IJRFCAD
IJRFCAD
DOI: 10.1002/mmce.21895
RESEARCH ARTICLE
KEYWORDS
gas sensor, microwave resonator, nanorods, PCB
Int J RF Microw Comput Aided Eng. 2019;29:e21895. wileyonlinelibrary.com/journal/mmce © 2019 Wiley Periodicals, Inc. 1 of 10
https://doi.org/10.1002/mmce.21895
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variation, and phase change) and the variation is specific to frequency is the most effective for remote sensing because
a gas and sensitive material.4 This mechanism uses different the amplitude is susceptible to interference and noise, lead-
microwave designs such as resonator, antenna, and wave- ing to false positives (ammonia detection), while the fre-
guides. Materials, which are used as sensitive layers in this quency shift is relatively insensitive to these detrimental
technique, can be polymers, metal oxides or carbon nan- factors.7 The gas sensors operated at microwave frequencies
otubes (SWNT or MWNT), and zeolites. Sensitive materials offer better sensitivity.12 In Reference 12, the gas sensor is
are selected based on their gas sensing properties such as exposed to 100 ppm ethanol gas in humidity condition. Elec-
response time, recovery time, sensitivity, and selectivity to trical properties of conducting polymer get changed by
the target gas. The widely used sensitive materials are metal chemical interaction between the conducting polymer
oxides which are based on the adsorption and the reaction and ethanol gas which results in the frequency shift. In
between the surface of the sensitive materials and the gas Reference 13, the designed sensor is a microstrip patch
molecules. Gas sensing properties of sensitive material vary antenna coated with single-walled carbon nanotubes
with variations in the specific area, particle size, porosity, (SWCNTs). A frequency shift and change in permittivity have
and thickness of the sensing film.5 In Reference 6, a micro- been observed when the ethanol-water vapor is injected.
wave circular disk resonator coated with carbon nanotubes Thus from the study of the literature, several authors have
for the detection of NH3 with a response time of 10 minutes reported microwave gas sensing at a single narrow fre-
is reported. The researchers have concluded that changes in quency band. The sensing accuracy is not verified at differ-
the dielectric constant of the carbon nanotubes lead to ent frequency scales. Also, the validity of the results is not
change in the effective dielectric constant which alters the reported using time domain analysis. Therefore, effort is put
frequency domain characteristics of the microwave resona- in this research to analyze the gas sensor performance in
tor. In Reference 3, a grounded coplanar waveguide with both the time domain and frequency domain and also to
phthalocyanine as sensitive material for ammonia. Their improve the accuracy of the results by extending the mea-
work is based on the variation of real and imaginary parts of surements at three different frequencies. The proposed
the reflection coefficient when exposed to ammonia. In Ref- method adopts two sensitive layers viz., TiO2 and ZnO for
erence 7, a gas sensor using a patch antenna with PABS- ethanol gas detection. Ethanol sensing performance of this
SWNT as sensing material is reported. Measurements work shows a lower operating temperature, faster response
showed a frequency shift of 43 to 49 MHz for ammonia con- behavior, and better selectivity.
centrations ranging from 50 to 100 ppm and response time is
30 seconds. In Reference 8, a microwave resonator coated 2 | SYNTHESIS AND
with a PDMS layer act as an acetone sensor. The variation C H A R A C T E R I Z A T I O N OF
in the microwave resonance frequency is because of the SE NSITIVE MATER IAL
absorption-induced change in the permittivity of the sensi-
tive layer. Microwave-based gas sensors can be used in the This section outlines the laboratory procedure involved in
wireless sensor system. In Reference 2, the authors reported the synthesis of TiO2 and ZnO nanorods for use as sensitive
conductor-backed coplanar waveguides (CBCPW) with zeo- material for ethanol gas detection.
lite for sensing of toluene and the measurement is based on
amplitude variations of real and imaginary parts of imped-
ance for different concentrations at different frequencies. In 2.1 | Synthesis of TiO2
Reference 9, a technique based on SIW cavity resonators for Tetrabutylorthotitanate (TBT) is mixed with acetylacetone
ammonia gas detection operating at microwave frequency (ACA) in the equimolar ratio (1:1) to slow down the hydro-
with graphene as a sensing material is reported. Measure- lysis and condensation reaction. Forty milliliter of Millipore
ments showed that the resonant frequencies increase gradu- water (18.2 MΩ cm) is added slowly with the solution, and
ally with the injection time. In Reference 10, the researchers vigorously stirred for 10 min at room temperature. While
have deposited phthalocyanine thin films on microwave gas stirring, 30 mL of aqueous ammonia solution (28-30%) is
sensor substrate designed in stripline technology which will added in drops to the solution prepared. The resultant yellow
act as a sensor to ethanol, methanol, and acetone. In Refer- colored solution is then transferred to a Teflon-lined auto-
ence 11, microwave-based sensing measurements for the clave vessel and is placed in a silicone oil bath. Then auto-
detection of NH3 using titanium dioxide nanoparticles. clave contains the precursors which are heated to 170 C and
Numerous variables can be tracked using this technique, kept for 3 days without any interruption under stirring condi-
which improves the sensor differentiation capabilities tion. After 3 days, the autoclave is cooled to ambient tem-
through data crossing.11 Among all different detection mech- perature. The final product is washed several times with
anisms, the method relying on the shift of the resonant aqueous hydrochloric solution, 2-propanol, and Millipore
MOHAMMED ET AL. 3 of 10
2.2 | Synthesis and characterization of ZnO substrate is annealed at 350 C for 1 hour to improve the
crystalline nature of the ZnO nanorods grown.15 Figures 3
The FTO coated glass substrate is precleaned using Mil- and 4 show the XRD and FESEM images of the prepared
lipore water and ethanol in an ultrasonicator, prior to the
ZnO nanorods, respectively.
hydrothermal growth synthesis of ZnO nanorods and is dried
in room temperature. The preparation of seed solution
involves continuous stirring of Zinc acetate and potassium 3 | TWO-PORT MICROWAVE
hydroxide (KOH) at an equimolar ratio in 50 mL of ethanol RESONATOR DESIGN
using a magnetic stirrer. Then ZnO seed layer is deposited
on the substrate using the spin coating technique at This section presents the design and characterization of a
3000 rpm for 30 seconds. At last, the ZnO seeded FTO sub- two-port microwave resonator which is to be used as a
strate is annealed in a homemade furnace at 350 C for microwave transducing device. Further, this section also pre-
30 minutes and cooled to room temperature. The aqueous sents the experimental procedure adopted.
growth solution of ZnO nanorods is prepared by stirring the
zinc nitrate hexahydrate and hexamethylenetetramine
3.1 | Sensor design
(HMTA) at an equimolar ratio in a magnetic stirrer continu-
ously. This solution is then transferred to a stainless steel The geometry of the proposed two-port microwave sensor is
autoclave and kept inside a hot digital air oven at 90 C for shown in Figure 5. The resonator is developed on a 1.6 mm
4 hours and then cooled to room temperature. Finally, the thick FR4 glass epoxy substrate with dielectric constant 4.3
4 of 10 MOHAMMED ET AL.
Note: Concentration ethanol gas = 27.78*(frequency shift) + 21.69. FIGURE 15 Concentration of ethanol vs change in impedance
(TiO2 layer)
TABLE 3 Sensitivity of the proposed microwave gas sensor frequencies. Thus, the reported sensor is enabled to calculate
the gas concentration to provide accurate results on the pres-
Sensitivity
ence and the concentration of the gas to which it is exposed
Sl. No. Frequency Layer of TiO2 Layer of ZnO to. Unlike the single frequency microwave gas sensors, the
1 f1 = 2.2 GHz 1.275 2.321 proposed sensor is more reliable. In summary, the following
2 f2 = 4.6 GHz 1.295 2.355 are claimed to be the distinct features of the proposed micro-
3 f3 = 6.3 GHz 1.30 2.374
wave sensor.
Mean sensitivity 1.29 2.35
1. Sensor performance is evaluated in three frequency
bands for quick validation of the results. The results
ΔΓ Γ gas −Γ vacuum obtained in the three frequency bands can be used to
sensor response = = ð7Þ accurately sense the gas to which the sensor is
Γ Γ vacuum
exposed.
where Γ vacuum and Γ gas are the reflection coefficients 2. The sensitivity analysis is carried out using two different
before and after the introduction of the gas, respectively. sensing medium unlike the work reported in many other
Table 3 presents the sensitivity of the proposed microwave works of literature. An effective comparison is also
sensor at three different frequencies. The average sensitivity drawn to validate the claim that ZnO offers better sens-
of the microwave resonator with TiO2 nanoparticles as the ing performance than TiO2.
sensitive layer is calculated to be 1.29 while for ZnO 3. Some statistical analysis is carried to quickly determine
nanorods it is estimated as 2.35. With the measured sensor the concentration of the ethanol gas.
response to ethanol sensing device with ZnO nanorods as a 4. The performance is evaluated in both time domain and
sensitive layer showed higher sensitivity to ethanol while frequency domain and hence more valid results are
obtained using the proposed technique.
compared to that of using TiO2 nanoparticles as a sensitive
layer.
Thus from the experiments carried out above in both time
domain and frequency domain it is evident that the proposed 5 | CONCLUSION
sensor has a higher sensitivity toward ethanol gas detection.
Table 4 compares the proposed gas sensor with other exis- This article presented the design and implementation of a
ting sensors in literature. From the table, it is evident that the microwave-based ethanol gas sensor. The two-port reso-
proposed sensor offers higher sensitivity compared to other nator with triangular split ring structures designed to
sensors reported in the literature. Also, the three frequency operate at three frequencies was designed. In single fre-
measurement using a single microwave resonator is pro- quency testing, the reaction of other gases with the sensi-
posed for the first time. The gas reaction with the sensitive tive layer affected the frequency shift which decreased
layers creates different response at low, mid and high the accuracy of measurement whereas; in triple-frequency
T A B L E 4 Performance comparison
Performance
with other sensors reported in the
Frequency literature
Ref. No. Sensitive material T in C in GHz Sensitivity
3
Metallophthalo-cyanine 27 – 0.0150
22
Teflon 27 – 0.4000
23
Single-walled carbon nanotubes 19.5 0.1356 0.7610
(SWCNT)
5
SnO2 200-600 1-3a 0.1513
5
ZrO2 200-600 1-3a 0.3940
5 a
ZnSO4 200-600 1-3 0.2640
This work ZnO nanorods 27 2.2, 4.6, 6.3 2.35
This work TiO2 nanorods 27 2.2, 4.6, 6.3 1.29
a
The broadband measurement offers varying sensitivity throughout the bandwidth and the reliability is higher at
the upper-frequency edge.
MOHAMMED ET AL. 9 of 10
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A U T H O R B IO G R A P H I E S
Srinithya Rapuru is an undergraduate
student in the Department of ECE,
Gulam Nabi Alsath Mohammed
SSN College of Engineering.
received his BE, ME, and PhD degrees
from Anna University Chennai in the
years 2009, 2012, and 2015, respec-
tively. He is currently serving as an
Associate Professor in the Department
Tusharika Yarasi is an undergraduate
of Electronics and Communication
student in the Department of ECE, SSN
Engineering, SSN College of Engineering, Chennai,
College of Engineering.
India. His research interests include Microwave Compo-
nents and Circuits, Antenna Engineering, Signal integrity
Analysis, and Solutions to EMI problems. To his credit,
he has filed 12 patents and published several research
articles on antennas and microwave components in lead-
Navya Dommalapati is an undergrad-
ing International Journals. He has also presented and
uate student in the Department of ECE,
published his research papers in the proceedings of Inter-
SSN College of Engineering.
national and National conferences. He is currently serv-
ing as an Associate Editor in IET Microwaves Antennas
and Propagation.