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Abstract
Zinc Oxide Thin Film is a promising piezoelectric material. The piezoelectric zinc oxide (ZnO) thin film was
deposited using dielectric (RF magnetron) sputtering method. The crystalline structures, surface roughness
(morphology) and charge reversal of ZnO film were evaluated by X-ray Diffractometer (XRD), scanning electron
microscopy (SEM) and atomic force microscopy (AFM), respectively. It was found that the deposited ZnO film has a
preferred ZnO (002) orientation and the c-axis is perpendicular to the substrate surface. The grain size in the ZnO thin
film was found to be of the order of 35-40 nm, with a columnar structure. This novel ZnO thin film microcantilever
was fabricated by micromachining technique and wet etching of Si (TMAH) to release the cantilever. The functioning
of the released device was tested by the Laser Doppler Vibrometer (Polytec MSA-500) using variation in applied
voltage. The transverse piezoelectric coefficients d 31 of the ZnO film, obtained from the deflection of the cantilever
with influence of applied voltage, was calculated as 2.87 pC/N. The observed dynamic characterization of the novel
piezoelectric microcantilever had linear response with the applied driving voltage. The obtained values of Young
Modulus and Hardness are 208±4 GPa and 4.84± 0.1 GPa respectively. This microcantilever may be used to fabricate
the smart slider with inbuilt sensor/actuator and energy scavengers for replacing traditional batteries (In wireless
sensors network) with low resonant frequency and high power output.
With advancement in technology, the power demand novel ZnO thin film microcantilever energy scavenger
of individual devices has drastically come down. using the simple and inexpensive wet etching method.
Therefore energy scavenging method which is used to To convert electrical power into mechanical energy, i.e.
convert vibration energy into useful output electrical force and displacement, the converse piezoelectric effect
power has been observed as a promising solution. This has been utilized in piezoelectric cantilever actuators.
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1
Typical applications of piezoelectric cantilever actuators flexibility in processing ZnO thin films can be deposited
includes, ultrasonic motors, explosive detectors, probe at room temperature with varieties of acidic etchants are
tips of atomic-force microscopy (AFM), hard disk drives also available [5]. ZnO is an n-type semiconductor with
suspensions, nanodevices like sensors and power a wide direct band of 3⋅3 eV (at room temperature) good
generators, with ease and flexibility in operation [1–2]. electron transporting properties and solution-based
Piezoelectric materials are perfect candidates for processibility at low work function [6, 7, 8]. It has a
harvesting power from ambient vibration sources. hexagonal quartzite structure and large excitation
Among the variety of available piezoelectric materials, binding energy of 60 meV which makes ZnO a potential
the most popularly used material is lead zirconate material to realize the next generation MEMS and UV
However, poor stability, loss of polarization with The fabrication and characterization of ZnO thin film
continuous usage is the major issues with PZT. Their cantilever has been reported over past decade in many
piezoelectric properties are also strongly affected by research papers. They fabricated with the use of Deep
operating temperatures and due to brittleness they Reactive ion etching (DRIE) to release the cantilever.
cannot be deformed mechanically for long duration. The fabrication of ZnO cantilever with wet etching
Zinc oxide (ZnO) is another important piezoelectric method is difficult due to sensitivity of ZnO for wet
material which is popularly used as one of the pollution- etching and treatment by temperature, acid bases and
free piezoelectric material and is free from limitations even water [9, 10]. Therefore a novel method was
found with PZT. ZnO is highly tensile and may undergo developed for the successful fabrication of ZnO based
huge mechanical deformations for a long duration MEMS devices. The V-grooves in the Si wafer were
without the effect of temperature variation. Therefore it created by TMAH wet etching before deposition of ZnO
has received increased attention for various Micro layer on substrate [11]. The SEM images of the fully
Electro Mechanical Systems (MEMS) device fabricated ZnO cantilever are shown in Fig. 1. A laser
applications [3]. Due to the unique combinations of Doppler Vibrometer [LDV] Polytec MSA-500 was used
electrical, optical and piezoelectric properties of ZnO, it to measure the dynamic response of the piezoelectric
detectors, and light emitting diodes (LEDs), also it can 2. Modelling and Design
be easily integrated with other processes and materials. The most popular approach to design the
than that of PZT [4] but has the additional advantage of evenness of moments and forces and the compatibility
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condition of strain at the piezoelectric and elastic Where, L, M, I and E are the length of the beam, mass
material interface by solving the consecutive equations per unit length area, moment of inertia and Young’s
[13,14]. The actuation force can be calculated with the modulus, respectively [15]. Per unit length equivalent
use of equivalent force and deflection relationship at the mass M for the piezoelectric micro cantilever is given
The resonant frequency of the cantilever can be microcantilever, which consists of two materials, its
obtained with the solution of eigen value problem of the cross section can be converted into the corresponding
fourth-order ordinary differential equation in space. The cross section of a single material by the transformed-
fundamental resonant frequency f0 of a beam which is section method [19]. The equivalent flexural rigidity EI
free at one end and fixed at the other end may be given can be calculated by
by [17, 18]. W
EI
12 Esubt sub Et t p
.1615
f0 2
L E t
sub sub E pt p tsub sub t p p
(1)
(5)
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The tip deflection δ is [17] Corporation of America (RCA) method. The Si substrate
3L2t sub (t p tsub ) Esub E pVd31 used was p-type conducting (0.0001-0.0005 Ω cm). The
l
E p2t 4p Esub
2 4
t sub 2 E p t p Esubt sub 2t sub
2
2t 2p 3t p t sub 1 µm SiO2 layer was grown on Si wafer by wet thermal
The tip deflection δ(l) and resonant frequency f 0 are the process of TMAH etching of Si [5]. The deposited
the functions of the piezoelectric cantilever dimensions. SiO2 layer is patterned by lithography and BOE etching.
Equations (1 & 8) show, that the width w does not affect For TMAH etch of Si wafer (shallow or deep) 25%
the resonant frequency and the tip deflection under any TMAH with water was used. The quantity of, TMAH
external load condition. Under the consideration of and water in the mixture were 90 ml and 30 ml
external load F, the driving voltage required for a certain respectively [10]. Further ZnO thin films were deposited
tip deflection δ is inversely proportional to the width w. by dielectric sputtering method using a ZnO target
A wider cross section of the piezoelectric cantilever is (99.9%) with a 2 inch diameter and 3 mm thickness.
preferred for lower less power consumption. The effect During the deposition of ZnO thin film the RF power
of length L can be easily seen from equations (1) and was 100 W, the base pressure was 5×10 -5 mbar and
(8). The resonant frequency decreases parabolically with operating pressure was 2.2×10-2 mbar. Thin films were
L, while the tip deflection increases parabolically with L deposited in Ar atmosphere with a deposition rate of 5
[23] are listed in table-1 and the design parameters for The Piezoelectric ZnO microcantilevers were
the piezoelectric ZnO microcantilever are listed in table- fabricated by micromachining process and patterned by
The ZnO microcantilevers were fabricated with cantilevers were fabricated with novel Wet Chemical
novel wet etching and lift off method. Tetramethyl method (such method reported first time). The substrate
ammonium hydroxide (TMAH) is an anisotropic silicon was p-type silicon (100) wafer on which a 1 μm
etchant. The side walls of the etched Si were defined by thickness of silicon dioxide (SiO 2) was deposited using a
the (111) planes. The angle between the (100) plane and wet thermal oxidation method. At the outset the V-
sidewalls of etched Si was 54.7º as depicted in Fig. 3. groove was created with the depth of 150 µm on silicon
The complete process flow of releasing cantilevers is wafer. Then SU-8 2100 of 150 µm thickness was
illustrated in Fig. 4. The process flow starts with spinned on the wafer and the scraper was used to put the
cleaning of silicon wafers by standard Radio SU-8 uniformly. Now SU-8 covered Silicon wafer was
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placed on the heater, to remove the bubbles and to shown in Fig. 6 and the thickness of the ZnO film is
smooth the surface by heating. Finally, wafer was about 0.3 μm. It clearly indicates that the grown ZnO
dipped in SU-8 developer to the process the SU8 [24, thin film in the cantilever is polycrystalline and
25]. columnar texture, which also confirms that the ZnO film
The fabrication process containing the sequence of is highly c-axis preferred orientation and therefore has
steps is shown in Fig. 4. hexagonal crystal. Further, Fig. 7 and Fig.8 show atomic
Therefore complete microfabrication process of the force microscope (AFM) images of ZnO thin film with
micro cantilever mainly included successive etching of 500 nm scan area and 30 nm scanning height. Fig. 8
Si and ZnO thin film, top electrode deposition and shows there is a clear charge reversal when sample bias
patterning. The Hysitron, Inc Minneapolis USA make is changed from positive 5000 mV to negative bias. The
nanoindenter model TI-900, were used for measurement SEM images of the fully fabricated ZnO cantilever are
of Young Modulus and Hardness of ZnO thin films. shown in Fig 1, which clearly illustrates that the
4. Results and Discussions fabricated device is stable and maintains its freestanding
X-ray from Rigaku (Cu-K radiation, state without structural deformations. The dimension of
=1.5405 Ǻ) was used for structural phase the ZnO microcantilever is about 500 × 100 μm2.
identifications. The XRD pattern in Fig.5 indicates that The above explained characterizations of the ZnO
the deposited ZnO film has high diffraction peak located thin film and the ZnO microcantilever were just done to
at around 34.4220 is very high and which is equivalent to see the quality of the film. In reality, the most desirable
the ZnO (002) peak. So the deposited ZnO thin film on parameter for the ZnO piezoelectric film is to observe its
the Si substrate has a c-axis preferred orientation, which high piezoelectric performance. So in the following
is an essential condition for good piezoelectric quality. experiment, to measure the dynamic response of the
The depth of the etching of Si was assessed by ZnO microcantilever first LDV (Laser Doppler
profilometer (Ambios, USA). The measured depth of the Vibrometer) was used, and then the transverse
V-groove in Si wafer was 160 μm. To determine the piezoelectric constant d31 of the ZnO film was calculated
grain morphology of ZnO film, Scanning electron using the obtained data [26]. The obtained values of
microscopy (SEM) was done using Raith150. SEM and Young Modulus and Hardness in GPa units with respect
profilometer were also used to find the uniformity and to penetration depth in nm is plotted in the Fig.9. The
the thickness of ZnO films with granular structure. approximate values of Young modulus of ZnO film is
The surface morphology of the fabricated ZnO 208±4 GPa and hardness as a function of penetration
microcantilever was measured by SEM Raith 150 two as depth is 4.84± 0.1 GPa. These obtained values of
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Young’s modulus and hardness are almost constant resonant frequency of the microcantilever actuator was
indicates that effect of substrate is not meaningful for measured by an impedance analyzer (Agilent 4294A)
To evaluate the performance of the fabricated sensitivity, bandwidth and nonlinearity were observed.
piezoelectric microcantilever actuator, characterization Fig.12 shows the cantilever’s tip velocity magnitude
was done by Polytec MSA 500 laser Doppler vibrometer curve as a function of input vibration frequency. It has
(LDV) [21]. The experimental setup is shown in Fig. 10 been observed that the resonant frequency of the
and 11. The dynamic response of the fabricated ZnO microcantilever is 72,312 Hz. When a sine wave signal
microcantilever was captured using LDV, and then the was applied (AC voltage) by the probe station on the
tested data is analyzed and transverse piezoelectric bottom and top electrodes of the ZnO microcantilever, in
constant d31 of the ZnO film was calculated. accordance to piezoelectric effect the cantilever
RF function generator (Agilent 33120A) was used to generates vibration. These vibrations of the cantilever
supply the driving voltage and deflection of the were detected by the LDV and the velocity and
cantilever’s tip is measured by the Polytec-500 micro displacement of the cantilever were measured. The plot
system analyzer (LDV). Driving voltage and tip of the driving voltage versus measured amplitude of the
deflection signals are processed by a dual channel FFT cantilever tip is given in Fig. 13. In this measurement,
spectrum analyzer through data analysis and evaluation the driving voltage frequency was fixed at 10 kHz. From
signal processing software Intuitive 8.8 (PSV 8.8). The Fig. 13, it was observe that when the driving voltage
package of PSV data acquisition software has an increases from 1 to 15 V, the amplitude of the ZnO
analyzer of high featured in time domain. For a variety cantilever tip increased from 4.8 to 62 nm. It has been
of input wave forms it provides Zoom Fast Fourier observed that amplitude of the cantilever tip increases
transform (FFT), averaging and peak hold linearly with the driving voltage.
measurements. Its high resolution data visualization in For a bimorph piezoelectric cantilever structure
three dimensions (3D) includes full frequency response included one piezoelectric layer and one elastic layer, if
(FRF), deflection shape (ODS) and function of both of them have same width, the tip deflection δ(l) of
operational capabilities. At the input, sinusoidal the cantilever may be expressed a equation 8 [27,28].
waveforms of different driving voltages are applied and Where, L is the length of the cantilever i.e. distance
corresponding time responses were investigated. A wide from fixed end; δ(l) is the deflection; t p and tsub are the
band amplifier 7802 M also integrated with system for thicknesses of both piezoelectric and elastic layers (Si
proper amplification of the detected signals. The substrate), respectively and Ep and Esub are the Young’s
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modulus of their materials, respectively; V is the applied transverse piezoelectric constant d31 of deposited ZnO
voltage; and d31 is the transverse piezoelectric constant film is little smaller than that of the ZnO bulk material,
of the piezoelectric material. In this device, since the but it is still high in comparison to other published
conducting Si, and by TMAH etching out of the Si from Further, it will also intrusting to investigate the
the substrate, therefore only the thickness of ZnO film piezoelectric properties of the microcantilever harvester,
has been considered. Owing to the large volume of the fabricated using the ZnO film integrated with another
material it is easy to measure the mechanical properties multifunctional multiferroic thin films in order to
of the Si substrate and the properties are also stable. enhance the properties.
properties is difficult due to small volume. Using the This research paper deals with the fabrication and
criteria of linear dependency of the deflection on the characterization of ZnO piezoelectric microcantilevers
applied voltage, the piezoelectric coefficient d 31 of the by the simple and inexpensive wet etching method. The
ZnO can be calculated by the use of equation 7[28,29, ZnO film was deposited on conducting p-type Si
All the parameters except d31 are known for our temperature. XRD pattern clearly explains that the
fabricated ZnO microcantilever, L is the length of the deposited ZnO film has a desirable c-axis-preferred
cantilever which is 500 μm, tp is 300nm, tsub is 300 nm, orientation, and the normal grain size of the ZnO film
Ep is 2.1 × 1011 Pa, and Esub is 1.9 × 1011 Pa. δ(l) and V was found approximately 35.48 nm.
can be obtained from Fig. 13 therefore, the d 31 of the The AFM image showed that the ZnO thin film has
ZnO thin film was calculated using equation 7. very uniform surface, and the roughness of surface was
The calculated d31 of the ZnO film for the different 5.687 nm. The SEM images at different magnification
values of driving voltages is shown in figure 13. From confirmed that the ZnO film grows columnar, and the
Fig. 13, it has been observed that the transverse direction is perpendicular to the surface. The ZnO film
piezoelectric constant d31 of the ZnO film remains piezoelectric microcantilever was fabricated by wet
constant regarding the variations in different values of etching techniques. Its dimension is about 500 × 100 × .
driving voltages. The average calculated value of d31 is 3 μm3. The obtained values of Young Modulus and
-2.87 pC/N, which is almost in the same order as that of Hardness are 208±4 GPa and 4.84± 0.1 GPa
the ZnO bulk material. The value of d 31 for bulk respectively. These obtained values of Young’s modulus
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7
and hardness are nearly constant indicates that effect of
References
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Acknowledgement Kun Shyong Chowa, Mingsheng Zhangb,
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Email: dbhatia@rtu.ac.in
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FABRICATION STEPS
(1) (2)
(3) (4)
(5) (6)
(7) (8)
PPR layer spinning for Lift-Off PPR Patterning by lithography and Neg. Mask
(13) (14)
(15) (16)
Color Scheme for Figure 4
Lift off Cr/Au and ZnO SU-8 2100 removal by PG remover at 70oC
Figure 4. Fabrication steps used in the fabrication of Piezoelectric ZnO microcantilevers.
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Figure 5. X-ray diffraction pattern obtained of ZnO film grown on Si substrate
Figure 6. SEM image of ZnO Layer at different magnification (a) Inset shows the image at 100 nm (b) at 200 nm
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Figure 7. AFM (Topography) Images of ZnO thin films of 300nm for scan height30 nm (a) 2 D view(b) 3D
View.
Figure 8. AFM (Topography) Images of ZnO thin films of 300nm for scan area 500 nm at bias (a) 5000mV (b)-5000mV.
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Figure 9. Hardness and Young Modulus of ZnO film with Penetration Depth
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Camera
Optics
LDV
RF Generato
Amplifier
Figure 10. LDV (Laser Doppler Vibratometer) setup used for the characterization of piezoelectric ZnO-microcantilever.
Cantilever
Fig.11. LDV (Laser Doppler Vibratometer) FEM and FFT setup for characterization of the piezoelectric ZnO microcantilever.
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Figure 12. The cantilever’s tip velocity magnitude variations with input vibration frequency.
RF Generator
Figure 13. Cantiliver tip’s measured amplitude and d 31 of ZnO thin film v/s Voltage applied on
microcantilever (measurement was taken on driving AC voltage frequency 10 kHz).
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List of figures
Figure 1. SEM image of fabricated ZnO microcantilever.
Figure 2. Cantilever deflection mechanism
Figure 3. Side Profile of TMAH etching of Si (Anisotropic etching)
Figure 4. Fabrication steps used in the fabrication of Piezoelectric ZnO microcantilevers.
Figure 5. X-ray diffraction pattern obtained of ZnO film grown on Si substrate
Figure 6. SEM image of ZnO Layer at different magnification (a) at 100 nm, (b) Inset shows the image at
200 nm.
Figure 7. AFM (Topography) Images of ZnO thin films of 300nm for scan height30 nm (a) 2 D view(b) 3D
View.
Figure 8. AFM (Topography) Images of ZnO thin films of 300nm for scan area 500 nm at bias (a) 5000mV
(b)-5000mV.
Figure 9. Hardness and Young Modulus of ZnO film with Penetration Depth
Figure 10. LDV (Laser Doppler Vibratometer) setup used for the characterization of ZnO piezoelectric
Znmicrocantilever.
Figure 11. LDV (Laser Doppler Vibratometer) FEM and FFT setup for characterization of the
piezoelectric ZnO microcantilever.
Figure 12. The cantilever’s tip velocity magnitude variations with input vibration frequency.
Figure 13. Cantiliver tip’s measured amplitude and d 31 of ZnO thin film v/s Voltage applied on
microcantilever (measurement was taken on driving AC voltage frequency 10 kHz).
Table- 1
The basic properties of materials Zinc Oxide and Silicon
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Table -2
Design Parameters for the piezoelectric ZnO microcantilever.
ZnO thin film microcantilever energy scavenger by simple and inexpensive wet etching method.
Novel method of Fabrication.
Obtained values of Young’s modulus and hardness are nearly constant for indentation depth.
The transverse piezoelectric coefficients d31 is much higher compared and nearly closed to the ZnO bulk material.
Integration with multifunctional multiferroic film enhance the piezoelectric properties and output voltage.
Cover Letter from the authors
To
The Editor
Nano Structures and Objects, Elsevier
Dear Sir,
We are submitting a manuscript titled “Fabrication and characterization of a novel zinc oxide thin film
piezoelectric microcantilever with wet etching and lift off methods” by Deepak Bhatia et al. for publication in the
Nano Structures and Objects, Elsevier.
Our paper belongs to the area of fabrication and characterization of a novel zinc oxide thin film piezoelectric
microcantilever with wet chemical process is being reported. Recently a great interest has been developed to
complete the requirement of self powered sensors/electronics by using renewable energy sources or energy
scavengers to replace traditional batteries. Therefore energy scavenging method which is used to convert vibration
energy into useful output electrical power has been observed as promising solutions. The fabrication and
characterization of ZnO film cantilever in the past decades were reported in many research papers. They fabricated
with the use of Deep Reactive ion etching (DRIE) to release the cantilever. The fabrication of ZnO cantilever with
wet etching method is difficult due to sensitivity of ZnO for wet etching and treatment by temperature, acid bases
and even water. Therefore need was felt to develop a novel method for the successful fabrication of ZnO based
MEMS devices. The V-grooves in the Si wafer were created by TMAH wet etching before deposition of ZnO layer
on substrate. The piezoelectric zinc oxide (ZnO) thin film was deposited using dielectric (RF magnetron) sputtering
method. The crystalline structures, surface roughness (morphology) and charge reversal of ZnO film were evaluated
by X-ray Diffractometer (XRD), scanning electron microscopy (SEM) and atomic force microscopy (AFM),
respectively. The deposited ZnO film has a preferred ZnO (002) orientation and the c-axis is perpendicular to the
substrate surface. The grain size in the ZnO thin film was found to be the order of 35-40 nm and has a columnar
structure. This novel ZnO thin film microcantilever was fabricated by micromachining technique and by wet etching
of Si (TMAH) to release the cantilever. The functioning of the released device was tested by the Laser Doppler
Vibrometer (Polytec MSA-500) using variation in applied voltage. The transverse piezoelectric coefficients d 31 of
the ZnO film, obtained from the deflection of the cantilever, with influence of applied voltage was calculated as 2.87
pC/N. The observed dynamic characterization of the novel piezoelectric microcantilever had linear response with the
applied driving voltage. The observed dynamic characterization of the novel piezoelectric microcantilever shows
linear response with the applied driving voltage. Some of the Physics issues in this regard also not fully understood.
Our results add an important understanding to the concept of the microcantilevers harvester and enable to
fabricate energy scavengers to replace traditional batteries (for wireless sensors network) with low resonant
frequency and high power output which is a topic of intense experimental and theoretical research at present due to
its potential applications. To enhance the piezoelectric properties of deposited films and output voltage generated by
the microcantilever harvester it is proposed to integrate the ZnO film with another multifunctional films. The
generated energy also in consideration to store, and the relative experiments are ongoing will be reported in soon.
We are sure that this paper will be well appreciated by the readers of Nano Structures and Objects, Elsevier
Thanking you
Yours sincerely,
Deepak Bhatia
Department of Electronics Engineering, Rajasthan Technical University, Kota and
Department of Electrical Engineering and Centre for Excellence in Nanoelectronics,
Indian Institute of Technology Bombay,
Mumbai-400076,
Cell:+91-9461513242, +91-9414317401
Email: dbhatia@rtu.ac.in, keshav_eck26@yahoo.com