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JOURNAL OF MICROELECTROMECHANICAL SYSTEMS 1

Resonant Gas Sensor and Switch Operating in Air

With Metal-Organic Frameworks Coating
Nizar Jaber , Saad Ilyas , Osama Shekhah, Mohamed Eddaoudi, and Mohammad I. Younis, Member, IEEE

Abstract— We demonstrate a resonant gas sensor uniformly to introduce perforations in the resonator surface with careful
coated with a metal-organic framework (MOF) and excited design of the holes size and shape to minimize the damping
near the second vibration mode for enhanced sensitivity. The effect [19].
possibility of realizing a smart switch triggered upon exceeding
a threshold mass is demonstrated when operating the resonator To improve sensitivity, different dynamical principles have
near the dynamic pull-in instability. The resonator is based on been utilized, such as bifurcation points and pull-in insta-
an electrostatically excited clamped–clamped microbeam. The bilities [20]–[22], weakly coupled resonators [23]–[26], and
microbeam is fabricated from a polyimide layer coated from the coupling between bending and torsional modes [27]. The
top with Cr/Au and from bottom with Cr/Au/Cr layer. The sensitivity can be further improved by reducing the resonator
geometry of the resonator is optimized to reduce the effect
of squeeze film damping, thereby allowing operation under size. However; shrinking the size reduces the area available for
atmospheric pressure. The electrostatic electrode is designed to functionalization and requires more controlled environmental
enhance the excitation of the second mode of vibration with the condition for sensing. Alternatively, operating the resonator
minimum power required. Significant frequency shift in kilohertz near the higher order modes can improve sensitivity [28], [29].
is demonstrated for the first time upon water, acetone, and To excite the higher order modes with high amplitudes above
ethanol vapor exposure due to the MOF functionalization and
the higher order mode excitation. The adsorption dynamics and the noise level and with the minimum required power, partial
MOF selectivity are investigated by studying the decaying time electrode configurations have been proposed [30], where the
constants of the response upon gas exposure. [2017-0218] lower electrode is designed to enhance and trigger the desired
Index Terms— Bifurcation, gas detector, electrostatic actuation, mode. Also, an increase in the quality factor is reported near
and resonators. the higher order modes, which is desirable for ultra-small gas
concentration sensing [31], [32]. The pull-in instability [33]
has also been exploited for several applications, including
I. I NTRODUCTION mass detection. For instance, it has been recently demonstrated
for threshold inertia switches [34] and switch-based mass
M ICRO/NANO resonators have shown promising results
for the detection of gasses and minute masses [1]–[13].
Enhancing the sensitivity, reliability, and reducing the power
detectors [22].
The ability to selectively detect specific gasses under ambi-
of electrostatically actuated resonant gas sensors have been the ent conditions represents a constant technological challenge.
subject of extensive research in the past two decades [14], [15]. Functionalizing the resonator surface gives the capability for
Electrostatic actuation is one of the most commonly used selective detection. To detect a particular gas, resonators are
methods due to the low power consumption, ease of fabrica- coated with a thin film that has affinity to a specific gas due to
tion, and integration with CMOS circuits [16]. However, most the chemical and/or physical interaction [35]–[38]. Depending
of the electrostatically actuated resonators for gas sensing need on the targeted gas, different materials were synthesized and
to be operated under controlled environmental conditions and engineered [35], [36]. Gold coated resonators are proposed
at low pressure to reduce the effect of squeeze film damping for mercury detection in [39]. Depending on the gold coating
and obtain a high signal-to-noise ratio [17]. One solution, profile whether uniform layer or isolated islands, different
which requires complex circuit design, is to use positive responses have been reported. Functionalization with zeolitic
and amplified feedback signal from the resonator oscillation imidazolate framework (ZIF), which has nanoporous structure,
velocity to enhance the quality factor [18]. Another approach is is proposed for detecting CO2 . The selectivity of the ZIF
coating to different gasses is demonstrated by studying the
Manuscript received September 11, 2017; revised January 6, 2018; accepted adsorption time constant for IPA and CO2 [23]. A cantilever
January 14, 2018. This work was supported by the King Abdullah University
of Science and Technology. Subject Editor D. DeVoe. (Corresponding author: coated with ZIF has been investigated for detecting nitro-
Mohammad I. Younis.) toluene, which is an explosive related molecule [4]. In [12],
The authors are with the Physical Science and Engineering Division, an artificial nose is developed by coating an array of eight
King Abdullah University of Science and Technology, Thuwal 23955-6900,
Saudi Arabia (e-mail: nizar.jaber@kaust.edu.sa; saad.ilyas@kaust.edu.sa; cantilevers with different polymers for selective gas sensing.
osama.shekhah@kaust.edu.sa; mohamed.eddaoudi@kaust.edu.sa; Metal-organic frameworks (MOFs) are porous materials
mohammad.younis@kaust.edu.sa). composed of organic and inorganic materials with exposed
Color versions of one or more of the figures in this paper are available
online at http://ieeexplore.ieee.org. inner chemical functionality and large surface area that can
Digital Object Identifier 10.1109/JMEMS.2018.2794546 be easily tuned, functionalized, and engineered to selectively
1057-7157 © 2018 IEEE. Personal use is permitted, but republication/redistribution requires IEEE permission.
See http://www.ieee.org/publications_standards/publications/rights/index.html for more information.
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2 JOURNAL OF MICROELECTROMECHANICAL SYSTEMS

detect a specific gas [40], [41]. Resonators coated with MOFs

are proposed for detecting a wide range of gasses, including
volatile organic compounds [42], humidity [43], and H2 S [44].
It is noted from the aforementioned literature survey that
few studies have been dedicated to the development of elec-
trostatically actuated resonant sensors, operated at higher order
modes, working in air, integrated with MOF, and can perform
active switching. In this paper, we present an electrostatically
actuated resonator, excited near the second mode of vibration,
and operated under ambient pressure and temperature. The
sensor can perform switching upon exceeding a threshold
value. The resonator is functionalized with MOFs to further
maximize its sensitivity when exposed to vapors.

II. FABRICATION
In this paper, we study and characterize clamped-clamped
microbeam resonators electrostatically actuated using a lower
electrode that spans half of the beam length to enhance the
excitation of the second vibration mode [30]. To reduce the
effect of squeeze film damping and operate the resonator in
air, the microbeam width is reduced to 20 μm, which is
the minimum width imposed by the fabrication process. The
microbeam is fabricated using the process developed in [45]
and composed of a 4.2 μm polyimide layer coated from
top with Cr/Au layer. The Cr/Au layer acts as a hard mask
that protects the beam during the reactive ion etching and
defines the microbeam dimensions. The upper electrode is
formed by coating the beam from the bottom with Cr/Au/Cr of Fig. 1. (a) Top view picture of the fabricated microbeam with the MOF
thicknesses 50/200/50 nm. The lower electrode spans half of coating. (b) Schematic of the clamped-clamped microbeam with the lower
the beam length to optimize the excitation of the second mode half electrode indicating the beam dimensions.
shape. The two electrodes are separated by 3.3 μm air gap.
In addition to its chemical and thermal stability, polyimide
has low modulus of elasticity (8.5 GPa), which significantly
reduces the voltage required to excite the resonator compared
to the more stiff material; such as silicon (160 GPa).
The microbeam surface is functionalized with a
COOH-terminated layer by immersing the chip in an
ethanolic solution of 16-mercaptohexadecanoic acid for
24 hours [46]–[48]. Before releasing the microbeam,
a uniform MOF layer is grown using a layer-by-layer
approach, by dipping the unreleased chip in copper acetate
metal precursor ethanolic solution and organic ligand Fig. 2. Schematic of the experimental setup used for testing the device.
(terephthalic acid) ethanolic solution for two and three
minutes, respectively. The process is repeated for 12 cycles coating on the resonator surface. Any nonuniformity of the
where the chip is rinsed with ethanol every cycle [43]. coating produces distorted mode shapes. In practical devices,
Fig. 1 shows an optical and schematic of the MOF coated an on-chip capacitive detection scheme can be used to measure
microbeam. the resonance frequencies [49].The microbeam is placed into
a chamber connected to a gas bubbler. The gas flow into the
III. C HARACTERIZATION chamber is controlled using the flow controller. A detailed
description of the characterization experiment is presented in
The experimental setup is shown in Fig. 2. The microbeam the following two sections for the 500 μm long microbeam.
is electrostatically actuated by a data acquisition card con- The results for the 300 μm long microbeam are summarized
nected to an amplifier, which provides actuation signals of in Section V.
wide range of frequencies and amplitudes. A laser Doppler
vibrometer (MSA-500) is utilized to monitor the beam
response, track the shift in the amplitude of vibration due to A. Natural Frequencies
gas exposure, and to obtain the mode shapes of the resonator. To reveal the resonance frequencies, we experimentally
The modeshapes are used to evaluate the uniformity of the excite the device with a white noise signal. The measured
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JABER et al.: RESONANT GAS SENSOR AND SWITCH OPERATING IN AIR WITH MOFs COATING 3

Fig. 3. Frequency response curve of the 500 μm long microbeam to a white

noise excitation at V DC = 15 V and V AC =10 V. Insets: The corresponding
mode shapes.

resonance frequencies of the beam can be used to calculate

the residual stress and the flexural rigidity of the beam,
which are needed for the analytical modeling of the beam
behavior [30]. The vibration at different points along the
beam is recorded to extract the frequency response curve
and the corresponding mode shapes, as depicted in Fig. 3.
The measured mode shapes, insets of Fig. 3, are qualitatively
matching the theoretical ones; except very close to the anchors,
where the laser measurements become less accurate.

B. Frequency Response Curves Fig. 4. Frequency response curves at V DC =30 V and different V AC
excitation near (a) the first mode, (b) the second mode of the 500 μm long
Next, we experimentally investigate the frequency response microbeam.
of the microbeam near the first and second mode of vibration
when excited by harmonic forces. The excitation signal is monitoring the gain or phase change for a fixed frequency
composed of an AC signal V AC superimposed to a DC excitation, and measuring the change in the quality factor (Q).
signal V DC . The measurement is performed by focusing the The most conventional method is to monitor the frequency
laser at the mid-point for the first mode measurements and shift using the phase locked loop (PLL). This method is
quarter of the beam length for the second mode measurement. adequate for high Q resonators. However, for low Q resonators,
Then, the frequency response curve is generated by sweeping which is the case for our resonator (Q 1st = 9.7, and Q 2nd =
the frequency  of the AC source near the mode of inter- 28.3), designing and implementing the PLL circuit becomes
est and taking the steady state maximum amplitude of the challenging and complicated. In this case, another method
motion Wmax . Figure 4 shows the frequency response near is recommended, in which the resonator is excited near the
the first (72.5 kHz) and second (184.2 kHz) modes of vibration resonance frequency, and the amplitude change due to gas
for different AC loadings. As can be seen in Fig. 4, increasing exposure is recorded. Then, the amplitude change is calibrated
the AC voltage near the first mode causes a slight shift in the into a frequency shift, which is used to calculate the amount of
resonance frequency towards lower values (softening) due to the adsorbed gas [50]. Figure 5 shows the frequency response
the quadratic nonlinearity coming from the electrostatic force. and the calibration formula near the first and second mode
While near the second mode, the frequency increases toward of vibration of the 500 μm long microbeam. The operating
higher magnitudes (hardening) due to the dominance of the point is chosen close to the peak of the response curve, i.e., at
cubic nonlinearity. The reported frequency sweeps help to 72.5 kHz near the first mode and 184.2 kHz near the second
understand the effect of the actuation voltage and choose the mode. As vapor is being absorbed on the resonator surface,
suitable operating voltages in the gas sensing experiment. the amplitude decreases following the right branch of the
response. This decrease is transformed into frequency shift
by using the slope, as shown in each plot.
C. Sensor Sensitivity
The responsivity is defined as
To quantify the amount of adsorbed gas, different methods
have been utilized in the literature, such as tracking the ∂f −f
= = (1)
frequency shift by implementing a phase-locked loop circuit, ∂m 2m
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4 JOURNAL OF MICROELECTROMECHANICAL SYSTEMS

Fig. 5. The frequency response of the 500 μm long clamped-clamped Fig. 6. The maximum amplitude evolution of the 500 μm long microbeam
microbeam at V DC = 30 V near (a) the first mode and V AC = 35 V, over time for a fixed frequency excitation at V DC = 30 V near the (a) first
(b) the second mode and V AC = 45 V. mode, V AC = 35 V, and = 72.5 kHz. (b) Second mode at V AC = 45 V, and
= 184.2 kHz.
 
where, m is the beam mass, and f = ω2π non EI
ml 3 is and second mode is Wmax 1st = 20nm, and W 2nd = 19nm,
the operating frequency, ωnon is the nondimensional natural max
respectively, which correspond to the minimum detectable
frequency of the clamped clamped microbeam (varies with 1st = 216.2H z and  f 2nd = 317.7H z,
frequency of  f min min
the mode number), EI is the flexural rigidity, m is the beam
respectively. Using Eq. (2), the minimum detectable mass is
mass, and l is the length of the beam. By rearranging Eq. (1),
defined as m min = 3 × m noise = 3 ×  f noise −1 , which
the amount of the uniformly adsorbed gas mass m along the
yields m 1st
min = 2.3 pg and m min = 1.3 pg.
2nd
beam surface can be calculated as
−2m IV. G AS S ENSING
m = × f (2)
f
The partial pressure of the generated vapor is calculated by
The mass m of the microbeam was calculated from the utilizing Antonio’s equation [43]
geometrical dimensions and the material properties m = B
128.1 pg. From Eq. (2) we found that the −1 of the resonator Log10 Pv = A − (3)
near the first and second mode equals to −1 f g C+T
 1st = 3.5 Hz where T is the bubbler temperature that is measured experi-
and −1
2nd = 1.4
fg
H z , respectively. mentally using a thermocouple. A, B, and C are parameters
Using the laser Doppler vibrometer, The minimum
that are defined for each material in a specified range of
detectable mass is measured by exciting the resonator at the
temperature. The gas concentration Cvapor in ppm is found
operating frequency and monitoring the amplitude fluctuation
by using the following formula:
due to noise over a 5 minute period. The experiment is con-
ducted near the first and second mode of vibration as depicted Pv
Cvapor = × 106 (4)
in Fig. 6. The measured amplitude fluctuation near the first Pat m
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JABER et al.: RESONANT GAS SENSOR AND SWITCH OPERATING IN AIR WITH MOFs COATING 5

TABLE I
S UMMARY OF THE B UBBLER T EMPERATURE AND THE
C ONCENTRATION OF THE D IFFERENT VAPORS

TABLE II
F REQUENCY S HIFTS AND THE F ITTED T IME D ECAY C ONSTANTS D UE
TO D IFFERENT G AS E XPOSURES N EAR THE F IRST (72.5 K Hz) AND
S ECOND (184.2 K Hz) M ODE OF V IBRATION

As shown in Table 1, Acetone has the highest concentration

while water vapor has the lowest concentration under the
current experimental conditions.
The chamber is flushed with nitrogen for an extended
period of time until the response is stabilized. We used a
flow rate of 4 l/min to reduce the transient time required
to completely flush or fill the chamber with a particular gas
concentration. Then, the resonator is exposed to vapors while
monitoring the response until saturation, which corresponds
to the maximum vapor adsorbed on the resonator surface.
To ensure the repeatability of the results, the vapor flow is
replaced with nitrogen to flush the resonator and return to the
original state. The exposure and flushing cycle is repeated for
several times to ensure a complete reversibility of the sensor. Fig. 7. Real time measurement of the frequency shift near the first
Figure 7 shows the frequency shift of the resonator over time (72.5 kHz) and second (184.2 kHz) mode of vibration due to vapor exposures
of (a) water vapor, (b) Acetone, and (c) Ethanol.
due to water vapor, Acetone, and Ethanol exposures near the
first and second mode of vibration. A higher frequency shift for
the different gasses is reported near the second mode as shown
beam velocity compared with the first mode, which implies
in Table 2. The dynamics of the absorption is studied by fitting
that more time is needed for the gas molecules to stabilize on
an exponentially decaying function f(t) = f exp(-t/τ ) to the
the resonator surface. The reported results can be promising
experimental data, where τ is the time constant, and  f is the
for humidity sensing in wide range of applications, such as air
amplitude of the frequency shift [23]. As shown in Table 2,
quality control, process control, and biomedical sensors [51].
although water vapor has the lowest concentration, a higher
frequency shift and smaller time constant is measured, which
indicates a strong affinity of MOF to water vapor compared V. S WITCH T RIGGERED BY M ASS
with Acetone, and Ethanol. Also, a higher decay time constant It is desirable to realize a smart sensor that can act as
is reported near the second mode of vibration due to the higher an electrical switch to trigger an action on demand if the
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6 JOURNAL OF MICROELECTROMECHANICAL SYSTEMS

TABLE III
S UMMARY OF THE C HARACTERIZATION R ESULTS OF
THE 300 μm L ONG M ICROBEAM

Fig. 9. Real time measurement of the amplitude change due to water vapor
exposure until pull in. The vapor exposure started at time = 4.5 minutes.
Inset: the fluctuation due to noise.

pull-in, and hence can be functionalized as an electrical

switch. As a case study, we selected the operating frequency
160 kHz, which corresponds to a threshold mass of 6 pg.
Before exposing the resonator to water vapor, we monitored
the amplitude fluctuation due to noise to ensure the stability
of the response as depicted in the inset of Fig. 9. Then,
the microbeam is exposed to water vapor and the amplitude of
vibration increased following the left branch of the frequency
Fig. 8. Frequency response near the first mode showing the softening response shown in Fig. 8. When the amount of adsorbed
behavior and the pull-in band at V DC = 50 V, and V AC = 80 V. mass exceeded the threshold value, the resonator collapsed
into pull-in, Fig. 9.
amount of absorbed mass/gas exceeds certain threshold [15].
This concept was demonstrated first in [22] using resonators VI. C ONCLUSIONS
operating in vacuum. Here we demonstrate the concept for We presented a sensitive resonant gas sensor, functionalized
the first time in air. The concept is based on operating a with a uniform MOF layer, and electrostatically excited near
resonator at a fixed operating frequency close to the dynamic the second vibration mode under ambient pressure and tem-
pull-in band [22]. As the mass of the resonator is increased perature. Using the optical vibrometry readout, a minimum
due to gas absorption, the pull-in band shifts toward the fixed detectable mass of 1.3 pg and resolution of 1.4 fg/Hz are
frequency until the operating fixed frequency lies completely reported near the second mode of vibration. Also, we demon-
inside the pull-in band; hence leading to the collapse of the strated a smart switch that can sense the presence of a
resonator. By designing and implementing the appropriate particular gas and can simultaneously perform switching upon
circuit, the collapse of the two electrodes can be used to exceeding the certain threshold value. As a case study, the pull-
activate an alarm or close a valve. in due to water vapor exposure was demonstrated. Water
Next, we demonstrate the concept of the switch triggered by vapor, Acetone, and Ethanol gasses were tested near the first
exceeding a certain threshold of gas in air using the same set of and second mode of vibration where large frequency shift in
characterization experiments and calibration procedures imple- (kHz) was measured for the first time. The selectivity of the
mented previously, however on a 300 μm long microbeam. MOF coating to water vapor is demonstrated by studying the
The results are summarized in Table 3. The microbeams were adsorption dynamics of the experimentally recorded response.
fabricated on the same chip using the same material and layer
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 This article has been accepted for inclusion in a future issue of this journal. Content is final as presented, with the exception of pagination.

8 JOURNAL OF MICROELECTROMECHANICAL SYSTEMS

Nizar Jaber received the B.S. degree in mechanical Mohamed Eddaoudi was born in Agadir, Morocco.
engineering from the Jordan University of Sciences He received the Ph.D. degree in chemistry from
and Technology, Jordan, in 2010, and the master’s the Université Denis Diderot (Paris VII), France.
degree in mechanical engineering from the King He held a post-doctoral position at Arizona
Abdullah University of Science and Technology, State University and the University of Michigan.
in 2014, where he is currently pursuing the Ph.D. He joined the University of South Florida as Assis-
degree in mechanical engineering. His research tant Professor in 2002, as an Associate Professor
interests include linear and nonlinear dynamics of in 2008, and as a Professor in 2010. He is cur-
MEMS-based resonators with their applications in rently a Distinguished Professor of chemical science
MEMS sensors and actuators. and the Director of the Advanced Membranes and
Porous Materials Research Center, King Abdullah
University of Science and Technology, Saudi Arabia. His research focuses on
developing strategies, based on (super) molecular building approaches (MBB,
SBB, and SBL) for rational construction of functional solid-state materials,
namely, metal-organic frameworks. Their prospective uses include energy
Saad Ilyas received the B.S. degree in mechanical and environmental sustainability applications. His eminent contribution to the
engineering from the Ghulam Ishaq Khan Institute burgeoning field of MOFs is evident from his selection in 2014 as a Thomson
of Engineering Sciences and Technology, Pakistan, Reuters Highly Cited Researcher.
in 2012, and the master’s degree in mechanical
engineering from the King Abdullah University of
Science and Technology, in 2014, where he is
currently pursuing the Ph.D. degree in mechanical
engineering. His research interests include linear
and nonlinear dynamics of MEMS devices with
applications in MEMS sensors and actuators. He Mohammad I. Younis (M’17) received the B.S.
is a Student Member of the American Society of degree in mechanical engineering from the Jordan
Mechanical Engineers. University of Science and Technology, Irbid,
Jordan, in 1999, and the M.S. and Ph.D. degrees
in engineering mechanics from Virginia Polytechnic
Institute and State University, Blacksburg, VA, USA,
in 2001 and 2004, respectively. He is currently
Osama Shekhah received the Ph.D. degree an Associate Professor of mechanical engineering
in physical and surface chemistry from the with the King Abdullah University of Science and
Free University Berlin and the Fritz-Haber Insti- Technology, Thuwal, Saudi Arabia, and also with the
tute, Berlin, in 2004, under the supervision of State University of New York (SUNY), Binghamton,
Prof. R. Schlogl. He held a post-doctoral posi- NY, USA. He serves as the Director of the MEMS and NEMS Characterization
tion at the Fritz-Haber Institute for one year. and Motion Laboratory. He has authored the book MEMS Linear and
In 2005, he joined the Physical Chemistry Group of Nonlinear Statics and Dynamics (Springer, 2011). He holds several U.S.
Prof. C. Woll at Ruhr-University Bochum, as a Staff patents in MEMS sensors and actuators. He is a recipient of the SUNY
Scientist. In 2009, he moved to the Institute of Func- Chancellor’s Award for Excellence in Scholarship and Creative Activities
tional Interfaces, Karlsruhe Institute of Technology, in 2012, the National Science Foundation Faculty Early Career Development
with Prof. C. Woll as a Group Leader. In 2011, Award in 2009, and the Paul E. Torgersen Graduate Research Excellence
3
he joined the FMD Group of Prof. M. Eddaoudi, KAUST, as a Group Award in 2002. He serves as an Associate Editor for Nonlinear Dynamics,
Leader. His research interests include surface chemistry, material chemistry, the Journal of Computational and Nonlinear Dynamics, and the Journal of
self-assembled monolayers, and metal–organic frameworks porous material Vibration and Control. He is a member of the American Society of Mechanical
synthesis, growth, and their thin films fabrication and applications. Engineers.