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Smart materials are different from every day materials due to the flexibility in altering
its properties which can be significantly altered in a controlled fashion by external stimuli
such as stress, temperature, electricfield, and magnetic field. Representation of the smart
Photoconductor Electrical
Optical Optical
Photo Chromic
Piezoelectric
Electrostrictive Electrical
Magnetostrictive Magnetic
Mechanical
Magneto chromic Optical
1
Among the above smart materials, piezoelectric materials are of great interest, as
they are commonly used as sensors, actuators and memory devices. As technology is
advancing, efforts are being made to use piezoelectric materials in combination with
voltage applied across the material. Piezoelectric materials occur naturally and also
occur in the form of multiphase ceramics and films. Berlinite, quartz, cane sugar,
rochelle salt are some of the naturally occurring piezoelectric materials. Some of the man
made piezoelectric ceramics are barium titanate, lead titanate, lead zirconium titanate
Barium Titanate (BaTio3) is the first piezoelectric ceramic introduced for applications
in ultrasonic transducers as fish finders [2]. After that PZT was introduced this has better
widely used piezoelectric material in sensors and actuators applications. The major
2
Flexibility in the change of characteristics due to varying stoichiometry of the
PZT.
PZT is a pervoskite crystal with lead atoms at corner and oxygen atoms at the face
center of unit cell. The atomic size of the lead and oxygen is 1.4 Å; titanium or
Lead (Pb)
Titanium/Zirconium (Ti/Zr)
Oxygen (O2)
Lead, oxygen and titanium/zirconium atoms together form a face centered cubic
array, as shown in Figure 1. PZT is manufactured by the sol-gel process and the radio
frequency magnetron sputtering process. They are usually available in the form of discs,
wires, plates and rods. To understand the properties of PZT it is important to be familiar
3
Dipole: A pair of opposite charges is called dipole. there moment is called dipole
moment.
Poling: The method of aligning the randomly occurring domains in the direction
distortion of the piezoelectric material under the applied electric field of uniform
piezoelectric property. Curie temperature for the PZT film is 2800 C (553 K).
4
Coercive field: Piezoelectricity is a property of ferroelectric materials. During
poling the domain structures are aligned along the direction of the applied electric
field. When the applied electric field is removed, polarization produces the
hysterisis loop. The reverse electric field required to cancel the remanent
The application of PZT ranges from sensor to power harvesting devices as shown
in Figure 2.
POWER
HARVESTING
ACTUATORS
Industrial applications of PZT for the economic benefits of the community and future
5
(a) Sensor
PZT is used for self-powered strain energy sensors (SES) to convert the applied
mechanical strain to electrical charges for charging a capacitor. Equation (1) explains the
Dn = d i ,j T j+εnm E m ……………………………(1)
in the signal strength is due to the amount of charges in the capacitor and the amount of
charges in the capacitor is related to the straining of PZT. The piezoelectric approach for
self powering has several advantages including: a) small size, b) low sensor cost, and c)
(b) Actuators
There are various types of actuators, like bilayer and multilayer piezo ceramic
actuators. In the case of the multilayer actuator, various PZT materials are stacked
together. PZT materials on their own are not suitable for actuation tasks; they must be
(expands) roughly proportional to the voltage given up to about 0.1% at typically 150V,
6
based on the converse piezoelectric property [4].
ferroelectrics. Poling of the PZT aligns the randomly oriented dipoles along the direction
of applied electricfield and hence the PZT becomes polarized. When the applied
electricfield is removed, all dipoles do not fall back to their initial state, leading to a
PZT as shown in the Figure 3. The hysterisis property is used for memory allocations in
PZT. PZT is used as ferroelectric random access memory (Fe-RAM) in the memory
device manufacturing industries. PZT in Fe-RAM has many advantages such as non-
7
(d) Power Harvesting
energy into an usable energy for the electrical devices. Polyvinylidene fluoride (PVDF)
was implemented in vivo on a mongrel dog for power harvesting. Periodic expansion and
contraction of the rib cage in the mongrel dog strains the PVDF to generate charges [6].
PVDF was used in a self-powered damage detection unit; the charge generated during the
crack generation was stored in a capacitor, which in turn charges the transmitter to
transmit the signal to a receiver [7]. Much of the research in the field of power
harvesting has involved in the studies of optimizing the circuit design to store the energy.
Gradually researchers realized that the circuit built for optimizing the charge storage lead
to more leakage of charges [8]. PZT was used to charge the batteries ranging form 40 to
1000 mAh. PZT was vibrated at a random frequency range of 0-500 Hz; the
electromechanical efficiency was 6.57%; the typical charge cycle of one battery is shown
in Figure 4 [9].
8
Physics and media group from MIT conducted three different experiments on
parasitic power harvesting. They used PZT unimorph, PVDF stave and electric generator
for energy scavenging. PZT unimorph was glued in a shoe sole, under the heel of the
foot as shown in the Figure 5. Unimorph PZT produced 2mW at 2 Hz, which was greater
then the PVDF stave; the power generated as a function of time during the brisk walk is
Figure 5. PZT pasted on the shoe sole under the foot heel.
9
Factors affecting the Properties PZT
hysterisis and dielectric constant determines the wide range applications of PZT. The
PZT; Leakage current with smooth surfaces and rough surfaces was 10 -7A/cm2 and10-
6
A/cm2 respectively [11]. The factors that affect the ferroelectric properties of the
PZT like local crystallographic orientation and the local grain-grain interactions play
was used for analyzing the polarization switching behavior at the grain corners and
boundary sites [12]. The influence of poling temperature, poling electric field, poling
coupling factor of the PZT were studied; the results of the above research are
From all of the above data, the importance of PZT is seen in the field of sensors,
actuators, memory devices, power harvesting and also the factors affecting the PZT
properties. Nanoparticle coating is one of the many research areas to improve the
10
Table II. PZT property as a function of poling time, temperature and electricfield.
electrode
Saturated at
constant temperature-
180o C
Saturated at
coupling temperature-
180o C
Nanoparticles are the particles with the size less than 100 nm. There are several
forms of nanoparticles available in the market. Most common are carbon nanotubes,
quantum dots, ferrous nanoparticle (FNP), zinc oxide (ZnO) nanoparticle, gold [Au] and
copper (Cu) nanoparticles. Nanoparticles are widely used in the medical and engineering
fields. For example, FNP is used for drug delivery and as charge injection devices.
11
a) High surface area to volume ratio.
magnetic storage devices, optical grating, energy harvesting and antireflective coating.
Thin film deposition of nanoparticles has been achieved successfully on a wide range of
silicon, m-plane of alumina, glass and (100) plane of NaCl single crystal [14]. Sprayable
conjugative polymer, acts as a light harvesting films, shows a photovoltaic effect in the
infrared region [15]. Nanoscale mechanical energy was converted into electrical energy
using zinc oxide nanowire arrays; energy transfer efficiency was 17-30% [16].
Nanoparticle coating for power harvesting or energy harvesting is a new field and has
interest in power harvesting. Hence, understanding the properties of the ZnO and FNP is
Zinc oxide nanoparticles are gaining importance because of its applications in the
field of optoelectronic and photovoltaic devices; Zinc oxide nanoparticles observed under
a SEM is shown in Figure 7. Zinc oxide nanoparticles are transparent conducting oxides.
12
The ZnO nanoparticle is a wide band energy [3.3eV] semiconductor as shown in Figure
8. ZnO possesses high exciton binding energy of 60 meV; high exciton energy leads to
The ZnO nanoparticle is the hardest of the II-VI family of semiconductors. This
means that its performance will not be degraded as easily as other compounds through the
appearance of defects [17]. Some of the physical and chemical properties of the ZnO are
described below.
13
Figure 8. Band gap energy of ZnO compared with various semiconducting
materials.
GaAs).
Very large shear modulus ~45.5 Gpa (indicates stability of the crystal), compared
14
with 18.35 Gpa for ZnSe, 32. 60 Gpa for GaAs and 51.37 Gpa for Si.
nature and possess low coercive field and high magnetic susceptibility. The viscosity of a
to the ferrous nanoparticle density. The particle appears like a catalyst and produces free
radicals, which lead to the cross linking of the molecular chains and eventual congealing
of the fluid. The catalytic action is high at elevated temperatures. Therefore, they tend to
by Brown and Neels mechanisms [19]. Ferrofluids with FNP are used as lubricants,
charge injection devices, high memory data storage arrays (5nm FNP could store one bit
of information) and actuators; they have an average size of 10nm. Properties of the FF
are shown in the Table IV. The carrier used may be organic solvents or water. Various
surfactants are used to prevent the agglomeration of the magnetic nanoparticles. Oleic
acid, citric acid, tetra methyl ammonium hydroxides are the common surfactants used.
The magnetic property of the FNP in the ferrofluid encouraged Sai et al [20] for FNP
coating on the PZT; it will act as an additional magnetic energy on the PZT surface. The
response change of PZT due to FNP coating on the PZT surface is represented in Figure
9. FNP coating under the influence of a magnetic field on PZT improved the
15
polarization due to the additional magnetic energy on PZT surface [21].
(1hr@500c)
16
PZT with FNP Treatment
25
0
20
0 PZT under
15
magnet
0 FNP coated
10 PZT
0
PZT
E (mV)
5
0
O
R
N
E
S
P
S
0
0 5 10 15 20 25
Current (Amps)
Figure 9. Comparison of the responses of PZT, FNP coated PZT and PZT treated
under the magnetic field.
magnetic field overcomes the surface energy of the ferrofluid and forms ferrous cones.
These ferrous cones are used as low electron source for charge injection devices [23].
The arrays of pointed structure or the cones as shown in the Figure 10 have various
17
Figure 10. Ferrous cones on the aluminum substrate.
cones with a wide band gap semiconductors like ZnO nanoparticles. Ferrous cones could
semiconductors, which can absorb and emit photons in the ultraviolet light bands.
Coating the ferrous cones with the ZnO nanoparticles will be an alternative for the
photocathode systems and source of electrons. This technology has various advantages
a) ZnO avoids the oxidizing properties associated with ferrous cones and can be
b) ZnO in ferrous cones are expected to impact a wide range of electronics and
18
tunneling microscopes, atomic force microscopes and low-power propulsion
systems.
How to coat ferrous cones with a semiconductor like ZnO for the above
described advantages?
FNP coating on PZT has increased sensitivity [20]. How will the
mixture?
Though PZT has various applications, literature on its tribological properties are
scarce. To enhance the PZT applications in the field of MEMS it is essential to study the
structures with the ability to resist failure under mechanical and thermal loads. The large
surface to volume ratios and low restoring forces, unwanted adhesion and friction
dominate the performance of the MEMS. The macroscopic contacts of MEMS are
cracks due to the high friction at the asperities contact. The characteristics of surface
morphology and properties of single asperity contacts can be studied by atomic force
microscopy (AFM). Based on the above facts, minimizing the effect of adhesion,
19
fractal morphology and to evaluate efficiency of the D-RAM component [25]. PZT
domain stability, mobility and structure are a function of friction due to the fluctuating
stresses. Low friction leads to low mobility and decreases the domain walls. Change in
defects and change in the real structure of the PZT. Presence of these defects is going to
affect mobility and stability of domain walls. Predicting the surface defects, interfacial
friction and energy and early elastic deformation with respect to the ramped load at the
Improving the piezoelectric property of the PZT is a major concern to expand the
range of applications. FNP coating on PZT is going to provide the additional magnetic
energy and improve the magnetoelectric effect of the PZT and in turn increase the
response of the PZT [21]. The effect of mixing ZnO nanoparticles in a ferrofluid is
studied by coating this mixture on the PZT and subjecting it to power harvesting.
Comparison of the power harvesting capability of plain PZT, FNP coated PZT, and (ZnO
The importance of studying the atomic friction and interfacial atomic defects on
necessity for development of a high spatial resolution tool to analyse these challenges.
analyse the atomic friction and to identify the atomic defects at the sliding interface. This
tool is effectively used on the silver coated PZT by considering its applications to
20
MEMS.
21
CHAPTER II
THEORY
2.1 Tribology
Tribology relates to the study of friction, wear and lubrication at the interface of
two or more surfaces in contact. Tribology is a vast subject and it is important to prevent
failures at the contact interface due to sliding, rolling, or rubbing. In 1966, the lack of
million in the year 1966. One-third of the world’s energy resources used are subjected to
friction in one form or the other [27]. Research in tribology has gained importance after
these statistics were realized and extensive research on preventing the loss due to friction
The better performance of the MEMS is possible through the study of tribology at
the microscale or nanoscale leading to a new subject known as nano/micro tribology. The
Friction is a part of tribology and is defined as the force opposing the motion of
rubbing surface. There are various laws that define the factors affecting friction. In
1699, Amontons law was stated as, “friction forces are proportional to the load applied
and independent of the surface area”. After some years, Hirn [28] distinguished the
22
friction variation on the unlubricated and lubricated surface. The coefficient of friction
for the lubricated surface was reduced as compared to the unlubricated solid surface.
Hence, Hirn added the effects of velocity, load and surface area on friction. In 1892,
Ewing related the origin of the friction to the surface forces and defined friction as the
opposing molecular force for the applied load, eventually leading to the molecular
displacement.
Tomlinson’s theory correlates the interaction between the two sliding elements at
the molecular level. According to Tomlinson, the energy is dissipated as the molecules
are forced into each other atomic field. This is the theory widely used to analyse the
nanoscale is proportional to the contact area, load applied, contact pressure and surface
forces at the sliding interface [27]. In many cases, simple empirical formulas used for the
describing friction at macroscale is not applied to the nanoscale because of the high
surface area to volume ratio, surface chemistry, adhesion and the roughness effects.
Hence, the friction force varies nonlinearly to the load applied and the models used to
analyze it are explained in the Section 4.1.1 [29]. For example, Figure 11 represents
friction force variation at the nanoscale over an increased load on Carbon-60 (C 60) and
Germanium Sulphide (GeS) surface. The nonlinear response of the friction vs. load is due
Corrugations seen on the friction forces which are distinctively different in shape
is called as stick-slip friction. Sliding action of the surface asperities undergoes sudden
slips during sliding motion [31]. The friction due to stick-slip is studied to analyse the
23
friction at nanoscale.
Figure 11. Friction force vs. load [Si tip on the GeS and C60].
2.1.2 Stick-Slip
When the two surfaces slide on each other they can have an abrupt motion or an
irregular motion. This irregular motion is due to the asperities on sliding surface which
leads to stick-slip motion. The sliding process is not a continuous one; the motion
proceeds by jerks. The asperities “stick” together until, as a result of the gradually
increasing pull, there is a sudden break with a consequent very rapid “slip” [28].
Periodic Stick-Slip: The signal with potential (friction force) maxima and minima has
Random Stick-Slip: The signal with friction force potential maxima and minima have
Stepped Stick-Slip: There is a step increase in the friction force potential. The saw
toothed maxima, has increased force maximum than the force amplitude before.
24
Figure 12. Different types of stick-slip process.
Stick-slip friction provides information on the interface science in many ways. Some
As the atoms in one plane are in equilibrium with the neighboring plane, when
the shear forces are applied at the interface, the atoms deform elastically
called as slip and the prior situation where atomic equilibrium existed is called
as stick. This slip may be related to loss of energy or fracture due to periodic
Between the two sliding surfaces, asperities at the interface undergo elastic
deformation known stick” and the release of the energy leads to plastic
to the dislocations of atoms and the freezing is related to the strain hardening
25
of the atoms [33]. In many cases the rapid slip of the upper surface relieves
some of the applied force which eventually falls below another critical value
Fk, the kinetic friction, at that point the film resolidifies and the whole stick-
Stick-slip behavior varies with applied load, scan speed and scan direction
between different regimes of atomic scale friction and provides insight into
the origins of friction and may lead to the ability to control it [36].
predict the intensity of the friction force. Reducing the force amplitude is
friction [37].
Could the extensive study of stick-slip explain the relation between friction
Slip due to the atomic dislocation could be also due to the atomic defects;
hence, stick-slip could be used for imaging the atomic defects [38].
tribological behavior of the PZT. Further, these tribological characteristics could be used
for designing the PZT based MEMS for sliding applications and the relation between
26
PZT electromechanical efficiency and load acting on it. AFM is used for obtaining the
stick-slip signal at the sliding interface; AFM description is given in the following
Section.
physical properties of a surface using a profiler or sharp tip probe. The probe is placed at
a point where the surface force effect exists. The probe is raster scanned over the surface
by keeping a constant force; this raster scan displays the surface topography. AFM
consists of a cantilever beam with a probe, laser beam, piezotube scanner and a laser
The probe is very sensitive to surface forces and as the probe scans over the
sample, the probe gets deflected due to the surface forces; the feed back control system is
27
used to keep the probe and sample distance constant. The deflection of the probe will
yield a surface image; AFM has been effectively used in the field of friction analysis at
Force calibration mode is used in studying the interface science [tip and the
sample surface interaction]. In force calibration mode X and Y voltages applied to the
piezotube is held at zero and a saw tooth voltage is applied to the Z-electrode of the piezo
tube. The force measurement starts with the sample far away and the cantilever tip at its
rest position. As a result of the applied voltage the sample is moved up and down and a
cantilever tip deflection signal is monitored using the photodiode. The force curve, a plot
of the cantilever tip deflection signal as a function of the voltage applied to the piezotube,
is obtained. Figure 14 shows the force separation curve; the arrow head reveals the
direction of the piezo tube travel. At point 1, the tip is off the sample surface. From
point 1 to 2 there is no change in the deflection signal as the piezo tube extends, because
the force is initially zero and the sample has not come into contact with the tip. At point
2, the force between the tip and sample becomes attractive. The attractive force increases
till the point 2’ of the sample-tip, until the sample-tip force becomes repulsive. The
maximum forward deflection of the cantilever multiplied by the spring constant of the
cantilever is the “pull-off” force. At point 3, the deflection signal reaches maximum and
the piezo tube starts to retract. At point 4 the cantilever is not deflected, but due to
adhesion between the tip and the sample. The tip sticks to the sample and the cantilever
is bent down as the piezo retracts. The attractive force between the tip and sample
becomes equal to the spring force at point 5. At point 6 the cantilever has returned to its
28
undeflected state. Cantilever deflection signal remains constant as the piezo continues to
retract to point 7.
AFM is used for measuring friction in the form of friction force microscopy. A 0o
scan angle corresponds to sample scanning in the “y” direction, and a 90o scanning angle
corresponds to the sample scanning perpendicular to the “y” axis in the xy-plane (along x
axis). This scan is called as perpendicular scan, where the scanning tip experiences only
frictional force.
As the tip is perpendicularly scanned over the sample, twisting of the tip takes
place. Twisting of the tip will deflect the laser beam on to the horizontal and vertical
quadrant of the photodetector. The differential signal between the left (L) and right (R)
photo detector is denoted as friction force signal and calculated from {(L-R)/ (L+R)}
[27].
29
High Speed Data Capture is a function in the AFM used for collecting the friction
time resolution is going to provide high spatial resolution. This property is important in
analyzing the atomic scale stick-slip friction. Phase fluctuation based processor is used to
Phase fluctuation based processing produces better gain over the amplitude based
analysis of the signal. Studying the amplitude variation of the acoustic signal to identify
the noise and signal is a traditional method of obtaining high signal-to-noise ratio.
Sometimes the noise also has the same fluctuation as that of the signal and it is difficult to
identify the difference between the signal and noise. Amplitude based signal-to-noise
ratio does not consider the unpredictable dynamic changes in the signal. High signal-to-
noise ratio is obtained by reading the variation of phase angle with respect to time, where
deviation from the aligned phase angle is called as noise. Phase fluctuation based signal
30
2.2.1 Working Principle
Figure 15.
Phase fluctuation is defined on three planes for self correction of the phase rate and
direction of phase angle rotation. As phase angle approaches zero, the phase angle
temporal coherence increases with gain (signal-to-noise ratio). The mathematics used in
31
i i 1
(t ) d dt i ………………………………………… (3)
ti ti 1
(t ) d d
2
…………………………………………… (4)
dt 2 dt
i = Aligned phase angle of the vectors
(i 2i 1 i 2 )
i i …………………………………………… (5)
t 2
For a coherent signal,
(t ) =Constant; (t ) = 0
The phase fluctuation ( i ) on the polar plane is defined as the phase angle i of
pressure vector Ri is out of uniform phase angle rotation with phase angle i 1 and i 2 of
the previous two phasors Ri 1 and Ri 2 , as represented by the equation 2. Uniform rate of
phase fluctuation is termed as constant angular velocity; constant angular velocity gives
zero angular acceleration. Any deviation of the angular acceleration from the zero point
Twisting of the cantilever tip corresponds to the friction force experienced by it.
Uniform deflection of the cantilever tip is considered to have uniform phase fluctuation
and hence, called as signal or “stick” and the deviation from this uniformity is considered
High spectral resolution and friction signal-to-noise ratio is essential for analyzing
the stick-slip at nanoscale and will solve the challenges mentioned in stick-slip studies.
This phase fluctuation mathematics and HSDC function in the AFM together form the
tribo-diagnostic tool.
32
CHAPTER III
EXPERIMENTAL DETAILS
The AFM with HSDC function is used for collecting the friction signal data. This
friction signal data is analysed using the phase fluctuation based mathematics coded in
Matlab. The AFM calibration and HSDC methods followed in this research for
Atomic Force Microscopy is used for the tribo diagnostics of the PZT smart
material. AFM supplied by the digital instruments with the nanoscope V software is used
for this experiment. Various AFM parameters used for this experiment are shown in the
Table V.
33
Table V. AFM Parameters for studying the friction force signal.
High Speed Data Capture (HSDC) is used for obtaining unprecedented time
resolution of the interfacial friction signal. This is a data collection tool in the
collecting data [41]. The step-by-step procedure used to collect the friction signal
PZT surface and silicon nitride [AFM cantilever Tip] is cleaned with methanol
The cleaned PZT surface is glued on the metallic disc and stuck on the
34
For contact mode the feed back control system with proportional gain = 3 and
The laser point is concentrated on the cantilever tip using upper and lower
knob in the AFM. In the meantime, look at the laser signal on the screen and
try to get the laser point below the center of the cross (to get ~-2 V vertical
silicon nitride tip and the silver coated PZT surface. Calculate the deflection
Based on the deflection sensitivity of cantilever, the load acting on the sample
At each load applied on the PZT surface, sliding of the silicon nitride
The twisting of silicon nitride tip during scanning on the PZT surface
generates a differential signal [lateral force deflection] from the left and right
The friction signal data in the form of ASCII format is saved in the computer
analysis mathematics was coded in Matlab. The interfacial friction signal data
35
collected at each load ranged from 40 to 200 nN was exported in ASCII
format to Matlab.
The Section below explains the experimental setup for nanoparticle coating to
This Section explains the experimental set up for nanoparticle coating to improve
Coating Materials:
5E thin sheets were used for the power harvesting experiment. The
properties of P-5E piezofilm are given in Table VI [2]. The SEM image of
36
Table VI. Property of the PZT [P-5E].
[18].
37
Edmund Saturation Surface
[42]. The properties of the ZnO nanoparticles are short listed in Table VIII.
4) Ultraviolet (UV) light of wavelength 130 nm was used for curing the
Experimental Procedure:
harvesting.
38
b) The surface of the aluminum strip is cleaned with alcohol and PZT is
39
Magnet glued wooden board
Rectangular box with an
aluminum strip UV Light
glued aluminum strip is drenched with the ferrofluid and the ferrofluid
40
Figure 19. Rectangular box with the slot to hold the PZT glued aluminum
strip.
e) Disc magnets of strength 400 gauss are glued on the small wooden plate
as shown in the Figure 20. Two wooden plates with south and north poles
of the magnets are glued. These magnet glued wooden plates are placed
with the north Pole disc magnets on the top and the south pole disc
magnets below the rectangular box. Hence, the magnetic field passes
41
Figure 20. Magnet glued wooden piece to create the magnetic field on the
coating surface.
g) The PZT glued aluminum strip is pushed into the rectangle box slot.
h) For FNP coating, the ferrofluid is poured on the PZT glued aluminum
strip in the slot, and the ZnO nanoparticles mixed in ferrofluid solution
i) Disc magnet glued wood pieces are placed on the rectangular box. The
magnetic lines of flux pass through the coated PZT glued aluminum, from
42
l) Three each of PZT glued aluminum strips, FNP coated PZT glued
aluminum strips and FNP+ZnO coated PZT glued aluminum strips were
prepared.
The nanoparticle coated PZT glued aluminum plates are shown in Figure 21.
Sometimes the base of PZT glued aluminum strip was coated, to avoid the effect of
coating on the PZT base in the power harvesting, the coating at the base is scraped using
a scrapper.
a)
b)
Figure 21. a) FNP coated PZT glued aluminum strip; b) FNP+ZnO coated PZT
glued aluminum strip.
43
3.3 Power Harvesting
This Section presents the equipment and the experimental set up for implementing
the above coated PZT and plain PZT for power harvesting.
Equipment used for the power harvesting experiment are as listed below:
a) Exciter
b) Function Generator
c) Oscilloscope
Exciter has a dc generator fixed to the output shaft. The AC-voltage from the
used for oscillating the aluminum plate with either PZT or nanoparticle coated
PZT.
b) Function Generator: It is used for the generating the sinusoidal signal at the
frequency.
harvesting experiment.
44
The experimental setup used for the power harvesting experiment is
shown in Figure 22. The step-by-step procedure for the power harvesting setup is
explained below.
Alligator clip
Function generator
Aluminum strip
Exciter
Oscilloscope
1) The tip of the PZT glued aluminum plate is fixed on the exciter [basically
a cantilever support].
cables.
the PZT glued aluminum plate; they are connected to the oscilloscope.
45
3.3.2 Experimental Procedure
The function generator is used for generating the sinusoidal signal at a frequency
of 90 Hz [kept constant]. As the PZT glued aluminum strip is excited at 90 Hz, due to
piezoelectric property of the PZT, a voltage is generated which is then recorded with the
oscilloscope. Similarly, the FNP coated PZT and FNP+ZnO coated PZT are used to
analyze the importance of nanoparticle coated PZT over plain PZT as related to power
harvesting.
46
.
Chapter IV
4.1 Tribo-Diagnostics
Based on the experimental procedure described in Section 3.1, the friction signal
data was collected and analyzed using the tribo-diagnostic tool. The tribo-diagnostic tool
possesses high spatial resolution, spectral representation of the friction signal, and pattern
representation of the stick-slip friction. The results of the tribo-diagnostic tool on the
Friction force at nanoscale is calculated based on the surface forces during the
sliding of cantilever tip on the silver coated PZT (P-5E) surface. There are two models
used for calculating the nanofriction, the JKR model [Johnson, Kendall and Roberts] and
The JKR model is appropriate for strongly adhering materials with short range
surface forces. The DMT model is opposite to the JKR model. The DMT model is used
for stiff, weakly adhering materials with long range forces. Since the PZT surface is stiff
and has long range forces, the DMT model is used to predict the nanofriction at the PZT
interface [44].
47
DMT Model [44], [45]:
F= Friction Force, nN
= Adhesive force, nN
F * A ………………………………… (6)
Geff
25
……………………………… (7)
2* GPZT *GTIP
Geff ………………………. (8)
(GTIP GPZT )
Contact area and pull off force is given in the equation 9 and 10
2/3
3R
A * L 2 R ………………………. (9)
4E
48
Lc
……………………………. . (10)
2 R
Friction force is calculated based on the following data, under the load (L) of 40nN.
GPZT 124Gpa
GTIP 33.5GPa
Geff =52.749Gpa
=2.110Gpa……………………………… (11)
A =1.44*10-17m2……………………… (13)
The above mathematics is used for calculating the friction force at each load
(80,120,160 and 200nN) and it is depicted in Table VIII and as shown in Figure 23.
49
Table VIII. Load vs. Friction Force (nN).
40 0.3
80 0.48
120 0.63
160 0.77
200 0.91
The interfacial friction force as a function of the load with the topographic image
after each load is represented in the Figure 23. The friction force in the region of 40 to
50
120 nN is non-linear relates to the surface force effects at low load or high friction at low
load. Beyond 120 nN the friction force is linear till 200 nN.
The friction signal data [43122 data points] from the AFM was collected in 2.47 s
at a sampling frequency of 17.4 KHz. Each sond of the force signal data is magnified to
17 sec, and totally 42 sec of data is plotted for 2.47 sec. Hence, 58 ms of friction signal
data is analyzed as one second in the specgram. Each 58 ms friction signal data is
divided into 1024 points for recognizing the friction signal temporal coherence.
At 80 nN Figure 24 (a) shows the friction signal in the random stick-slip form
obtained directly by the AFM. This friction signal is represented in the form of a
represented on the “y- axis” and time (s) on the “x-axis”. The dark red region in the
specgram represents a high friction region and its FFT shows high amplitude. High
amplitude relates to high intensity of twisting of the silicon nitride cantilever tip.
51
(a) (b)
Figure 24. a) Friction force signal collected at a time resolution of 6. 25 MHz for a
load of 80nN. b) Specgram and FFT of the friction signal at 12-23 Hz for a load of
80nN.
a) Load: 40nN
52
a) Load: 40nN
b) Load: 120nN
53
c) Load: 160nN
d) Load: 200nN
Figure 25. a), b) c) and d) Friction signal, specgram and FFT of the friction signal ,
with an increasing load 40, 120, 160 and 200 nN respectively.
Spectral representation of the friction signal shows the region of high and low
54
friction. It is hard to differentiate the amplitude of the friction signal variation over the
load ranging from 40 to 200 nN due to lack of spatial resolution. The FFT of this friction
signal as represented above is windowed using the Hilbert transform. This windowed
signal is used for phase fluctuation analysis to obtain better spatial resolution. The above
results are an approach towards better spatial resolution of the friction signal.
High resolution pattern representation of the silicon nitride tip scanning on the
PZT (P-5E) surface represents the stick-slip behavior of the interfacial friction. Tip
velocity is 199 nm/s; the distance traveled in 58 ms (1024 points) is 11.61 nm. Hence,
100 points represents 11.3 Å. This is represented in the stick-slip chart shown in Figure
26. As the tip is scanned over the PZT surface, slip/atomic displacement or acoustic noise
aligned phase fluctuation from zero or the deviation from the uniformity of tip twisting
during the tip sliding on the PZT surface. The region before this fist slip is considered as
the elastic deformation regime. The downward arrows represent the qualitative relation
between the slip and zero magnitude. The pattern as shown in the Figure 26 is a precise
55
Slip/Atomic Defect
Elastic Regime
before first slip 11. 3Å
Figure 26. The phase and magnitude representation of stick-slip and elastic regime
before first slip at a load of 40 nN.
a)
56
43Å
b)
51Å
c)
57
108Å
d)
188Å
Figure 27. a), b), c) and d): Represents the stick-slip variation and the elastic
regime before first slip due to the increase in load from 80 to 200 nN respectively.
The pattern described in this Section shows the time and length of the first slip.
There is an increase in the early elastic regime due to increased load ranging from the 40
58
to 200 nN. The relationship between the elastic deformation regimes with respect to
The friction signal data was obtained from the AFM at a sampling frequency of
17.4 KHz. Windowing of this friction signal data is carried out using Hilbert transform at
a frequency range of 12-23 Hz. Frequency of the friction signal data is varied as a
function of the phase of the signal and provides high spectral representation. Windowed
friction signal data represents the continuous sliding and random stick-slip as represented
in the Figure 28. For 58 ms (11.61 nm) of friction signal data, the tip has scanned a
length of 11.61 nm on the silver coated PZT. In this 11.61 nm of distance covered; 11 13
Å of the sliding has continuous sliding and 91 Å of sliding has random stick-slip behavior
as shown in Figure 28. Continuous sliding and random stick-slip represents the region of
59
Stick
Slip
Figure 28. Continuous sliding and random stick-slip at a load of 40 nN and a band
pass frequency of 12-23 Hz.
The length of early elastic deformation regime as shown in Figure 26 and Figure 27 is
calculated and plotted with the increasing load. Cubic relation between the elastic
deformation regime and load due to curve fitting is shown in the Figure 28.
X = load in nN
60
Figure 28. Elastic regime vs. load.
During scanning, magnitude of the dissipated or interfacial energy (ET) and the
energy for plastic deformation (Ep) is calculated by the equation (14. a.) and (14. b.)
…………………………… (14. a. )
ET Fx * L * N
EP H *Vwear …………………………… (14. b. )
The linear relationship between the interfacial energy and load is given in the
Figure 29.
61
Table IX. Variation of interfacial energy with respect to increasing load.
40 2. 048
80 4. 096
120 6. 144
160 8. 192
200 10. 24
y = 0. 051*x - 1. 5e-015
4.2 Coating
62
The methods of FNP coating, FNP+ZnO mixing and coating was described
earlier. Results on the geometric structure of the FNP cones and verification of the ZnO
The magnetic field strength is higher than surface energy of the ferrofluid and
hence, the ferrofluid with ferrous nanoparticles form cones along the applied magnetic
field. The ferrous cones are at equidistance and form an array as shown in Figures 30 and
32.
63
Figure 31. Array of ferrous cones.
The array of ferrous cones at the macro scale is the magnified image of the
ferrous cones at nanoscale. These ferrous cones act as a low source of electron and
contribute to the flow of charges on the PZT surface. The significance of this equidistant
In Section 3.2.1 the method used in mixing of the ZnO in ferrofluid is explained.
Fluroscene microscope (FM) is used to verify the presence of ZnO nanoparticles in the
ferrous cones. The FNP cones and (FNP+ZnO) cones were exposed to ultraviolet rays
for 20 min. The ferrous nanoparticle cones with the ZnO nanoparticles are shown in the
Figure 32; the tip of the ferrous cones acts as the region of charge concentration and a
low source of electrons. Figure 33 shows the emission of light from the (FNP+ZnO)
cones due to the distribution of the ZnO nanoparticles on the surface. FNP cones after 20
min of UV rays exposure, produced a dark picture. Qualitative analysis showed presence
64
of the ZnO nanoparticles in FNP cones due to the mixing procedure followed in Section
3.2.1.
Figure 32. Array of ferrous nanoparticle and ZnO nanoparticle mixed cones.
Figure 33. Shows the light emitted by the (FNP+ZnO) cones exposed to an UV light
of wavelength 130 nm.
65
The intention of the ZnO coating on the FNP was to produce more charges due to
the piezoelectric property and thus control the flow of charges in the FNP cones due to its
semiconducting ability.
The above Section explains the advantages of the FNP coating and ZnO+FNP
coating in the field of charge conduction. In this Section we analyze the advantages of
these coating on the PZT in the field of power harvesting where the magnetic and
PZT.
When the PZT glued aluminum was excited at 90 Hz, the voltage generated was
51.1 mV. The magnitude of the voltage at a frequency 90 Hz is shown in Figure 34.
66
Figure 34. The magnitude of the voltage (51. 1 mV) at an excitation frequency of 90
Hz for a plain PZT.
FNP coated PZT glued aluminum was excited at 90 Hz and the voltage generated
was 115.4341 mV. This is due to the additional electron source on the surface and may
Figure 35. The magnitude of the voltage (115.1 mV) at an excitation frequency of 90
Hz for a FNP coated PZT.
When the (FNP+ZnO) coated PZT glued aluminum was excited at 90 Hz, the
voltage generated was 366.8 mV. This is due to the additional piezoelectric effect on the
PZT surface by the ZnO in the ferrofluid coating. ZnO also acts as an additional source
67
of electrons, due to its ability to emit charges at room temperature. The magnitude of the
Figure 36. Represents the magnitude of the voltage (366.8 mV) at an excitation
frequency of 90 Hz for a FNP +ZnO coated PZT.
All the above results are plotted in the Figure 37. It shows the increase in voltage
response of the PZT due to the nanoparticle coatings. This increase is due to the
magnetoelectric effect or increase in the capacitance of the silver coated PZT (P-5E) due
68
Voltage response vs. coatings on the PZT
400
350
300
Voltage 250
response 200
(mV) 150
100
50
0
1 2 3
1=Plain PZT; 2=FNP coated PZT;
3=FNP+ZnO coated PZT
CHAPTER V
CONCLUSIONS
1. The importance of High Speed Data Capture (HSDC) in the AFM was
region of high and low intensity of friction with respect to time. There
to 200 nN.
3. At low load the friction on the silver coated PZT is high to the surface
force effects.
69
4. Relationship between Interfacial energy and load shows an exponential
relationship.
information:
(P-5E).
defects at atomic scale, during the tip sliding on the silver coated
PZT surface.
event with increase in the load. The reason for this behavior has
yet to be analysed.
Florescence Microscope.
8. An equidistant array of ferrous cones and ferrous cones with ZnO coating
of the FNP coating and (FNP+ZnO) coating on the PZT. Results, show
70
that (FNP+ZnO) coating on the PZT and FNP coated PZT has better
CHAPTER VI
to identify the polarized regions over a given area. This will give the
71
3. Experiments have to be conducted to study the hysterisis behavior of the
FNP coated PZT and analyse the effect of remanent polarization on the
plain PZT and FNP coated PZT. Studies on the change of crystal
conducted.
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