Proceedings of the 2010 5th IEEE International

Conference on Nano/Micro Engineered and Molecular Systems

January 20-23, Xiamen, China

A Chemical Surface Acoustic Wave(SAW) Sensor

Array For Sensing Different Concentration of NH3
Hsu-Chao Hao
Institute of NanoEngineering and MicroSystems, National
Tsing Hua University,
Hsichu, Taiwan
haohsuchao@gmail.com

Tai-Hsuan Lin
Institute of NanoEngineering and MicroSystems, National
Tsing Hua University
Hsichu, Taiwan
thlin@mx.nthu.edu.tw

Mei-Ching Chen
Institute of NanoEngineering and MicroSystems, National
Tsing Hua University,
Hsichu, Taiwan
g9735505@oz.nthu.edu.tw

Da-Jeng Yao
Institute of NanoEngineering and MicroSystems, National
Tsing Hua University
Hsichu, Taiwan
djyao@mx.nthu.edu.tw

AbstractSurface acoustic wave (SAW) sensor is generally

known as high-resolution mass-sensitive transducers. We
developed a novel SAW sensing array based on 2x2
non-continuously working oscillators equipped with differently
coated SAW sensors, respectively, which is used to analyze
organic compound gases. The sensing array consisting of four
two-port SAW resonator sensors with a fundamental frequency
at 99.8 MHz was fabricated on LiNbO3 substrate. Four different
polymers were coated on the surface of sensing regions. The gas
sensing array was put into 10L reaction chamber with
temperature and humidity controllable environment. The
frequency outputs from each sensor were used to compare with
the frequency from a reference device for eliminating the
environmental effects. The results suggest that frequency shift of
the designed gas sensor array changes with different
concentration of the target gas(NH3).
Surface acoustic wave (SAW); non-continuously; LiNbO3;
organic compound gases

I.

INTRODUCTION

Organic vapors are colorless with sharp, penetrating,

intensely irritating odors under pressure, which could be
corrosive and fatal if inhaled. Therefore, detection of organic
vapors is essential for human safety[1, 2], industrial
hygiene[3-5], and clinical diagnosis[6]. Gas detection methods
may be split into two groups, (i) direct methods, which
monitor a physical parameter of the target gas, and (ii) indirect
methods, which use a chemical reaction or indicator to show
the concentration of the gas being sensed. Various types of
sensors have been used for gas sensing, including
electrochemical sensors, metal oxide semiconductor (MOS)
sensors, infrared sensors, photoacoustic sensors, etc[7].
Electrochemical sensors usually contain several different
electrodes, including sensing electrodes, counter electrodes,
reference electrodes and a membrane which is porous to gas
but not to liquid. As air diffuses into the cell, certain gases are

978-1-4244-6545-3/10/$26.00 2010 IEEE

adsorbed by the sensor and a parameter differential is

produced. The current produced by the chemical reaction is
proportional to the concentration level of the reacting gas.
In order to achieve high sensitivity, a polymer-coated
surface acoustic wave (SAW) array is one of the best choices
for organic gas sensing applications. Currently SAW devices
are also used for chemical applications because of their high
sensitivity, fully reversible behavior, and high signal-to-noise
ratio[8].
For the proposed portable E-nose system based on
the SAW sensor array, a piezoelectric substrate was chosen for
energy transformation between mechanical strains and electric
signals. The interdigital transducers (IDTs), input and output
comb-like metal electrodes, were used as energy
transformation structures on the surface of the selected
substrate. When an AC voltage was applied to the input IDTs,
the IDTs would induce dynamic strains in the substrate, which
would launch surface wave on the top of substrate. The
induced surface wave would propagate through the active
sensing region, and then be received and transformed into
electric signals by the output IDTs. According to the
magnitude change and phase shift of the AC electric signals
between input and output IDTs, the mass change on the active
sensing region could be detected.
So as to increase selectivity and sensitivity of the sensor,
different polymers were coated on the active sensing region of
the SAW sensors to absorb molecules of the target gas. For
example, poly(N-vinylpyrrolidone , PNVP) was used in this
study as one the sensing films due to its good selectivity to
amine vapors. Several studies have been carried out to develop
pernicious gas sensors using organic layers [9],
semi-conducting metal oxides[10], and self-assembled
layers[11, 12]. However, the persistence and reproducibility of
the sensing devices based on organic layers were poor.
Semi-conducting metal oxide films have shown better
performance, but most of them are suitable only for high

1092

temperature sensing, which is not appropriate for the portable

sensing system. On the other hand, polymer-based sensing
films have shown good performance in room temperature,
which is more appropriate for a portable E-nose system. For
example, a self-assembled polymer layer, polydiacetylene
(PDA)/calyx[13]arene(CA), assembled on ST-quartz SAW
sensor chip, shows good linear response for amine vapors in
room temperature [14].
We have made chemical SAW sensors by using MEMS
technology and designed oscillator circuits to improve sensing
results. We have constructed a SAW delay line onto a 128
YX-LiNbO3 piezoelectric substrate with high K2 value as our
SAW devices, and we have coated them with polymers on the
active sensing region by a self-assembled process to form 2u2
non-continuously SAW array chips. Polymer selection and
preparation as chemical interfaces for the SAW array has been
tested. We have designed and implemented frequency shift
readout electronics comprising multiplexer, counter and
89C51 microprocessor. Frequency variation of the SAW
device between its start and stable states has been tested to be
smaller than 1 kHz. We have investigated the selectivity,
sensitivity, reversibility and chemical characteristics of the
sensor at room temperature. The results will be reported in the
following sections.
II.

EXPERIMENTAL

The way of a SAW-based electronic nose system is to read

out the frequency by the use of an instrument such as
spectrum analyzer or frequency counter. In this paper, we
present our recent progress about five gas sensing as database
and focus on the identification of isopropyl alcohol (IPA),
which is as simulate unknown gas. At first, we introduce the
SAW array sensor system in four parts: surface acoustic wave
sensor fabrication, polymer coated on the piezoelectric
substrate, SAW array circuit, and measurement system finally.
A. Surface Acoustic Wave Sensor Fabrication
In general, a chemical sensor consists of two major
components: a transducer and a sensitive coating. A
transducer is required to transform information to a
measurable signal. A parameter K2 gives the capacity of
translation between electric and mechanical potentials [15].
The value of K is determined by
e2
(1)
K2
cH
Where e, c,  are the piezoelectric coefficient, elastic
coefficient, and dielectric coefficient of the substrate. The
value of K2, which can be calculated by equation (1), depends
on the properties of the piezoelectric substrate or on the
experimental results due to the velocity shift under
metallization. LiNbO3 is chosen as the chip substrate for high
acousto-electric effect to enhance the sensitivity of the chip
comparing with other substrates.

to the capacity of absorption on the active sensing region and

result in frequency shift or phase shift. Considering the effects
of perturbation by mass loading including elastic loading and
electric loading, the propagation characteristics of the surface
wave are affected as follows [16, 17]:
'v
v0

4P
2 K  P 
2

v
V s2
N


'
cm f 0 'U s  ce f 0 h' 0

2
K  2P 2 V s  v0 2 C s 2

(2)

where cm and ce are the sensitivity coefficients for the mass

and elasticity, s is mass per area,  and  are the shear and
bulk moduli of the film, s is the sheet conductivity of the film,
and Cs is the capacitance per length of the SAW substrate
material and N is the wavenumber (N = 2/). It is important
that these three terms of equation (2) indicate the contributions
of changes to total change in SAW velocity in mass, in elastic
constants, and in electrical conductivity, respectively. Since
polymers are not conductive but stiff materials resistant to
surface waves, the variation of frequency is only influenced by
mass loading. Thus, the center frequency of sensor would
decrease due to absorption of molecules of the target gas on the
film.
Interdigital transducers (IDTs) have been widely used for
electric signal excitation and detection of surface acoustic
waves (SAW). Each period of IDTs consists of multiple strips
aligned and connected to the bus-bars periodically. Different
center frequency and phase response, based on the design of
IDTs, have been measured by network analyzer. The electric
characteristics of IDT have been determined by the finger
geometry during the period, the number of finger-pairs, and the
substrate material. For simplicity, a simple velocity equation (3)
is used to design the center frequency of SAW device,

f O

(3)

Where V is the velocity of the surface wave for the chosen

substrate, f is the center frequency of the designed SAW device,
and  is the wavelength of the surface wave. The wavelength of
the surface wave is a function of the spacing between fingers
and the width of the fingers. The spacing of a
single-electrode-type IDT is determined to be one-fourth the
wavelength (/4) (figure 1), which gives the required definition
for photolithography.

When a SAW sensor is exposed to the target gas, its

electrical and mechanical characteristics will change according

1093

Figure 1. The designed parameters of SAW sensor.

B. Polymer
We have applied four different polymers, including Poly
N-vinylpyrrolidone (PNVP), Poly 4-vinylphenol (P4VP),
Polystyrene-co-maleic anhydride (PSMA), and Poly-caprolactone(PCL) [18] (figure 2), with different polarities and
functional groups. In order to coat the SAW sensor surface
with chemical interfaces, a simple spin-coating method was
used. Thickness of polymers is roughly 8~14 m and SAW
frequency shift is about 200~450 kHz. Before we coated the
sensing layer, the center frequency of every SAW sensor was
measured by network analyzer and marked as f0.The frequency
of the chip after coating fp was then measured. In order to
eliminate the effects from polymer and circuit, the
normalization method, fgas/fpolymer (fpolymer=fo-fp) was used.
For this purpose, dilute solutions of P4VP (in 95% ethanol),
PSMA and PCL, (in methyl ethyl ketone), PNVP (in
tetrahydrofurane) were prepared. Tableshows the polymeric
solutions dropping on the surface of interdigital transducer
(IDT) device to spin-coat the thin film. After the spin-coating,
the device was taken and left for hours for the solvent to
evaporate completely.

are controlled non-continuously by a multiplexing (MUX)

technique as switching element, respectively (figure 3) [10].

Figure 3. Schematic measurement setup of the non-continuously SAW

sensing array.PCB.

D. Measurement System
The test system is composed of a polymer-coated SAW
sensor array, a PC for data logging, a power supply, a vacuum
pump, a steel cylinder of nitrogen, a 10L reaction chamber,
and a frequency counter (Agilent 53131A). The SAW
oscillators are controlled non-continuously by a multiplexer
(MUX, Analog device ADG1406 ) and a counter (Fairchild
semiconductor 74VHC4040) as switching element(figure
4)[19, 20].

Figure 2. Structural formula of polymer.

Table
polymer
poly N-vinylpyrrolidone
PNVP
poly(4-vinylphenol)
P4VP
poly(styrene-co-maleic
anhydride)
PSMA
Poly-capro- lactone
PCL

M.W.
70,000~
100,000
9,000~
11,000

solvent
tetrahydrofurane
ethanol

~224,000

methyl ethyl ketone

~430,000

methyl ethyl ketone

C. SAW Array
Sensor array is the important technology in the research of
electronic nose field, because it not only saves us a lot of time
but also offers a result from variety of sensing films. By
coating different polymers on the surface of different
resonators, a SAW array is constructed. These SAW oscillators

Figure 4. Schematic setup of sensing gas system contains 10 L reaction

chamber, frequency counter, power supply, gas generator, FTIR and SAW
array.

The readout time of the array is below 1s, and the SAW
devices are designed to operate at 99.8 MHz. Multiplexing
technique is used to prevent cross talks from the individual
oscillators. This allows a compact single board setup for all
oscillators. When the MUX is set to a negative voltage, the

1094

oscillation is disabled (switch off mode). When it is set to a

certain positive voltage 5V, the oscillation is supported
(switch on mode), and the phase of the oscillator is set on a
desired value.
High frequency SAW devices were chosen as sensing chips
and combined with wide bandwidth external feedback
amplifier circuits to construct the oscillator circuit. This circuit
was used as a bionic E-nose for sensing molecules of the
target gas, and output signals were measured by the readout
electronics with frequency counter (Agilent 53131A) as a
reference. For data logging and control purposes, a GPIB card
was adopted as the interface and a monitoring program (visual
basic) was used to control the computer. Thus, digital values
could be obtained, which was better than the analog graph
from the network analyzer.
First, bake the sensor array for 20 minutes on 90 before
measurement. There are three steps in one cycle of gas testing:
(a) The system operates stably under vacuum pumped for
30 minutes.
(b) After the frequency stabilizes, turn off the vacuum pump.
Inject the test solution and respond for 60 minutes.
(c) Turn on the vacuum pump and air flow valve to clean
the chamber for 30 minutes.
(d) Turn off the air flow valve and return to step (a).
The total time of one cycle is about 120 minutes.
III.

SAW sensors for NH3 were investigated (Table ).

Compared with other polymer films, the larger frequency shift
of the sensitive P4VP and PNVP film for every assayed vapor
may be attributed with hydrogen bonding formation between
polymers (P4VP and PNVP) and polar organic molecules such
as amine. As well as P4VP film, PVAc-coated and
PNVP-coated SAW sensors also present good frequency
response for sensing polar vapors because of H-bond
formation. Their hydrophilic characters explain that they have
larger frequency variation than the other thin films. Otherwise,
PS, PSu and PSMA, all of three are more hydrophobic, so
their frequency shifts toward five kind of gas are small
approximately in 7~9 kHz. Regarding the structure of these
polymers, expect for PCL, the main chains are composed of
long sp3 carbons. Many polymers chosen in this study (e.g.
PVAc,P4VP and PSMA) contain polarizable carbonyl groups
in their side chains. The data show that for polymers bearing
carbonyl functional groups, their response to ammonia are
larger. However, PSMA-coated SAW sensors reveal smaller
frequency shift for sensing polar organic vapors. That is
because all of them consist of phenyl group, which is
hydrophobic and nonpolar functional group, to diminish the
adsorption of polar organic vapors.
Table : Frequency Shifts and normalization

RESULTS AND DISCUSSIONS

A. The Effect of Temperature and Humidity

The sensor characteristics were tested for temperature
between 30 and 50 and relative humidity (RH) between
45% and 50%. The correlation results were shown in table ,
that givs around 5 kHz per degree in temperature and 0.5 kHz
per percentage in humidity.The Simple regression equation for
frequency shift(Y, MHz) and temperature(X, ) is
Y= 0.10376+0.0032X, R2=0.9961.
Table: the frequency of ref. SAW at different temperature and humidity.

temp.
()
30

40

50

humi.
()
20
40
60
20
40
60
20
40
60

ref. 1
(MHz)
98.84068
98.84643
98.82532
98.78161
98.78418
98.77863
98.73811
98.73496
98.7315

ref. 2
(MHz)
98.70673
98.72894
98.69368
98.6522
98.65595
98.65324
98.60373
98.60272
98.60211

IV.

B. Sensing Different Concentration of NH3

The sensing array would be used to detect Different
Concentration of NH3.Follow the discussion from the four
polymer films, P4VP and PVAc are approximately in 20~30
kHz. The frequency responses of the different polymer-coated

CONCLUSION

The
frequency
responses
of
the
different
polymer-coated SAW sensors for various polar organic vapors
were investigated. Table shows frequency shifts from the
SAW array sensor for organic molecules (NH3). Compared
with other polymer films, the larger frequency shift of the
P4VP and PNVP sensitive film for every assayed vapor may
be attributed with hydrogen bonding formation between
polymer film and polar organic molecules such as amine and
alcohol. However, PSMA or PCL-coated SAW sensors reveal
smaller frequency shift for sensing polar organic vapors. That
is because all of them consist of phenyl group or long carbon
chain, which is hydrophobic and nonpolar functional group, to
diminish the adsorption of polar organic vapors. The results
suggest that frequency shift of the designed gas sensor array
changes with different concentration of the target gas.

1095

ACKNOWLEDGMENT
The authors would like to acknowledge the support of the
National Science Council of Taiwan, under Contract No. NSC
97-2220-E-007-036 and NSC97-3114-E-007-002.

[20] H. P. Hsu, J. S. Shih, "Surface acoustic wave olefin/alkyne sensor based

on Ag(I)/cryptand-22", Sensors and Actuators B, Vol. 114, pp. 720-727,
2006.

References
[1] Q. Cai, W. Wei, R. Wang, L. Nie, S. Yao, "Kinetic assay of antitrypsin in
human serum by a surface acoustic wave(SAW)-impedance sensor ",
Fresenius' Journal of Analytical Chemistry, Vol. 356, pp. 96-97, 1996.
[2] I. A. Casalinuovo, D. Di Pierro, M. Coletta, P. Di Francesco, "Application
of Electronic Noses for Disease Diagnosis and Food Spoilage Detection",
Sensors Vol. 6, pp. 1428-1439, 2006.
[3] C.Y. Shen, C.P. Huang, W.T. Huang, "Gas-detecting properties of surface
acoustic wave ammonia sensors", Sensors and Actuators B: Chemical, Vol.
101, pp. 1-7, 2004.
[4] F. C. Huang, Y. Y. Chen, T. T. Wu, "A room temperature SAW hydrogen
sensor using Pt coated ZnO nanorods", Nanotechnology, Vol. 20, pp.
065501, 2009.
[5] T. T. Wu, Y. Y. Chen, D. H. Chou, "A High Precision Nanomaterial
Based SAW Humidity Sensor", J. Physics D: Applied Physics, Vol. 41, pp.
085101, 2009.
[6] W. A. Groves, E. T. Zellers, G. C. Frye, "Analyzing organic vapors in
exhaled breath using a surface acoustic wave sensor array with
preconcentration: Selection and characterization of the preconcentrator
adsorbent", Analytica Chimica Acta, Vol. 371, pp. 131-143, 1998.
[7] K. Lnge, B. E. Rapp, M. Rapp, "Surface acoustic wave biosensors: a
review ", Analytical and Bioanalytical Chemistry, Vol. 391, pp.
1509-1519, 2008.
[8] J. W. Gardner, V. K. Varadan, Microsensors: MEMS and Smart Devices
Third ed, John Wiley and Sons, New York, 2001.
[9] D. Enguang, "Organic Vapor Based on SAW Resonator and Organic
Films", IEEE Transaction on ultrasonics,ferroelectrics and frequency
control, Vol. 44, pp. 1997.
[10] M. Penza, L. Vasanelli, "SAW NOx gas sensor using WO3 thin film
sensitive coating", Sensor and Actuators B, Vol. 41, pp. 31-36, 1997.
[11] H. C. Yang, D.L. Dermody, C. Xu, A. J. Ricco, R. M. Crooks,
"Molecular Interactions between Organized, Surface-Confined
Monolayers and Vapor-Phase Probe Molecules. 8. Reactions between
Acid-Terminated Self-Assembled Monolayers and Vapor-Phase Bases",
Langmuir, Vol. 12, pp. 726-735, 1996.
[12] C. Wang, X.W. He, L. X. Chen, "A piezoelectric quartz crystal sensor
array self assembled calixarene bilayers for detection of volatile organic
amine in gas", Talanta, Vol. 57, pp. 1181-1188, 2002.
[13] D. Enguang, F. Guanping, H. Zhenhua, C. Dafu, "Organic vapor sensors
based on SAW resonator and organic films", IEEE Transaction on
ultrasonics,ferroelectrics and frequency control, Vol. 44, pp. 1997.
[14] D. L. Dermody, R. M. Crooks, T. Kim, "Interactions between Organized,
Surface-Confined Monolayers and Vapor-Phase Probe Molecules. 11.
Synthesis, characterization, and chemical sensitivity of self-assembled
polydiacetylene/calix[n]arene bilayers", J. Am. Chem. Soc., Vol. 118, pp.
11912-11917, 1996.
[15] B. Drafts, "Acoustic wave technology sensors", IEEE Transactions on
Microwave Theory and Techniques, Vol. 49, pp. 795-802, 2001.
[16] M. Penza, "Gas sensing properties of Langmuir-blodgett polypyrrole film
investigated by surface acoustic waves", IEEE Transactions on
ultrasonics,ferroelectrics and frequency control, Vol. 45, pp. 1125-1132,
1998.
[17] B. D. Stephen, R. M. White, Acoustic wave sensors:theory, design, and
physico-chemical applications, Academic Press, 1996.
[18] S. H. Hosseini, A. A. Entezami, "Preparation and characterization of
polyaniline blends with polyvinyl acetate polystyrene and polyvinyl
chloride for toxic gas sensors", Polymers for Advanced Technologies, Vol.
12, pp. 482-493, 2002.
[19] M. Rapp, J. Reibel, A. Voigt, M. Balzer, O. Blow, "New miniaturized
SAW-sensor array for organic gas detection driven by multiplexed
oscillators", Sensors and Actuators B, Vol. 65, pp. 169-172, 2000.

1096