materials

Article
Graphene/PVDF Nanocomposite-Based Accelerometer for
Detection of Low Vibrations
Surendra Maharjan, Victor K. Samoei and Ahalapitiya H. Jayatissa *

Nanotechnology and MEMS Laboratory, Department of Mechanical, Industrial, and Manufacturing Engineering (MIME),
The University of Toledo, Toledo, OH 43606, USA
* Correspondence: [email protected]

Abstract: A flexible piezoresistive sensor was developed as an accelerometer based on Graphene/PVDF

nanocomposite to detect low-frequency and low amplitude vibration of industrial machines, which
may be caused due to misalignment, looseness of fasteners, or eccentric rotation. The sensor was
structured as a cantilever beam with the proof mass at the free end. The vibration caused the proof
mass to accelerate up and down, which was converted into an electrical signal. The output was
recorded as the change in resistance (response percentage) with respect to the acceleration. It was
found that this accelerometer has a capability of detecting acceleration up to 8 gpk-pk in the frequency
range of 20 Hz to 80 Hz. The developed accelerometer has the potential to represent an alternative to
the existing accelerometers due to its compactness, simplicity, and higher sensitivity for low frequency
and low amplitude applications.

Keywords: flexible piezoresistive sensor; proof mass; low-frequency; accelerometer

1. Introduction
Microelectromechanical system (MEMS)-based accelerometers have gained demand
in different applications since piezoresistive-based MEMS accelerometers were first used
in the automotive industry in 2000 for car suspension systems and airbags systems. Ac-
celerometers measure the mechanical stimulation of a device in single or multiple axes
Citation: Maharjan, S.; Samoei, V.K.; in terms of acceleration, vibration, shock, and tilt and convert them into electrical signals.
Jayatissa, A.H. Graphene/PVDF MEMS accelerometers are one of the highly efficient sensors [1] that lead to their expansion
Nanocomposite-Based Accelerometer in a multitude of a branch of science. For instance, several applications of accelerometers
for Detection of Low Vibrations. are navigation systems of the aerospace and aviation industry, stabilization of unmanned
Materials 2023, 16, 1586. https:// aerial vehicles (UAVs), detection of industrial vibration of machinery, display adjustment of
doi.org/10.3390/ma16041586 smart devices, bioengineering to detect subtle vibrations in rehabilitation [2], and activity
Academic Editor: Daping He tracking [3].
Based on the working mechanisms, MEMS accelerometers are categorized into piezore-
Received: 12 January 2023 sistive, piezoelectric, capacitive, tunneling, optical, and thermal types. However, piezore-
Revised: 7 February 2023
sistive accelerometers hold simple circuit configuration, low power consumption, and fast
Accepted: 10 February 2023
frequency response that enhances their importance among others. The gauge factors of
Published: 14 February 2023
most piezoresistive metals and semiconductors used in the strain gauges are around 2.
They are highly anisotropic for semiconductors due to the crystal orientation, dopant type,
and carrier concentration [4,5]. Polymer/elastomer-based MEMS accelerometers have
Copyright: © 2023 by the authors.
advantages such as ease of manufacturability, flexibility, simple configurations, optical
Licensee MDPI, Basel, Switzerland. transparency, and cost-effectiveness, which made them popular over metal and semicon-
This article is an open access article ductor accelerometers. The conductive materials such as graphene, carbon nanotubes, and
distributed under the terms and metal particles are coupled with polymer/elastomer substrates such as PE, PMMA, PVA,
conditions of the Creative Commons PDMS, and ABS to make flexible sensor devices.
Attribution (CC BY) license (https:// Detection of low-frequency vibrations is crucial in many applications. Vibrations
creativecommons.org/licenses/by/ in large rotating machinery, oil pipes [6], bridges, buildings, pillars [7], and ground mo-
4.0/). tions caused by earthquakes, volcanic eruptions, explosions, landslides, tsunamis, and

Materials 2023, 16, 1586. https://doi.org/10.3390/ma16041586 https://www.mdpi.com/journal/materials

Materials 2023, 16, 1586 2 of 10

avalanches [8] hold a low frequency and low amplitude. Misalignment of components,
mechanical looseness (nut, bolt, and fastener), and unbalance (about a central axis) are the
main causes of vibrations in machines, which can cause lethal damage if not detected and
maintained at the appropriate time. Accelerometers should have high sensitivity and relia-
bility for such measurements. Nowadays, different research is being conducted to explore
novel sensing materials, miniaturization techniques, sensitivity, reliability, and durability.
Table 1 depicts different types of accelerometers used for the detection of low frequency
and low amplitude vibrations. Piezoelectric (PZT) accelerometers have a wide bandwidth
and high sensitivity. Therefore, they are usually not applicable for low-frequency vibra-
tions. Because of their high stability and low price, strain gauge accelerometers are widely
used in industry. However, the accuracy is low to detect low-frequency vibrations. Fiber
Bragg Grating (FBG) accelerometers can detect the vibration of low frequency but their
resolution is limited. A MEMS accelerometer has a wide frequency response range and
quite better sensitivity and acceleration (g) range than the previous types. In addition to
the above technologies, Zheng et al. [9] developed a new maglev sensor that has a hybrid
magnet levitation structure with the supporting components of electromagnets and per-
manent magnets. This accelerometer can measure an ultra-low frequency (ULF) vibration.
A polysilicon-based piezoresistive MEMS accelerometer has been developed in recent
years [10]. It has a capability to detect different frequencies from 75 Hz to 475 Hz as sinu-
soidal signals. Polymer composite materials made of Poly (Vinylidene-Trifluoroethylene)
have been successfully used to develop an accelerometer, which has sensitivity in 20–50 Hz
range [11]. However, we did not find any report about development of piezoresistive
accelerometer based on Graphene/Polyvinylidene Fluoride (Gr/PVDF) composite.

Table 1. Summary of accelerometers for low vibration detection.

Principle Sensitivity (V/g) Range (g) BW (Hz) Ref.

9 mV/g – – Tian et al. [12]
PZT 15.6 mV/g – 60–1.5 k Nishshanka et al. [13]
2.82 – 2–500 Tims et al. [14]
Strain - 0–5 <100 Kamentse et al. [15]
0.135 0.1–2 80–800 Gao et al. [16]
FBG
0.362 <0.5 1–10 Zhang et al. [17]
2 ±1 0–50 Swartz et al. [18]
MEMS 1 ±2 0–50 Cho et al. [19]
1.2 ±3 0.2–1500 Sabato et al. [20]
Others - - 0.2–0.4 Zheng et al. [9]

In this study, a piezoresistive MEMS accelerometer with a novel material having high
sensitivity, cost-effectiveness, and simple configuration, was developed for measuring
low-frequency and low-amplitude vibrations. Gr/PVDF composite was used as conduc-
tive material and was coated on a polyethylene (PE) substrate to develop this flexible
accelerometer [21]. The device was designed as a cantilever structure, which can vibrate
and generate a change in resistance. This accelerometer can be calibrated for frequencies
based on resistance change.

2. Sensing Mechanism
The piezoresistive accelerometer consists of a cantilever beam of substrate material
coupled with sensing nanocomposite, which holds the proof mass at the free end and the
other end supported by the fixed frame. This model has one degree of freedom and displace
in the direction normal to the sensor surface. When the sensor is subjected to acceleration, a
force equal to the product of mass and acceleration causes the proof mass to displace in the
Materials 2023, 16, 1586 3 of 10

direction normal to the sensor surface [1]. According to Newton’s second law of motion,
acceleration (a) is the function of displacement (x) of the proof mass and is given by [22],

a = f ( x ).
(1)
a = mk x,

where k and m are the spring constant and mass, respectively. The resistivity of nanocom-
posite at the sensor legs will change, which in turn changes the resistance. The final output
was taken as resistance change in this paper instead of voltage calculation to simplify circuit
configuration. Thus, the acceleration applied to the sensor can be calibrated in terms of
resistance change.
The change in resistance of the sensing material can be interpreted by the disconnection
mechanism. The disconnection process between the adjacent nanoflakes is caused by three
situations: contact area change, tunneling effect, and crack propagation. The change in
the contact area between adjacent nanoflakes is dominant when the applied pressure or
strain is small, and the electrons travel through the overlapped nanoflakes within the
percolation conductive network. As the applied pressure increases, the adjacent nanoflakes
pull apart and create a tunnel. However, electrons can pass through the tunnel due to very
small separation. This is called the tunneling effect, and the separation space is called the
tunneling distance. As the distance grows, so does the tunneling resistance. The distance at
which no electron passes through by tunneling is called the cut-off tunneling distance. The
tunneling resistance between two adjacent particles can be estimated by using Simmons’
theory [23].
h2 d 4πd √
 
Rtunnel = √ exp 2mλ (2)
Ae2 2mλ h
where A, e, h, d, m, λ represent the cross-sectional area of the tunneling junction, single-
electron charge, Plank’s constant, the distance between adjacent nanoflakes, the mass of
an electron, and the height of energy barrier for insulators, respectively. The third one
is crack propagation, which occurs when the applied pressure or strain is even higher.
Initially crack initiates and later propagates along with time and pressure conditions. The
separation of crack edges critically limits the electrical conduction. The sensors developed
in this thesis are based on the piezoresistive mechanism.

3. Experimental Method
3.1. Materials Preparation
Graphite particles were mixed with acetonitrile as a solvent in the ratio of 1.0 g: 20 mL [24].
Large particles of graphite were broken down by rod stirring in the solution before trans-
ferring to the ultra-sonicator. It was sonicated 4 times, each for 10 min, keeping an interval
of 10 min to prevent aggregation of graphite particles, which can be caused by temperature
rise during sonication. The solution was kept at steady condition in a long measuring
cylinder for a few hours (usually 12 h) to settle heavy particles at the bottom and 2.5 mL
of suspended graphene layer was taken to the small beaker [25,26]. It was estimated from
Raman spectroscopy and SEM images that 4–5 monolayer thick graphene is produced by
this method. To prepare PVDF solution, 50.0 mg of PVDF powder (Alfa Aesar, 99.99%) was
added acetonitrile and sonicated 2 times with the same procedure. Finally, graphene and
PVDF solutions were mixed and sonicated for 20 min to achieve a homogeneous Gr/PVDF
solution of the nanocomposite, which acts as the sensing element.
A thin and transparent flexible polyethylene sheet of thickness 0.1 mm was chosen as
the substrate. The substrate was cut into 10 mm × 10 mm size to design a sensor as shown
in Figure 1. The substrate was rubbed with sandpaper to better adhere the composite to the
surface and then rinsed with isopropanol to wash away any contaminants before applying
20–22 µm thick graphene/PVDF nanocomposite using a doctor blade method.
Materials 2023, 16, 1586 4 of 10

Figure 1. Accelerometer and experimental setup. (a) Top view and (b) side view of cantilever.

3.2. Design and Fabrication of Accelerometer

The sensor was designed as a cantilever structure (Figure 1) and one end of the sensor
was attached to the proof mass while the other end was attached to the vibrator using an
epoxy resin. The vibrator has a capability to produce different frequencies and amplitudes.
Some space was maintained to freely vibrate the free end of the sensor along with the proof
mass. The thin width legs of the sensor also support for ease of vibration. The vibration
was only in the direction normal to the sensor surface. Two-wire terminals were attached
to the sensor legs to record electrical signals using a Keithley Multimeter.

3.3. Resonance Frequency Calculation

The resonance frequency (f ) of the system is given by Equation (3) [27],

w2 n =qmk ,
1 k
(3)
f = 2π m.

The spring constant of the π-shaped structure follows the following equation [28].

Wb 3
 
1
k = Ets , (4)
2 Lb

where E is the Young’s modulus for PE substrate, Wb is the width of the beam, Lb is the
length of the beam, and ts is the thickness of the beam. The geometric parameters and
accelerometer characteristics are shown in Table 2. Using Equations (2) and (3), spring
constant and resonance frequency were found to be 56.7 N/m and 85 Hz, respectively.
 Table 2. Geometric parameters and accelerometer characteristics.

Parameters Symbols Values

Length and width of the spring beam W b × Lb 1.5 mm × 10 mm
Mass m 0.2 g
Materials 2023, 16, 1586 5 of 10
Young’s modulus E 1.08 X 109 Pa
Thickness of beam ts 105 µm
Table 2. Geometric parameters and accelerometer characteristics.
4. Result and Discussion
Parameters Symbols Values
4.1. Acceleration Response
Length and width of the spring beam W b × Lb 1.5 mm × 10 mm
The
Mass device was placed in a vibrator m as shown in Figure 1. 0.2One
g end of the device was
fixedYoung’s
to the modulus
vibrator and the other end was E kept free. The device 1.08 was
× 109excited
Pa with a sinus
oidalThickness
loadingofand beamthe rectangular proof tmass s
at the free end oscillates
105 µm up and down, which
is perpendicular to the sensor surface. The acceleration of the vibration was measured
with4.respect to time.
Result and It was found that the sensor could measure the acceleration up to 8
Discussion
gpk-pk4.1.
(peak to peak).
Acceleration For a representative case, a frequency of 30 Hz and amplitude from
Response
−6 dB toThe −3 device
dB was was placed for
chosen in athe excitation
vibrator as shownof the device.
in Figure The end
1. One results are
of the depicted in
device
Figure
was2, which
fixed to theindicates
vibrator that theother
and the deviceendcould convert
was kept free. a vibrational
The device wassignal
excitedinto
withaccelera
tion.a sinusoidal loading and the rectangular proof mass at the free end oscillates up and
down, which is perpendicular to the sensor surface. The acceleration of the
Controlling the acceleration of the vibration, the frequency was varied, and three rep vibration was
measured with respect to time. It was found that the sensor could measure the acceleration
resentative cases were studied. Acceleration was kept at 2 gpk-pk and frequency was set to
up to 8 gpk-pk (peak to peak). For a representative case, a frequency of 30 Hz and amplitude
20 Hz,
from30−Hz,
6 dB and
to −340dBHz.
wasTime
chosenresponses of acceleration
for the excitation of the device.atThe
three representative
results are depicted infrequen
ciesFigure
were 2,recorded by the device as shown in Figure 3.
which indicates that the device could convert a vibrational signal into acceleration.

FigureFigure
2. Results of acceleration
2. Results measurement
of acceleration at at
measurement 3030Hz
Hzand
andamplitudes from−-6
rangingfrom
amplitudes ranging dBtoto -3 dB.
6 dB
−3 dB.

Controlling the acceleration of the vibration, the frequency was varied, and three
representative cases were studied. Acceleration was kept at 2 gpk-pk and frequency was
set to 20 Hz, 30 Hz, and 40 Hz. Time responses of acceleration at three representative
frequencies were recorded by the device as shown in Figure 3.
Materials 2023, 16,
Materials x FOR
2023, PEER REVIEW
16, 1586 6 of 10
6 of 10

Figure 3. Time
Figure response
3. Time responseof
ofacceleration atthree
acceleration at threerepresentative
representative frequencies.
frequencies.

4.2.4.2. Resonance
Resonance
The resonance frequency was calculated theoretically and was found to be 85 Hz.
The resonance frequency was calculated theoretically and was found to be 85 Hz.
Usually, the MEMS accelerometer works below the resonance frequency. The lower limit
Usually, the MEMS accelerometer works below the resonance frequency. The lower limit
of the vibration generator is 20 Hz, which is the lower possible limit of the device. The
of the
devicevibration generator
was excited with a is 20waveform
sine Hz, which is the
signal lower
with possible
a variable limit of
frequency the device.
ranging from The
device
20 to 80 Hz with an interval of 10 Hz. From 20 Hz to 60 Hz, data were collected for higher from
was excited with a sine waveform signal with a variable frequency ranging
20 to 80 Hz with
amplitude an interval
(−5 dB) whereas,of for10
70Hz. From
Hz and 80 20
Hz,Hz to were
data 60 Hz, data were
recorded collected
at smaller for higher
amplitude
amplitude
(−9 dB). (−5WhendB)thewhereas,
amplitude foris70higher
Hz andat a80 Hz, data
higher were recorded
frequency, vibration at smallersoamplitude
becomes high
(−9that
dB).it When
damages thethe sensor. Figure
amplitude 4a presents
is higher the repeatability
at a higher frequency,curves in the experimental
vibration becomes so high
thatfrequency
it damages range
theover a certain
sensor. Figuretime
4aframe.
presentsThethehigher response at
repeatability 80 Hzin
curves wasthedue to the
experimental
proximity to the resonance. However, the data were displayed over 2
frequency range over a certain time frame. The higher response at 80 Hz was due to thes for each frequency
and each sinewave lies within the range. When the sensor was tested at 85 Hz, the vibration
proximity to the resonance. However, the data were displayed over 2 s for each frequency
of the proof mass was so high that the sensor was damaged. Even after multiple testing,
andtheeach sinewave
sensor could notlies within
read the range.
the data, When
validating the sensorresonance
the calculated was tested at 85 Hz, the vibra-
frequency.
tion of the proof mass was so high that the sensor was damaged. Even after multiple test-
ing,4.3.
theSensitivity
sensor could not read the data, validating the calculated resonance frequency.
The accelerometer was tested at a particular frequency varying the amplitude of the
excitation. Figure 5a presents the repeatability of the curve lying within the range over
a period and the data were displayed for 5 s for each amplitude. The highest sensitivity
of the accelerometer was found to be 21% g−1 at 30 Hz with a Pearson squared corre-
lation coefficient of R2 = 0.999, presented in Figure 5b. This means the response of the
accelerometer can reach up to 21%, when the system is excited with 1 gpk-pk at 30 Hz. The
response was carried out in terms of resistance change. It was found that the correlation
between acceleration and response (in terms of resistance change) is linear as the data
were also recorded for 40 Hz and 50 Hz. The response in resistance change simplifies the
circuit configuration.
 Materials 2023, 16, x FOR PEER REVIEW 7 o
Materials 2023, 16, 1586 7 of 10

Figure 4. (a) Repeatability

Figure 4. (a) test. (b) Response
Repeatability measurement
test. (b) at differentatfrequencies
Response measurement with a fixed
different frequencies with a fixed
amplitude of −5plitude
dB. of -5 dB.

The vibrations generated by machines can be dangerous if left unmarked as they

4.3. Sensitivity
can grow with time, leading to catastrophic damage to the system. The very common
The accelerometer was tested at a particular frequency varying the amplitude of
sensors that used to detect vibrations are piezoelectric accelerometers. These accelerometers
excitation. Figure 5a presents the repeatability of the curve lying within the range ov
are costly andperiod
basedandon the
piezoelectric material, which is very limited. This proposed
data were displayed for 5 s for each amplitude. The highest sensitivit
piezoresistive the
sensor generates electrical resistance change instead of electrical voltage or
accelerometer was found to be 21% g−1 at 30 Hz with a Pearson squared correla
current when coefficient
there is a change in motion or acceleration. As observed in Figure 5b, the
of R2 = 0.999, presented in Figure 5b. This means the response of
vibrational input of the vibrating machine in terms of acceleration (gpk-pk ) and frequency
can be correlated to the output in terms of change in resistance.
 that used to detect vibrations are piezoelectric accelerometers. These accelerometers are
costly and based on piezoelectric material, which is very limited. This proposed piezore-
sistive sensor generates electrical resistance change instead of electrical voltage or current
when there is a change in motion or acceleration. As observed in Figure 5b, the vibrational
input of the vibrating machine in terms of acceleration (gpk-pk) and frequency can be cor-
Materials 2023, 16, 1586 8 of 10
related to the output in terms of change in resistance.

Figure
Figure 5.
5. (a)
(a) Repeatability test
Repeatability test atat a representative
a representative frequency
frequency of 30 of
Hz30
forHz for different
different amplitudes
amplitudes ranging rang-
ing from
from −6 dB-6 dB
to −to -3 dB.
3 dB. (b) (b) Response
Response measurement
measurement at a representative
at a representative frequency frequency
of 30 Hz, of 30 Hz,
40 Hz, and40 Hz,
and 50 Hz for different g
50 Hz for different g values. values.

5. Conclusions
Accelerometers have been an indispensable part of most smart devices along with
application in various fields. Nowadays, high-tech accelerometers are being used in the
market with features including high sensitivity, light weight, durability, broad bandwidth,
and cost-effective. As a novel material for sensing elements, this accelerometer possesses
other features such as simple sensor configuration, light weight, and ease of fabrication.
This accelerometer has the potential to detect a low-frequency vibration ranging from 20 Hz
to 80 Hz for the acceleration up to 8 gpk-pk . The resonance frequency was found to be 85 Hz.
This low-frequency vibration accelerometer can be implemented in machinery for recording
vibrations caused by misalignment and unbalanced and mechanical looseness. This work
Materials 2023, 16, 1586 9 of 10

is the first time investigating the application of the piezoresistive effect of graphene-based
nanocomposite to develop an accelerometer covering a wide range of low frequencies.
We believe that 2D materials are the best candidate for developing piezoresistive devices
due to their stretchability and mechanical strengths. Further work is essential to realize
the full potential of graphene/polymer composites in the development of piezoresistive
MEMS accelerometers.

Author Contributions: S.M. data collection and prepared the initial draft of a manuscript, V.K.S.
prepared nanocomposite material and created an experimental setup, and A.H.J. managed and
supervised the project, created the concept, and revised and approved the final manuscript. All
authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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