Chapter 2
Chapter 2
Chapter 2
The integrity of thin films is influenced by the quality of its adhesion to and
conformal coverage of the underlying layer, residual or intrinsic stresses after
deposition, and the presence of surface imperfections such as pinholes. The
adhesion of a thin film to the substrate or underlying layer is of great concern in
ensuring the reliability of the thin film. A thin film that is initially adhering to the
underlying layer but lifts off after the device is subjected to thermo-mechanical
stresses can result in field failures. Reliable thin film adhesion depends greatly on
the cleanliness of the surface upon which the film is deposited. Optimum substrate
roughness also affects thin film adhesion. A very smooth substrate decreases
adhesion tendency. A very rough substrate on the other can result in coating
defects, which can also lead to thin film adhesion failures.
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Regardless of the deposition process, thin films always end up with an
intrinsic stress which can either be tensile or compressive. High residual stresses
can lead to adhesion problems, corrosion, cracking, and deviations in electrical
properties. Thus, proper deposition is critical to minimize intrinsic stresses in thin
films.
Formation of a thin film takes place via nucleation and growth processes.
The experimental and theoretical studies of a thin film growth can be presented as
follows:
2. The adsorbed species are not in thermal equilibrium with the substrate
initially and move over the substrate surface. In this process they
interact among themselves, forming bigger clusters.
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nucleus size depend on a number of parameters such as the energy of the
impinging species, the rate of impingement, the activation energies of
adsorption, desorption, thermal diffusion, and the temperature,
topography, and chemical nature of the substrate. A nucleus can grow
both parallel to the substrate by surface diffusion of the adsorbed species,
and perpendicular to it by direct impingement of the incident species. In
general, however, the rate of lateral growth at this stage is much higher
than the perpendicular growth. The grown nuclei are called islands.
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a. Island type, called Volmer-Weber type
Figure 2.1: Thin film growth modes- (a) Volmer Weber, (b) Frank-van der Merwe
and (c) Stranski-Krastanov
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2.1.1.2 Frank-van der Merwe growth
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grains oriented parallel to each other and connected by low-angle grain
boundaries. These films show diffraction patterns similar to those of single
crystals and are called epitaxial single-crystal films.
Besides grain boundaries, epitaxial films may also contain other structural
defects such as dislocation lines, stacking faults, micro twins, and twin boundaries,
multiple-positioning boundaries, and minor defects arising from aggregation of
point defects (for example, dislocation loops, stacking faults, and tetrahedral and
small dot like defects). Note that defects such as stacking faults and twin boundaries
occur much less frequently in polycrystalline films. Dislocations with a density of
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10 to 10 lines/cm2 are the most frequently encountered defects in polycrystalline
films and are largely incorporated during the network and whole stages due to
displacement misfits between different islands. Some other mechanisms which may
give rise to dislocations in thin films are
(3) Continuation into the film of the dislocations apparently ending on the substrate
surface.
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each vertical column grows multi granularly with possible deviations from normal
growth. Figure 2.2 shows various defects incorporated into thin film systems.
Figure 2.2: A schematic diagram showing the incorporation of defects in thin film
during synthesis.
There are certain factors which affects the growth of a thin film over a
substrate. Few of them are listed in figure 2.3.
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Figure 2.3: Qualitative representation of the influence of various deposition
parameters on the grain size of thin films.
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rough films which become continuous at relatively large thicknesses. High surface
mobility, in general, increases the surface smoothness of the films by filling in the
concavities.
Figure 2.4: Qualitative variation of (a) the roughness factor and (b) The film
density as a function of film thickness.
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2.1.3.2 Adhesion
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2.2 EXPERIMENTAL AND ANALYTICAL TECHNIQUES
X-Ray diffractometer
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Electron Beam Physical Vapor Deposition or EBPVD is a form of physical
vapor deposition in which a target anode is bombarded with an electron beam given
off by a charged tungsten filament under high vacuum. The electron beam causes
atoms from the target to transform into the gaseous phase. These atoms then
precipitate into solid form, coating everything in the vacuum chamber (within line of
sight) with a thin layer of the anode material.
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The BC300 box coater system procured from HIND HIVAC, Bangalore is a
versatile PVD system capable of supporting both electron beam and thermal
evaporators. Pumped by 550 l/s Turbo molecular pump (Varian Inc.) and support by
a rotary vane pump, the system can be pumped down to maximum vacuum of 2 x
10-7 mbar. Equipped with a four source selector, the system is capable to sequential
evaporation of up to four metals/alloys without breaking the vacuum. The system
also boasts of a substrate heater (800C), a radiant heater (200C) and a large rotary
drive capable of handling industrial grade samples.
The vacuum is measured by use of two digital Pirani gauges and one Inverted
Magnetron Gauge of high vacuum measurement. The electron beam gun is typical
270 bent beam gun which ensures least sample and filament contamination
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for sputtering light elements neon is preferable, while for heavy elements krypton or
xenon are used. Reactive gases can also be used to sputter compounds. The
compound can be formed on the target surface, in-flight or on the substrate
depending on the process parameters. The possibility of many parameters that can
control sputter deposition make it a complex process, but also allow experts a huge
degree of control over the growth and microstructure of the film.
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Figure 2.6: Plasma plume in a RF sputter deposition system
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2.2.3 Scanning Probe Microscope
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advanced versions, currents can even be passed through the tip to probe the
electrical conductivity or transport of the underlying surface, but this is much more
challenging with very few groups reporting reliable data.
The AFM consists of a cantilever with a sharp tip (probe) at its end that is
used to scan the specimen surface. The cantilever is typically silicon or silicon
nitride with a tip radius of curvature on the order of nanometers. When the tip is
brought into proximity of a sample surface, forces between the tip and the sample
lead to a deflection of the cantilever according to Hooke's law. Depending on the
situation, forces that are measured in AFM include mechanical contact force, van
der Waals forces, capillary forces, chemical bonding, electrostatic forces, magnetic
forces, Casimir forces, solvation forces, etc. Along with force, additional quantities
may simultaneously be measured through the use of specialized types of probe.
Typically, the deflection is measured using a laser spot reflected from the top
surface of the cantilever into an array of photodiodes. Other methods that are used
include optical interferometry, capacitive sensing or piezoresistive AFM cantilevers.
These cantilevers are fabricated with piezoresistive elements that act as a strain
gauge. Using a Wheatstone bridge, strain in the AFM cantilever due to deflection
can be measured, but this method is not as sensitive as laser deflection or
interferometry.
If the tip is scanned at a constant height, a risk would exist that the tip
collides with the surface, causing damage. Hence, in most cases a feedback
mechanism is employed to adjust the tip-to-sample distance to maintain a constant
force between the tip and the sample. Traditionally, the sample is mounted on a
piezoelectric tube that can move the sample in the z direction for maintaining a
constant force, and the x and y directions for scanning the sample. Alternatively a
'tripod' configuration of three piezo crystals may be employed, with each responsible
for scanning in the x, y and z directions. This eliminates some of the distortion
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effects seen with a tube scanner. In newer designs, the tip is mounted on a vertical
piezo scanner while the sample is being scanned in X and Y using another piezo
block. The resulting map of the area s = f(x, y) represents the topography of the
sample.
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microscopy, scanning tunneling microscopy and magnetic force microscopy. The
multipurpose scanner used for analysis is an 8 micron scanner. Equipped with a very
good software program for data collection, rendering and analysis the Pico LE is an
ideal system for characterization of thin film samples. Typical tips used are silicon
or silicon nitride tips depending on the necessary applications.
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Figure 2.8: Photograph of Xpert Pro XRD system
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audio speakers, though this approach was dropped due to the interferences through
the in phase magnetic noise produced. The induced voltage in the pickup coil is
proportional to the sample's magnetic moment, but does not depend on the strength
of the applied magnetic field. In a typical setup, the induced voltage is measured
through the use of a lock-in amplifier using the piezoelectric signal as its reference
signal. By measuring in the field of an external electromagnet, it is possible to obtain
the hysteresis curve of a material.
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Figure 2.9: Photograph of Scanning Electron Microscope
The scanning electron microscope used for the work is the FEIs Quanta 200
tungsten filament SEM. A typical electron microscope it is capable of resolving
images up to a resolution of around 50nm. Attached with a dry EDS system the
equipment is capable to elemental analysis of the samples in parallel with the
imaging of the samples. Non conducting samples need to be typically coated with a
catalyst before analysis.
When linearly polarized light reflects from a magnetic film, its polarization
becomes elliptic (Kerr ellipticity) and the principal axis is rotated (Kerr rotation).
The amount of rotation and ellipticity is proportional to a component of the
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magnetization of the film. The type component measured depends on the optical
configuration used. The most commonly used configurations are:
Figure 2.10: Typical homemade Magneto Optic Kerr Effect (MOKE) setup.
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2.2.8 Vibrating Sample Magnetometer (VSM)
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In a typical setup, the induced voltage is measured through the use of a lock-in
amplifier using the piezoelectric signal as its reference signal. By measuring in the
field of an external electromagnet, it is possible to obtain the hysteresis curve of a
material.
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Four-terminal sensing is also known as Kelvin sensing, after William Thomson,
Lord Kelvin, who invented the Kelvin bridge in 1861 to measure very low
resistances. Each two-wire connection can be called a Kelvin connection. A pair of
contacts that is designed to connect a force-and-sense pair to a single terminal or
lead simultaneously is called a Kelvin contact. A clip, often a crocodile clip that
connects a force-and-sense pair when it closes or slides onto a conductor is called a
Kelvin clip.
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