn to an anode and focused by two
successive magnetic lenses into a beam with a very fine spot size that is typically 10Å in diameter. Pairs of
scanning coils located at the objective (magnetic) lens deflect the beam either linearly or in raster fashion
over a rectangular area of the specimen surface. Upon impinging on the specimen, the primary
electrons decelerate and several processes such as elastic scattering viz., forward scattering and
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backscattering of the incoming electrons and inelastic scattering viz., generation of secondary
electrons, Auger electrons, Bremsstrahlung, characteristic X-rays, electron-hole pairs (in insulators and
semiconductors), long-wavelength electromagnetic radiation etc. A number of different types of signals,
which are emitted from the area of the specimen where the electron beam is impinging.
Various SEM techniques are differentiated on the basis of what is subsequently detected and
imaged, and the principle images produced in the SEM are of three types:
• Secondary electron images,
• Backscattered electron images and
• Elemental X-ray maps.
The secondary electrons are the electrons which are generated from the surface of the specimen
when it is bombarded by high energy primary electrons. These electrons are collected by detector
which creates a pattern of light and dark areas on a computer screen corresponding to the emission
of secondary electrons from the specimen. As the number of electrons produced at any given point can
be related directly to the topography of the specimen with respect to the detector, the patterns created
on the viewing screen represent the surface topography of the specimen.
Backscattered electrons are the high energy electrons that are elastically scattered and essentially possess
the same energy as the incident or primary electrons. The probability of backscattering increases with the
atomic number of the sample material. Therefore the primary electrons arriving at a given detector position
can be used to yield images containing information on both topography and atomic composition.
An additional electron interaction in the SEM is that the primary electron collides with and ejects a core
electron from an atom in the sample. The excited atom will decay to its ground state by emitting
either a characteristic X-ray photon or an Auger electron. By analyzing energies of characteristic of
the x-ray photon the atoms can be identified. Further the concentration of atoms in the specimen can be
determined by counting the number of X rays emitted.
Applications:
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The SEM is the most widely employed characterization instrument for obtaining thin film
surface topography and morphology, including
• grain size and shape
• existence of compounds
• formation of textured surfaces
• evidence of film voids
• micro-cracks and lack of adhesion
b. Atomic Force Microscopy (AFM)

Principle: Atomic Force Microscope (AFM) is a high-resolution microscopy technique which produces
precise 3-dimensional topographic images of a sample by scanning the surface with a nanometer-scale
probe/tip (lateral resolution ~ 1 nm, vertical ~ 0.1 nm) and by measuring attractive or repulsive forces
between a tip and the sample.
These deflection are used to study the morphological and textural
characteristics like roughness, waviness, lay and flaws of diverse
surfaces along with the physical properties like elasticity,
adhesion, hardness and friction
Instrumentation: An AFM system consists of a
• Cantilever with a sharp Tip
• Scanner (which moves the tip)
• Microscope (which holds the scanner and sample)
• Controller (which houses all the electronics)
• Computer (used for instrument control and image analysis).
Working: A cantilever with a sharp tip is scanned across the surface of the specimen. The short range or
long range forces between the tip of the cantilever and the specimen surface cause the deflection of the
cantilever according to Hooke’s law. This deflection of the cantilever is measured using the change in the
reflection angle of the laser spot incident on the top surface of the cantilever which behaves like a mirror.
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This reflected laser light is collected by a position sensitive detector to generate a map of the surface
topography.
There are three main operational modes viz.
i. Contact AFM (Probe-surface separation is < 0.5nm)
ii. Intermittent contact/tapping mode AFM (Probe-surface separation is 0.5-2 nm)
iii. Non-contact AFM (Probe-surface separation range is 0.1 – 10nm)
In contact mode, the cantilever drags across the sample surface and it uses the deflection of the cantilever to
measure the contours of the surface. To eliminate the noise and drift that can affect a static signal, low
stiffness cantilevers are used, but this allows strong attractive forces to pull the tip to the surface. To
eliminate this attraction, the tip is in contact with the surface where the overall force is repulsive.
In non-contact mode, the tip vibrates slightly above its resonance frequency and does not contact the surface
of the sample. Any long range forces, like van der Waals forces, decreases the resonant frequency of the
cantilever.
In tapping mode, the cantilever uses a piezoelectric element mounted on the top to oscillate it at near to its
resonance frequency with amplitude of up to 200nm. The forces cause the amplitude to decrease as the tip
gets close to the surface, and the height of the cantilever adjusts to keep the amplitude constant.
This tapping results in less damage to the sample than contact mode and is more accurate than non-contact
mode when moisture is present on a sample.
Cantilever and Tip

1) The stiffness of the caintilever needs to be less i.e., the effective spring constant holding atoms
together must be in the order of 1 – 10 nN/nm.
2) The tip should have a radius of curvature less than 20-50 nm (smaller the better) with a cone angle
between 10-20 degrees.
3) To obtain both low spring constant and high frequency ( >2 KHz), mass of the cantilever should be very
small (~ 10-10 kg).
4) Microlithography process is used to make the cantilevers. Si or Si3N4 are used for making tips. A thin
gold layer is deposited on upper side of the tip for good reflectivity of laser beam.
5) Tips are generally evaluated by their “end radius” which limits the resolution of AFM.
6) The "normal tip" is a 3 μm tall pyramid with ~30 nm end radius.
7) The electron-beam-deposited (EBD) tip or "supertip" offers a higher aspect ratio (it is long and
thin, good for probing pits and crevices) and sometimes a better end radiusthan the normal tip.
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8) The "Ultra-lever" is based on an improved microlithography process. Ultra-lever offers a moderately high
aspect ratio and on occasion a ~10 nm end radius.
Advantages of AFM
• Easy sample preparation
• Accurate height information
• Works in Vacuum, Air, and Liquids
• Living systems can be studied
• Magnification of the sample along all the three axes.
Limitations of AFM
• Limited vertical range
• Limited magnification range
• Data not independent of tip
• Tip or sample can be damaged
APPLICATIONS of AFM: AFM is a versatile tool to investigate
• Topography of surfaces
• Properties of surfaces – roughness, pin hole formation, defects, grain size analysis, Young’s modulus
• Properties of single molecules
• Forces within molecules
Electrical Characterization of Thin Films

a. FOUR PROBE METHOD:
The electrical conductivity of thin films deviates from the bulk conductivity due to the size effect
(film thicknesses < 1 µm) and because of other effects as e.g. grain size or incomplete continuity of the film.
The conductivity can be determined by the sheet resistance Rs. The four-point Probe technique is one of the
most common methods for measuring the electrical resistivity because two-probe methods are more difficult
to interpret.
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The four-point probe simply consists of four "pogo pins" closely spaced and mounted in-line. It's important
the spacing from pin-to-pin is exactly the same (S in the diagram). Generally, these are spaced about
2 to 4 mm apart. The measurement requires a four-terminal ohmmeter. The outer two pins are connected to
the constant current source and the inner pins connect to the voltmeter. The four –terminal ohmmeter
reads out the calculated resistance (V/I in the equations). The reason we use the four-terminal ohmmeter is
that the low resistance measurements are much more accurate than the two-terminal ohmmeters, because the
effect of probe and lead resistance is factored out.
The sheet resistance Rs of the thin film is independent of the film dimensions (any shape or size) other than
thickness.
V
RS = k /sq or /sq
I
Where k is a constant depends on the configuration and spacing of the contacts. If the “film is large in
extent compared with the probe assembly” and the “probe spacing is large compared with the film
thickness”, k = π/ln2 = 4.53. Otherwise, correction factors must be applied. If the film thickness (t) is
known, the resistivity ρ is readily obtained by ρ = t x Rs Ω cm
b. Hall effect method

Measurements of the Hall effect and resistivity form the most important technique to directly obtain the
charge carrier concentration and mobility of a conductive / semi conductive specimen.
When a current-carrying thinfilm is placed in a transverse magnetic field, the Lorentz force on the moving
charges produces a voltage perpendicular to both the field and the current. This is known as the Hall Effect.
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Measurements of the Hall voltage are used to determine the density and sign of charge carriers in the
specimen. When this is known, the effect is used as a probe for magnetic field measurement.
To measure the Hall voltage, a rectangular film/specimen is taken and a potential difference is applied
across its ends, a current ‘I’ flows through it along x direction. The current through the specimen is given by
I = nAevd (1)
Where n- concentration of electrons
A- Area of cross section of end face
e- charge on the hole
vd- drift velocity of holes
therefore current density J = I/A = nevd (2)
Any plane perpendicular to current flow direction is an equipotential surface. Therefore potential difference
between front and rare faces is zero. If magnetic field is applied normal to crystal surface and also to the
current flow, a transverse potential difference is produced between the faces F & F/. It is called Hall voltage
VH.
Before the application of magnetic field B, the electrons move in an orderly way parallel to faces F
& F/. On the application of magnetic field B, the holes experience a sideway deflection due to the Lorentz
force FC. The magnitude of this force is given by
FL = e B vd
Because of this force, holes are deflected towards the front dace F and pile up there. Initially the
material is electrically neutral everywhere. However as holes pile up on the front side, a corresponding
equivalent negative charge is left on the rare dace F/. As a result an electric field is produced across F &
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F/.The direction of electric field will be from front face to rare face. It is such that it opposes the further pile
up of holes on the front face F. A condition of equilibrium is reached when FE due to transverse electric
field EH balances the Lorentz force. The transverse electric field EH is known as Hall field.
In equilibrium condition
FE = FH
FE = e EH = e (VH/w) (3)
Where w- width of semiconductor plate
From eqn (2) vd= Jx/ne
BJ X
Therefore FL = (4)
n
Equating (3) and (4) we get
eVH BJ X
=
w n
wBJ X wBI
 VH = =
ne neA
If ‘t’ is the thickness of the semiconductor plate, A=wt. Then above equation reduces to
BI
VH =
net
Hall field per unit current density per unit magnetic field is called Hall co-efficient RHThus
EH V /w wBJ x
RH = = H =
BJ x BJ x wneBJ x
1
RH = (6)
ne
Substitute (6) in (5) we get
BI
VH = R H (7)
t
VH t
RH = (8)
BI
The Hall voltage can be measured with a voltmeter with the direction of magnetic field & current depicted
in this fig, the sign of Hall voltage is negative.
1 BI
The charge carrier concentration is given by n=− =−
R He VH te
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For metals and n-type semiconductor Hall voltage will be –ve, and for p-type semiconductor Hall voltage
will be +ve, when the direction of current is same as in the figure. Therefore by knowing the sign of Hall
voltage the conductivity of the material & the sign of the majority charge carriers will be known.
The carrier concentration of p-type semiconductor is
1 BI
p= =
R H e VH te
Optical characterization
Raman Spectroscopy
Raman Spectroscopy is a technique used to study vibrational, rotational and other low-frequency modes in a
system. It relies on inelastic scattering or Raman scattering of monochromatic light, usually from a laser in
the visible, near infrared or near ultraviolet range. The laser light interacts with phonons or other excitations
in the system, resulting in the energy of the laser photons being shifted up or down. The shift in energy
gives information about the phonon modes in the system.
A schematic layout of Raman spectrometer is shown in figure. The sample to be analyzed is illuminated
with a monochromatic light and the light scattered by the sample is examined using a spectrometer. At the
molecular level, photons can interact with matter by absorption or scattering process. Raman scattering
occurs when the system exchanges energy with the photon and the system subsequently decays to
vibrational energy levels above or below that of the initial state. The frequency shift corresponding to the
energy difference between the incident and scattered photon is known as the Raman shift. Depending on
whether the system has lost or gained vibrational energy, the Raman shift occurs either as an up-shift or
down-shift of the scattered photon frequency relative to that of the incident photon. The down-shifted and
up-shifted components are called the Stokes and anti-Stokes lines, respectively.
A plot of detected number of photons versus Raman shift gives a Raman spectrum. As different materials
have different vibrational modes and therefore characteristic Raman spectra can be used for material
identification.
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For material characterization most of the Raman spectrometers use a microscope to focus the laser beam to
a small spot (<1-100nm diameter). Light from the sample passes back through the microscope optics into
the spectrophotometer. Raman shifted radiation is detected with a charge-coupled device (CCD) detector
and a computer is used for data acquisition and curve fitting. These factors have helped Raman
spectroscopy to become a very sensitive and accurate technique.
Advantages:
• This technique can be used for the identification of a wide range of substances in solid, liquid and
gaseous states.
• It is a non-destructive straightforward technique requiring no special sample preparation procedures.
Ellipsometry - for optical and dielectric characterization

Ellipsometry is an optical technique for investigating the optical or dielectric properties (complex refractive
index or dielectric function and extinction coefficient) and thickness of thin films.
Ellipsometry measures the change of polarization upon reflection or transmission and compares it to a
model. It is an optical technique used to determine when a parallel beam of monochromatic light of known
polarization is incident on a semi transparent thin film, the amplitude of the two perpendicular components
of the polarized light and the relative phase difference between them changes due to reflection which results
in the film properties like thickness and optical constants, they can be determined using this technique.
Actually these parameters cause changes in the ellipticity of the polarized light and hence the name
“ellipsometry”.
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Thus by measuring the ellipsometric parameters viz. the relative change in amplitude (Ψ) and change in
phase (Δ) and knowing the refractive index of the material, angle of incidence and wave length of the light,
one can calculate the thickness of the film.
Construction:
A typical ellipsometer consists of the following six parts:
• Light source
• polarizer
• photo elastic modulator
• analyzer
• a detector
Light source: It can be either a laser or a lamp emitting continuous spectrum (Xenon) with a
monochromator and a focusing system.
Polarizer: It consists of a quartz window and a piezoelectric transducer. It modulates the light beam
polarization at 50kHz with the help of computer and control electronics.
The analyzer: It is a linear polarizer which resolves the polarization state of the reflected beam.
The detector: The detector can be any device, able to measure the intensity of the light wave. Generally,
two types of detectors are employed viz. photomultipliers and InGaAs photodiodes for UV-vis and NIR
applications respectively.
Working:
A light from the source is linearly polarized using a polarizer and is made to be incident on the surface
of the sample. The linearly polarized light from the sample surface, becomes elliptically polarized, and
travels through a PEM. The function of PEM is to introduce a difference in the phase velocity between
the ordinary and extraordinary rays leading to a modulated phase shift. Analyzer examines the
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incoming lights having different phase velocities and sends the information to the detector. The detector
converts the light into respective electronic signal to determine the polarization of the reflected light.
This information is compared with the known input polarization caused by the reflection at the sample.
From the ellipsometric parameters obtained from this experiment one can calculate the refractive index
and the thickness of the sample.
For the measurement of complex reflectance ratio ρ of a system, which may be parametrized by the
amplitude component Ψ and the phase difference Δ. The polarization state of the light incident upon
the sample may be decomposed into an s and a p component (the s component is oscillating
perpendicular to the plane of incidence and parallel to the sample surface, and the p component is
oscillating parallel to the plane of incidence). The amplitudes of the s and p components,
after reflection and normalized to their initial value, are denoted by RS and RP respectively. The angle
of incidence is chosen close to the Brewster angle of the sample to ensure a maximal difference in RP
and RS Ellipsometry measures the complex reflectance ratio ρ (a complex quantity), which is the ratio
of RP over RS
Thus, tanΨ is the modulus of amplitude reflection ratio, and Δ is the phase shift (difference) between s
and p polarized reflected light.
Mechanical properties
Nano-indentation- nano-scratch, and nano-wear testing.
Nano-indentation is a standard method to investigate mechanical properties like hardness,elasticity,plasticity
index of the surfaces on a submicroscopic scale. The indenter takes a small diamond, which is shaped as
either a pyramid or a sphere, and pushes the diamond tip into the surface of the material being tested. The
depth of indentation can range from a couple of hundred nanometers to a maximum of 4 microns. By
measuring the force required to push the diamond tip into the material compared to the depth of the
indentation, the instrument can determine the hardness of the sample. Seeing to what degree the material
returns to its previous shape determines its elastic modulus - the stiffness of its atomic bonds. In addition to
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mechanical properties, the nanoindenter can be used to scratch films and coatings to see how they stand up
to wear.
The figure shows an indentation load-displacement curve, illustrated along with important parameters. like
the stiffness, S*, is the slope of the tangent line to the unloading curve at the maximum loading point (hmax,
Pmax)
In most equipment currently in use, the load is applied either by an electromagnetic or a piezoelectric
device. In the former case, the load is determined by the current, while in the latter case, the installation of a
load cell is required. The resolution is often better than 10 nm. The displacements are typically measured by
a capacitive device giving resolutions as small as 0·1 nm. The most commonly used indenter is a diamond
of the Berkovich type, a triangular pyramid with the same depth-area relation as the standard Vickers
indenter (square pyramid), that is, the cross-sectional area varies as the square of the depth of the
indentation.
20

Unit 4 - Characterization of Thin Film Properties

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Unit 4 - Characterization of Thin Film Properties

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Characterization of Thin Film Properties 18G5B14

Film thickness measurement:

Film composition: X-ray Photoelectron Spectroscopy

Advantages & applications:

Surface morphology and topography

b. Atomic Force Microscopy (AFM)

Cantilever and Tip

Electrical Characterization of Thin Films

b. Hall effect method

Ellipsometry - for optical and dielectric characterization

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