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org Research Article

Smart Superhydrophobic Textiles Utilizing a Long-Range Antenna

Sensor for Hazardous Aqueous Droplet Detection plus Prevention
Kasra Khorsand Kazemi, Telnaz Zarifi, Majid Mohseni, Rakesh Narang, Kevin Golovin,*
and Mohammad H. Zarifi*

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ABSTRACT: This paper demonstrates the feasibility of a long-

range antenna sensor embedded underneath a liquid repellent
fabric to be employed as a wearable sensor in personal protective
fabrics. The sensor detects and monitors hazardous aqueous
liquids on the outer layer of fabrics, to add an additional layer of
safety for professionals working in hazardous environments. A
modified patch antenna was designed to include a meandering-
shaped resonant structure, which was embedded underneath the
fabric. Superhydrophobic fabrics were prepared using silica
nanoparticles and a low-surface-energy fluorosilane. 4 to 20 μL
droplets representing hazardous aqueous solutions were drop-cast
on the fabrics to investigate the performance of the embedded
antenna sensor. Long-range (S21) measurements at a distance of
2−3 m were performed using the antenna sensor with treated and untreated fabrics. The antenna sensor successfully detected the
liquid for both types of fabrics. The resonant frequency sensitivity of the antenna sensor underneath the treated fabric exhibiting
superhydrophobicity was measured as 370 kHz/μL, and 1 MHz/μL for the untreated fabric. The results demonstrate that the
antenna sensor is a good candidate for wearable hazardous aqueous droplet detection on fabrics.
KEYWORDS: antenna sensor, wireless sensing, liquid sensing, microwave sensing, patch antenna

I. INTRODUCTION biomedical applications, or drastically increase the fabrication

Personal protective equipment (PPE) is required to protect and implementation complexity. Therefore, functionalized PPE
professionals across many fields who work in hazardous with integrated sensors must be developed in tandem to better
environments, especially when dealing with toxic chemicals, protect workplace professionals.
Functionalized textiles or films that act as chemical barriers
radioactive substances, or pathogenic agents.1,2 Currently,
are a critical component of next-generation PPE. Spitz
efforts have been made toward improving the breathability,
Steinberg et al. demonstrated a breathable vapor toxicant
flexibility, and general comfort of PPE for firefighters,3 police
barrier based on graphene oxide, which allowed for the
officers,4,5 pilots,6 and military personnel.7,8 PPE has also been
selective transfer of water vapor while trapping toxic chemicals
functionalized to provide improved barriers as an additional
such as trichloroethylene and benzene.9 Although this
layer of safety against hazardous chemicals.9,10 However, this
technique provided a barrier against select organic agents,
additional layer may not protect against every hazardous
applications in the biomedical field require the resistance of
chemical and may degrade over time. In addition to
waterborne pathogens to mitigate infection transfer. Studies
functionalized PPE, protective textiles are used as a platform
have recently demonstrated the role of aqueous droplets and
for sensors and communication devices that can offer an
aerosols in infection transmission via talking, coughing, and
enhanced level of safety and awareness through sensing and
sneezing.18−20 This is especially important considering the
enabling faster responses to threats. Several reports present the
integration of PPE with various types of sensors, including fiber
optic sensors,11,12 electrochemical sensors,13 and enzyme- Received: April 29, 2021
based biosensors,14,15 for various purposes such as monitoring Accepted: July 2, 2021
the heart rate,11,12 respiratory rate, and skin temperature,12 or Published: July 13, 2021
detecting liquid or material residues and chemical threats on
PPE.13−17 However, these sensors require a substantial power
source, are costly and bulky for industrial and point-of-care

© 2021 American Chemical Society https://doi.org/10.1021/acsami.1c07880

34877 ACS Appl. Mater. Interfaces 2021, 13, 34877−34888
ACS Applied Materials & Interfaces
recent and rampant spread of the SARS-CoV-2 virus where
virus carrier particle sizes < 5 μm can remain airborne
indefinitely, and particle sizes of 100 μm can travel more than 6
m in distance. This serves as a path toward viral infection
transfer for healthcare professionals or scientists working with
hazardous pathogens.21 PPE has demonstrated a crucial role in
controlling and preventing airborne transmission of viruses,
such as SARS-CoV-2.22 Although hydrophobic PPE can assist
in preventing droplets and aerosols from permeating to the
skin, integrated sensors can serve as an early warning system,
alerting the professionals that their PPE has been exposed to
potentially hazardous droplets. Therefore, hydrophobic PPE
would be enhanced by parallel usage with sensors to provide
additional diagnostic information, particularly for biomedical
applications. Of the many available sensor technologies,
microwave sensors are attractive due to their real-time sensing
capability, feasibility in a diverse range of applications, cheap
fabrication and implementation requirements, and their ability
to be hybridized with superhydrophobic PPE.
Microwave sensing has recently demonstrated significant
potential in solid, liquid, and gas detection while operating in
wired or wireless systems by detecting changes in local
dielectric properties.23−28 It has proven to be accurate, non-
invasive, non-contact, sensitive, low-cost, and real-time for
material sensing applications.29,30 One of the leading structures
in microwave sensing are microstrip planar microwave
resonators.31 They are low-cost, easy to fabricate, planar,
compact, and compatible with complementary metal oxide
semiconductors (CMOSs).28,32−34 A microstrip planar micro-
wave resonator sensor is composed of a split ring resonator
(SRR) with a Gaussian-shaped frequency response.35−37
Current research has highlighted utilizing these resonators to
sense liquids, solids, and gases; 32,34,36,38−44 bacterial
growth;30,45−47 biomolecules;48 mechanical strain;49 and ice
deposits,50 a testament to the diversity of possible sensing
applications. However, in wireless sensing applications, planar
microwave resonators require additional apparatuses such as
antennas to act as a readout device for the remotely positioned
sensing structure to transmit the sensed signals to a remote
receiver.24,51−53 In order to fabricate a compact and efficient
device for sensing and transmitting the sensed signals, antenna-
based microwave sensors are currently being introduced for
long-range and wireless sensing applications.
Antenna sensors are able to act as sensors while
simultaneously maintaining their performance as a transceiver
unit for long-range communication between the sensor and
signal transducer. Antenna sensors are capable of collecting
data from their approximate environment or surface and
transmitting it to a receiver antenna. Recently, antenna sensors
have been used for material and liquid sensing.54−59 Yeo and
Lee designed and carved slots on a patch antenna as the
sensing regions, which exhibited a significant increase in the
sensitivity of an antenna sensor for large samples with different
permittivity values.54,55 Jun et al. designed and fabricated an
electromagnetic band gap (EBG) structure as a sensing spot
for liquid detection and positioned it beneath a microstrip
antenna.56 In their work, sensing was performed by monitoring
the S-parameter of the antenna. There have been other reports
of using antenna sensors to monitor temperature, strain, and
cracks, which validate the capability of these structures and
highlight the versatility of antenna sensors.60−62 Although
promising, these wireless sensors and antenna sensors are not
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suitable for the wireless sensing of liquid residues on PPE due
to their large size and low sensitivity to liquids and gases.
Currently, there have been reports of designing and
fabricating wireless sensing structures on fabrics and
textiles.63−67 In one study, a body area wireless sensor network
was designed and fabricated to monitor human physiological
signals.66 Stretchable passive tags with a skin-mimicking
interface were used on the body, and a flexible readout circuit
was implemented as an interrogator device for the tags where
the readout circuit had to be positioned in close range to the
tags (with a separation distance within the millimeter range).
The sensor network was used to monitor breath, pulse, and
movement. In another study, a wireless sensor network was
designed based on metamaterial textiles composed of two
layers of conductive textile and one layer of clothing.67 The
designed sensing network was used for wireless transmission of
personal health data over a distance of 10 cm. Despite their
advantages, these sensing structures suffer from a short
transmission range and are not optimized to detect hazardous
aqueous liquids.
This work presents fabric-based PPE consisting of a
modified patch antenna sensor and a superhydrophobic fabric.
The antenna consists of a meandering-shaped structure for
sensing and transmitting signals, forming a compact wireless
platform for long-range sensing and detection. Here, water
droplets were used to emulate hazardous aqueous droplets
from the human respiratory tract or other industrial droplets
containing hazardous water-soluble chemicals. The fabric,
treated with silica nanoparticles and fluorosilane, adds an
additional layer of safety in protecting the user against
hazardous aqueous droplets. This, in turn, keeps the fluid on
the outer surface of the fabric for standardized detection,
thereby creating more accurate results while protecting the
user from large splashes or tiny droplets of hazardous solutions.
The antenna is embedded underneath the treated and
untreated fabrics to perform sensing, where it is used to assess
the condition of the PPE prior to and during operation, as well
as to detect the hazardous liquid remaining on the fabric after
usage. The sensor exhibits a high sensitivity of 370 kHz/μL for
detection on the treated fabric and 1 MHz/μL on the
untreated fabric, with respect to the resonant frequency.
Further, the PPE comprised of the integrated sensor and
modified fabric is inexpensive to fabricate, does not need a
large power source, is not too bulky to implement in a
hazardous workplace, minimizes the permeation of water
through the fabric, and has a greater sensing range than other
comparable sensor technologies.
II. EXPERIMENTAL SECTION
II A. Materials. Tetraethyl orthosilicate (TEOS, 98 %) and
ammonium hydroxide (28.0−30.0 %) were purchased from Aldrich
and used without further purification. (Heptadecafluoro-1,1,2,2-
tetrahydrodecyl)triethoxysilane (95−100 %) was supplied from
Gelest. Ammonium persulfate (410) was purchased from MG
Chemicals. Ethanol (≥96 %) and methanol (≥99.8 %) were
purchased from VWR International (Radnor, PA). A Rogers RT/
duroid 5880 substrate was used for the fabrication of the microwave
structures, and a Keysight N5222B Vector Network Analyzer (VNA)
was used for the microwave spectrum measurements. Nylon/
polyurethane fabrics were used as the protective textiles suited for
PPE with a 91/9 nylon to polyurethane ratio.
II.B. Preparation of Superhydrophobic Fabrics. Super-
hydrophobic fabrics were prepared by applying a two-step formulation
via dip coating. The surface roughness of the fabrics was increased by
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Figure 1. Schematic of superhydrophobic fabric preparation using the dip coating of silica nanoparticles, followed by (heptadecafluoro-1,1,2,2-
tetrahydrodecyl)triethoxysilane.

the in situ growth of silica nanoparticles on the surface. The nanoscale
rough surface was then covered by low-energy surface fluorosilane, as
shown in Figure 1. For the first step, a methanol/deionized water
mixture with a weight ratio of 70/30 % was prepared. 6 vol % of
TEOS was added to this and magnetically stirred for 30 minutes to
achieve a homogeneous solution. The fabric was then immersed in the
TEOS solution with an L/R (liquor to goods ratio) of ∼17.5 w/w
while mixing the solution at 1200−1400 rpm. The temperature was
then elevated to 40 °C. 3.4 vol % of ammonium hydroxide was added
dropwise to the mixture, and the reaction was continued for 40
minutes. The nanoparticles were formed, and the solution changed to
an opaque colloidal suspension. The fabric was then removed from
the nanoparticle mixture and dried for 2 hours at room temperature.
In the second step, four different concentrations of the perfluorinated
silane in methanol (0.5, 1, 2, and 4 wt %) were prepared to find the
optimum silane concentration. The silica-treated fabrics were dipped
in the fluorosilane solutions with the L/R of ∼17.5 w/w at 25 °C for
10 minutes and then cured at 180 °C in an oven for 10 minutes.
II.C. Wettability Analysis, Surface Characterization, and
Durability Evaluation. Static water contact angle measurements
were performed using the sessile drop technique. 15 μL droplets of
water contact angle of washed or abraded textiles was measured after
each washing or abrading cycle.
II.D. Antenna Design and the Principle of Operation. A
microstrip patch antenna was designed in the ANSYS high-frequency
structure simulator (HFSS) to perform long-range sensing. Two
meandering lines were placed inside a carved rectangle in the center
of the patch antenna to create a sensitive region for the antenna
sensor when detecting materials over that region. These two
meandering-shaped microstrip lines were shorted to the ground
through a via on one end, while they were attached to the antenna on
the other end. Based on the quarter-wavelength matching theory,68 a
microstrip line with a length of λ/4, shorted to the ground, was
observed as an open-circuit component from the connected part of
the antenna at the associated frequency. The meandering lines were
designed to resonate at 3.2 GHz. The antenna was implemented on a
Rogers RT/duroid 5880 substrate. The width and the length of the
patch were derived for the frequency of 3.2 GHz using the following
relations:69
c
W=
2f0 εr + 1
2 (1)

ij yz
j zz
distilled water were deposited on the surface utilizing a 2 mL syringe

1 jjj zz
jj zz
(Gilmont), and the water contact angle was measured using a Ramé-
jj zz
jj 1 + 12 zz
hart goniometer (model 260-U1). The surface morphology and ε +1 ε − 1

j z
εeff = r + r

k {
elemental analysis of the fabrics were obtained from a scanning 2 2
electron microscope (Tescan Mira 3 XMU SEM) equipped with an ( Wh ) (2)
energy-dispersive X-ray analysis (EDS) module. A thin layer of
platinum (∼20 nm) was coated onto the textile surface to improve its L = Leff − 2ΔL (3)
electrical conductivity.
The elemental analysis was performed using energy-dispersive X- c
Leff =
ray spectroscopy in the point analysis mode at a 1.0 k× magnification, 2f0 εeff (4)

jij (εeff + 0.3) W + 0.264 ) zyzzzz

and the weight percentages of carbon (C), oxygen (O), silicon (Si),
j
ΔL = 0.412hjjjj
and fluorine (F) were scanned. The durability of the treated fabrics
z
(
jj (εeff − 0.258) W + 0.8 ) zzz{
was studied in terms of washing fastness and abrasion resistance. The h

washing fastness test was carried out according to ISO 105 C06.
Briefly, the modified textiles with 100 mm × 40 mm (L × W)
dimensions were immersed in 4 % w/v AATCC 1993 standard
reference detergent without an optical brightener and stirred
mechanically at 40 °C. The textiles were removed after 30 minutes
of stirring at 40 rpm, rinsed twice with warm water (40 °C), and then
dried at ambient temperature. The abrasion resistance of the treated
fabrics was investigated using Martindale abrasion according to ISO
12947. The modified textiles were mounted to the instrument and
abraded with the felt abrader in a standard Lissajous pattern. The
k (
h (5)
Here, c is the speed of light (3.0 × 10 m/s); εr and h corresponds to
8
the permittivity and height of the substrate; and W, L, and εeff
correspond to the width, length, and effective permittivity of the
patch, respectively. The length of the patch was modified for a good
return loss acquisition, which minutely altered the resonant frequency
of the resonator. The width of the meandering lines was 0.43 mm, and
they merged at their connection point to the via. Simulations were
performed in HFSS to evaluate the performance of the designed

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Figure 2. (a) Designed antenna sensor’s dimensions; (b) simulated antenna results for the two mentioned stages, with and without the sample
material; (c) far-field gain simulation results for the antenna sensor in the E-plane; (d) far-field gain simulation results for the antenna sensor in the
H-plane; and E-field concentration on the meandering lines, (e) without the sample and (f) with the sample.

antenna in the far-field. The final dimensions of the formulated
resonator are presented in Figure 2a. As observed in the simulation
results (Figure 2b−d), the patch antenna with meandering microstrip
lines and via termination had a resonant frequency and a resonant
amplitude of 3.11 GHz and −27.74 dB, respectively, and the far-field
gain observed was 5.6 dB. The far-field radiation pattern of the
antenna is presented in Figure 2c,d.
Further simulations were conducted in order to investigate the
sensitivity of the designed antenna sensor, which was implemented on
a Rogers RT/duroid 5880 substrate. According to the simulation
results, the meandering microstrip line region was chosen for
sensitivity investigation. A simulation sample of Roger RT/duroid
6006 (εr = 6.15) was placed on the meandering microstrip line region
as the simulations revealed that this region was the most sensitive
region of the antenna sensor (Figure 2e,f). The meandering-shaped
structure on the antenna had a high E-field concentration compared
to the other regions of the antenna sensor. Moreover, the E-field
concentration on the periphery of the meandering lines was higher for
the antenna with a sample on its surface as compared to the bare
antenna. Positioning the sample on the meandering line caused a
change in the effective permittivity, which in return shifted the
resonant profile of the antenna sensor, as shown in Figure 2b. As
dictated by eq 4, a change in the effective permittivity causes a change
in the resonant frequency of the antenna. The simulation results
(Figure 2b) show that the operational frequency was 3.049 GHz for
the antenna with the sample on its meandering line, which resulted in
a 62 MHz frequency shift compared to the initial 3.11 GHz operating
frequency. The simulations were continued for the antenna sensor’s
far-field gain to observe the gain change in the presence of the sample
on the meandering lines. Sample placement on the meandering
microstrip lines of the antenna sensor caused a gain reduction to 3.7
dB (Figure 2c,d). Therefore, the simulation results indicated that the
designed antenna sensor would be able to sense the sample by a
change in its S11 parameter and transmit the alterations to a distanced
receiver. The simulations also showed that the antenna sensor
maintained a good gain profile and radiation pattern even with a
sample on its surface, as shown by the relatively high gain. Thus, the
presence of the sample on the antenna sensor will not cause
significant attenuation in the antenna’s performance.
Simulations were also performed to evaluate the sensitivity of the
sensor to water with different conductivity values. A water sample
with a dielectric constant of εr = 81 was used in these simulations,
while the sample material’s conductivity was altered between 0 and 4
S/m. The conductivity of the sample with σ = 0 S/m represented pure
water, and the sample with σ = 4 S/m could represent seawater. The
achieved results are presented in Figure 3. The sample with σ = 0 S/m

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Figure 3. Simulation results for water with conductivity values ranging
between 0 and 4 S/m.
had a resonant frequency and a resonant amplitude of 3.03 GHz and
−13.7 dB, respectively. The results show that increasing the
conductivity would cause the resonant frequency of the antenna
sensor to shift to a higher frequency, while the resonant amplitude
would also increase. For instance, a sample with a conductivity of σ =
1 S/m would shift the resonant frequency and resonant amplitude to
3.045 GHz and −12.79 dB, respectively. Further, samples with σ = 2
S/m and σ = 4 S/m demonstrated resonant frequencies of 3.048 and
3.052 GHz, respectively, while the achieved resonant amplitudes for
the samples were −12.07 and −10.79 dB, respectively. The results
indicate that the meandering-shaped structure has good sensing
performance for materials with low conductivity. Moreover, the
simulations show that the designed antenna sensor structure is able to
differentiate water samples with different conductivities. The
simulations were followed by the fabrication of the antenna sensor
and the measurement of its performance.
II.E. Antenna Sensor Fabrication and the Experimental
Setup. The simulated planar patch antenna sensor was fabricated on
a Rogers RT/duroid 5880 substrate with a dielectric thickness of 1.56
mm, a relative permittivity of 2.2, and a loss tangent of 0.0009, with
copper cladding on both sides. A conventional chemical etching
method for printed circuit board fabrication was utilized to
manufacture the antenna with a fabrication error better than ±0.1
mm. The sensor pattern was laser-printed on glossy paper and heat-
transferred on the substrate to preserve the copper from the etchant.
The substrate was then placed inside a solution of ammonium
persulfate etchant for 30 minutes to implement the antenna sensor
structure on the substrate surface. After 30 minutes, the patch
structure was washed with acetone to remove the ink, and a
Subminiature version A (SMA) connector was soldered to the edge of
the microstrip feed structure.
Two fabric swatches with a size of 10 cm × 10 cm and a thickness
of 0.6 ± 0.1 mm were prepared to study the performance of the
antenna sensor for liquid detection in the presence of the treated and
untreated fabrics. Either treated or untreated fabrics were placed over
the antenna to cover the antenna sensor’s top surface. The fabrics
were pinned to Styrofoam to avoid mechanical movement and
electrical instability during the experiments. Prior to the experimental
testing of the sensor and based on the type of fabric used in this work,
the antenna sensor was also calibrated indoors and outdoors in order
to avoid the effects of humidity and temperature changes in the
sensing performance of the antenna sensor. This calibration allowed
the sensor to operate reliably at a greater range of temperatures and
humidity.
Further baseline measurements and calibration processes were
performed before running the experiments to suppress the impact of
initial values such as the fabric thickness and the presence of the
coating on the final measurements of the liquid samples. Different
volumes of water were used to validate the performance of the textile-
covered antenna sensor. The deposited water droplet volumes were 4,
8, 12, 16, and 20 μL. Initially, three different regions were chosen on
the antenna sensor surface to investigate the sensitivity of the device
and compare the results to the simulated values.
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The transmission line, antenna surface, and meandering-shaped
structure were used for sensitivity investigation, and two sets of
experiments were performed to evaluate the antenna sensor’s
performance. In the first experiment, the reflection coefficient (S11
parameter) of the antenna sensor was used to distinguish between
different liquid samples on the sensor. A measurement setup was
prepared, in which a VNA measured the reflection coefficient. The
VNA was calibrated for 2001 points, a 5 dBm microwave power, and
an IF bandwidth of 300 Hz. Broadband microwave absorbers (600
MHz−40 GHz) from ECCOSORB, AN-79, sized 24″ × 24″ × 4.49″,
were utilized under the antenna which surrounded the measurement
setup in order to reduce the impact of reflection and interfering
signals on the measured profile of the antenna sensor.
In the second test, the long-range performance of the antenna
sensor was studied by measuring the transmission coefficient(S21
parameter) between the antenna sensor and an ultra-wideband
antenna (UWB). The measurement setup consisted of an RFspace
TSA 900−12,000 ultra-wideband PCB tapered slot antenna with an
operational frequency range of 900 MHz to 12 GHz, a Keysight
N5222B VNA, and the antenna sensor. The distance between the
antenna sensor and the interrogator antenna was fixed at 2.3 m. Here,
the transmitted signal of the patch antenna sensor was absorbed by
the UWB slot antenna (the readout device), where it was displayed in
the readout as a transmission (S21) parameter. The VNA was
calibrated for 3601 points, a 5 dBm power, and an IF bandwidth of
300 Hz. Both the sensor and interrogator antennas were aligned to
minimize the polarization loss factor (PLF) as both had linear
polarization. The same microwave absorbers described above were
used to minimize any interference signals during the experiment.
III. RESULTS AND DISCUSSION
III A. Performance of Superhydrophobic Fabrics. The
superhydrophobic fabrics formed a robust Cassie−Baxter state
on the surface in which air pockets were trapped in the
surface’s porosity and the capillary resistance prevented the
transition from the non-wetting Cassie−Baxter state to the
wetted Wenzel state. Silica nanoparticles were used to increase
the nanoroughness on the fabric’s surface, and the surface
energy was reduced by applying fluorosilane on the nano-
roughened surface. Upon preparing the superhydrophobic
fabric, water contact angles were measured for each
concentration of fluorosilane used in the solution. The water
contact angle showed a significant increase from 152° ± 7° to
164° ± 7° as the fluorosilane concentration increased from 0.5
to 1 wt % and then slightly decreased to 156° ± 3° and 160° ±
3° by further increasing the fluorosilane concentration to 2 and
4 wt %, respectively (see Table 1). These results indicated that
Table 1. Static Water Contact Angle of Treated Fabrics with
Various Concentrations of (Heptadecafluoro-1,1,2,2-
tetrahydrodecyl)triethoxysilane in Methanol
formulation fluorosilane percentage (wt %) water contact angle (°)
F-0.5 0.5 152 ± 7
F-1 1 164 ± 7
F-2 2 156 ± 3
F-4 4 160 ± 3
grafting the fluorosilane to the hydroxy-rich silica nanoparticle
surfaces was sufficient with 1 wt % of fluorosilane. Further
increasing the fluorosilane concentration likely produced
unwanted side reactions, that is, self-condensation of the
trifunctional molecules. Therefore, the solution of 1 wt %
fluorosilane in methanol was chosen as the optimum
concentration as it displayed the highest contact angle and a
good combination of surface nanoroughness and low surface
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energy (see Figure 4). This sample was chosen for further
surface morphology and durability characterization.
Figure 4. SEM images of (a) untreated fabrics, (b) fabrics treated
with the silica nanoparticles with the optimized fluorosilane solution
(the magnified view is presented in the lower right panel), and (c)
abraded superhydrophobic fabrics after 1000 Martindale abrasion
cycles.
The surface morphologies of the untreated fabrics and
optimized treated fabrics are presented in Figure 4a,b,
respectively. The fibers of untreated textiles exhibited a
smooth surface with minimal roughness. The elemental
analysis of the surface revealed 56.8 wt % C, 43.2 wt % O, 0
wt % Si, and 0 wt % F on the surface. After treating the surface
of the fabric, the spherical nanoparticles were detectable on the
surface with an average particle size of ∼212 ± 8 nm. The
elemental analysis of the surface showed 51.4 wt % C, 38.0 wt
% O, 9.2 wt % Si, and 1.5 wt % F, indicating successful
deposition of silica nanoparticles and fluorosilane on the fabric
surface.
The washing fastness of the treated superhydrophobic
fabrics is presented in Figure 5a. The water contact angle of
the treated fabrics with 1 wt % fluorosilane was 164° ± 7°
before washing and was later reduced to 145° ± 2° after 15
washing cycles, still exhibiting water repellency. The water
contact angle of treated fabrics was also measured after 100,
250, 500, and 1000 Martindale abrasion cycles according to
ISO 12947. The water contact angle of the treated fabric
decreased from 164° ± 7° to 145° ± 4° after 100 abrasion
cycles. It then further reduced to 136° ± 3° after 500 cycles
and finally plateaued at approximately 131° ± 3°, as shown in
Figure 5b. The SEM image of the superhydrophobic fabric
after 1000 Martindale abrasion cycles is presented in Figure 4c.
Although the fabric exhibited a significant decrease in the
number of adhered nanoparticles, the ones still adhered to the
surface of the fabrics resulted in a water contact angle greater
than 130°. These experiments demonstrated the durability of
the treated fabric and indicated that the fabric finish was
suitable for long-term and reusable PPE applications.
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Figure 5. (a) Washing fastness of the superhydrophobic fabrics
according to ISO 106 C06. (b) Abrasion resistance of the
superhydrophobic fabrics according to ISO 12947.
III.B. Antenna Performance. Figure 6a presents the
fabricated antenna sensor and the size of the patch and
meandering lines. Two dyed water droplets were deposited on
the treated fabric to demonstrate the enhanced hydrophobicity
compared to the untreated fabric (Figure 6b,c). The measured
scattering parameter (S11) of the fabricated antenna sensor was
compared against the antenna sensor’s response when covered
with the treated and untreated fabrics (Figure 6d). Covering
the antenna with the fabrics affected the resonant frequency
and the resonant amplitude of the S11 profile by shifting the
resonant frequency to a lower frequency, from 3.220 GHz for
the bare resonator to 3.206 and 3.201 GHz for the untreated
and treated fabrics, respectively. Similarly, the resonant
amplitude changed to −25.0 and −22.4 dB for the untreated
and treated fabrics, respectively, whereas the bare antenna
sensor demonstrated a resonant amplitude of −23.3 dB.
The change in the S11 response of the antenna sensor could
be related to the permittivity change in the antenna sensor’s
proximity, where in this case the fabric affected the permittivity
of the antenna sensor, i.e., εeff. When relating to eq 4, the
resonant profile, namely, the resonant frequency (f 0), is
affected when the effective length retains its value while the
permittivity changes. The S11 response of the antenna can be
explained by S11 = (Z − 1)/(Z + 1), Z = Zin/Z0, where Z0 is
the characteristic impedance of the structure, which equals 50
Ω as a standard number for microwave systems.
In this case, the input impedance (Zin) of the antenna
sensors relies on the structure size and design, the substrate
material, and the dielectric constant of the materials in the
antenna sensor’s environment. Covering the surface of the
antenna sensor with fabrics and further depositing liquids
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Figure 6. (a) Fabricated antenna sensor with a patch length (L) of 36.5 mm, a patch width (W) of 22 mm, a meandering microstrip line length of
42 mm, and a width of 0.5 mm. (b) Antenna sensor covered with the treated fabric (dyed water is shown beading up on the fabric). (c) Antenna
sensor covered with the untreated fabric (water is shown to be absorbed into the fabric). (d) Measured S11 profile of the bare antenna sensor,
compared with treated and untreated fabrics.
changes the permittivity of the antenna sensor’s environment,
which would change the S11 response of the antenna sensor.
The downshift in frequency agrees with the simulation analysis,
although the resonant amplitude differs due to the local
permittivity being vastly different in the simulation environ-
ment (RT/duroid 6006) as opposed to an experimental trial
incorporating treated and untreated fabrics.
III.C. Liquid Sensing with the Antenna Sensor. A
measurement setup was prepared for a single port (S11) test to
perform liquid sensing, as depicted in Figure 7a. Three
different regions on the antenna sensor were investigated to
confirm the antenna’s most sensitive region for material
sensing purposes, as compared to the simulation. The results of
these experiments are compared in Figure 7b, where the
designed meandering shape microstrip line region demon-
strated the highest sensitivity to an 8 μL droplet of water. The
bare antenna displayed a return loss of −23.4 dB at a resonant
frequency of 3.22 GHz. By drop casting the 8 μL droplet of
water on the antenna sensor's sensitive region, the impedance
changed between the antenna and VNA’s power source. This
changed the power transmitted to the antenna, and the
resonant frequency subsequently shifted to 3.17 GHz, a 50
MHz reduction. The other regions of the antenna and
transmission line displayed no sensitivity to the water droplet
as no frequency shift was observed in the measurement results.
However, it should be noted that although an 8 μL water
droplet exhibits a >1 mm diameter, large droplets from sneeze,
coughing, or splashes from industrial chemicals in hazardous
workplaces can still exceed this droplet size after accumulation
and coalescence. Moreover, some studies have shown that the
droplet sizes in sneeze or cough are not limited to a specific
34883
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value and that there is a continuum of droplet size in a cough
or sneeze.70,71
The antenna sensor’s performance was validated by
detecting 4 to 20 μL water droplets deposited over the
sensitive region of the antenna sensor both while the sensor
was bare and while it was covered by the treated or untreated
fabrics. The results in Figure 7c show a significant change in
the resonant frequency for different volumes of water. The
measured resonant frequencies were 3.206, 3.195, 3.185, 3.175,
and 3.153 GHz for 4, 8, 12, 16, and 20 μL droplets,
respectively. The results validate the antenna performance for
detecting small volumes of water from 4 to 20 μL. Moreover,
the measured results for treated and untreated fabrics are
compared in Figure 7d,e, where the sensitivity of the sensor
covered with the treated fabric to the water droplet was found
to be 350 kHz/μL (R2 = 0.942). In contrast, the sensor’s
sensitivity was found to be 1.1 MHz/μL (R2 = 0.866) when it
was covered with the untreated fabric. The sensitivity
difference between the coated and uncoated fabrics was
expected due to the coated fabric’s tendency to repel the water
droplet, keeping it further from the sensitive region of the
sensor. Therefore, the water droplet had less impact on the
effective dielectric properties in the sensor’s approximate
environment.
The resonant amplitude of the antenna sensor also
demonstrated good sensitivity to the presence and volume of
the water droplets deposited on the treated and untreated
fabrics. However, the resonant amplitude should not be used as
the sensor’s response since the amplitude for an antenna sensor
varies with the distance between the antenna sensor and the
interrogator antenna, multipath signal reflection, and unknown
obstacles. It should be noted that a slight deviation from
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ACS Applied Materials & Interfaces www.acsami.org Research Article

Figure 7. (a) Antenna sensor’s measurement setup. (b) Sensitivity comparison on the different regions over the antenna sensor. (c) Comparison of
S11 parameters for a bare sensor with different volumes of water. Comparison of the resonant notch frequency and the resonant amplitude of the
antenna sensor for (d) treated fabric and (e) untreated fabric for water volumes deposited over the sensitive region, ranging from 4 to 20 μL.

linearity was observed with the treated fabric due to the exact
placement of the droplet on the fabric. However, these results
are still valid due to the high goodness of fit, R2 = 0.942, and
the distance between the droplets was within the micrometer
range. This deviation can be seen to a greater extent with the
untreated fabric (R2 = 0.866). Here, the water spread and wet
the fabric surface, which caused a more significant deviation, as
the effective permittivity changed over a larger area above the
resonator. This experiment showed that using superhydro-
phobic textiles in PPE provides greater protection for
professionals that require safety against hazardous liquids
soaking into the fabric. However, the sensitivity of the
microwave resonator was compromised to a value of 750
MHz/μL. Nonetheless, both sensing conditions achieved a
high standard for sensing potentially hazardous aqueous
solutions.
III.D. Long-Range Liquid Detection on the Treated
and Untreated Fabrics. A measurement setup was prepared
to validate the antenna sensor’s performance by measuring the
transmission coefficient (S21 parameter) between the bare
antenna sensor and an interrogator antenna located 2.3 m
away. Figure 8a shows the experimental setup for the long-
range measurement using the antenna. Transmission measure-
34884
ments between the antennas were compared for the bare
antenna, the antenna covered by the treated fabric, and the
antenna covered by the untreated fabric (Figure 8b). The
results showed that the resonant frequency and the resonant
amplitude changed from 3.231 GHz and −34.14 dB for the
bare antenna sensor to 3.194 GHz and −42.47 dB, and 3.191
GHz and −34 dB for the sensor covered by the treated and
untreated fabrics, respectively. These values for the resonant
frequency and resonant amplitude were used as the baseline for
the antenna sensor’s response for the rest of the experiments
with water droplets. Droplets with volumes of 4−20 μL were
placed over the sensitive region of the antenna to demonstrate
the efficacy of the antenna sensor in liquid droplet detection
for the treated and untreated fabrics. Figure 8c compares the
resonant frequency and the resonant amplitude for the
untreated fabric, where the 4−20 μL water droplets were
deposited on the sensing region.
Due to the wetting and spreading of the droplet into the
fabric, the resonant frequency was downshifted by 90 MHz and
the resonant amplitude dropped 4 dB for one 20 μL droplet.
As shown in Figure 8c, increasing the water droplet volume on
the untreated fabric not only created a large downward
frequency shift but also degraded the quality factor from 67
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ACS Applied Materials & Interfaces www.acsami.org Research Article

Figure 8. (a) Setup for long-range liquid detection on the fabric. (b) S21 measured results for the bare antenna and the antenna covered with the
treated fabric and untreated fabric. The resonant frequency and resonant amplitude response of the antenna sensor covered by (c) untreated and
(d) treated fabrics for water volumes deposited over the sensitive region, ranging from 4 to 20 μL.

with no droplet to 40 with a 20 μL droplet. Figure 8d presents Table 2 summarizes the resonant parameters of the antenna
an experiment with similar volumes on the same spot of the sensor with treated and untreated fabrics for 4 and 20 μL
antenna sensor but covered with the treated fabric. The droplets of water. The results show that the designed antenna
presence of a 20 μL water droplet shifted the resonant sensor was capable of sensing the presence of water on its
frequency by 12 MHz, which was around 8 times smaller than surface and transmitting the sensing data as a signal to a
the sensor’s response with the untreated fabric. distanced receiver for both treated and untreated fabrics.
As observed in the measurement results, positioning water
droplets on the fabric caused changes in the effective Table 2. Impact of Water Droplets on the Antenna Sensor’s
permittivity of the antenna sensor’s sensing region, which Response
caused a shift in the resonant frequency according to eqs 1−5.
resonant
A smaller shift in the resonant frequency was observed for the resonant frequency amplitude quality
treated fabric as compared to the untreated fabric. This was antenna sensor (GHz) ±0.0001 (dB) ±0.001 factor
due to the hydrophobicity of the treated fabric, which untreated no 3.192 −33.88 67
prevented the water sample from soaking into the textile, fabric drop
4 μL 3.169 −34.87 54
causing a smaller change in the effective permittivity of the drop
sensing region (Figure 8a inset, colored droplets). Comparing 20 μL 3.102 −38.25 40
the −3 dB quality factor of the measured S21 profiles revealed drop
that the quality factor of the treated fabric was slightly larger treated no 3.196 −42.7 70
fabric drop
than the quality factor of the untreated fabric with the water
4 μL 3.193 −42.8 69
droplets deposited on the fabric. This difference could be drop
utilized to identify treated or untreated fabrics and monitor the 20 μL 3.189 −43.1 66
lifetime of the finished fabric. drop

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ACS Appl. Mater. Interfaces 2021, 13, 34877−34888
ACS Applied Materials & Interfaces
Although the antenna sensor had a greater sensitivity to liquids
when the untreated fabric was placed on its surface, a greater
deviation from linearity was observed. This was due to the
water that soaked into the untreated fabric, as opposed to the
water beading up on top, as observed with the treated fabric.
On the other hand, the treated fabric maintained an air gap
(Cassie−Baxter state) between the antenna sensor and the
liquid sample, which reduced the sensor’s sensitivity.
Regardless, the antenna sensor showed a 12 MHz shift for a
20 μL droplet, which is sufficient for detecting the liquids.
IV. CONCLUSIONS
A patch antenna sensor was integrated with a robust and
durable superhydrophobic fabric for the construction of PPE
capable of detecting and repelling aqueous hazards. The
spherical silica nanoparticles with an average size of ∼212 ± 8
nm were synthesized on the fabrics using an in situ sol−gel
method. The silica-treated surface was then modified by a low-
surface-energy fluorosilane methanol solution with an
optimum concentration of 1 wt %. The elemental analysis
revealed 9.2 wt % silicon and 1.5 wt % fluorine on the surface.
The treated fabrics showed suitable durability as a protective
garment, and the water contact angle remained up to 145° ±
2° and 145° ± 4° after 15 washing cycles and 100 abrasion
cycles, respectively. Different areas of the antenna sensor were
investigated to find the most sensitive region through
simulations and experiments. Water droplets were used as
the test material to replicate hazardous aqueous solutions
found in an industrial workplace or generated by talking,
sneezing, and coughing. Measurements on the sensor showed
that the meandering-shaped section of the developed micro-
wave resonator was more sensitive than the other regions. The
designed antenna sensor was embedded under treated and
untreated fabrics to investigate its liquid sensitivity in both
configurations.
Single-port (S11) and transmission (S21) measurements were
performed for the treated and untreated fabrics, where water
droplets were deposited on the fabrics in volumes of 4, 8, 12,
16, and 20 μL. The antenna sensor sensed the presence of the
water droplets on both fabrics for both single-port and
transmission measurements. Changes in the resonant fre-
quency and resonant amplitude were observed for both sets of
measurements. It was demonstrated that the treated and
untreated fabrics had resonant frequencies of 3.196 and 3.192
GHz, respectively. Moreover, the presence of a 20 μL water
droplet on the antenna senor caused 90 and 12 MHz
downward shifts for untreated and treated fabrics, respectively.
This sensing response certifies the antenna sensor’s application
for the detection of hazardous aqueous liquids on the outer
layer of PPE fabrics. However, future work should integrate an
array of antenna sensors on PPE and fabrics to enhance the
safety of the wearer. The sensing capability of the device
should also be expanded beyond hazardous aqueous solutions.
Other droplet volumes and solutions beyond water should be
tested to validate and calibrate those hazardous liquids as
sensing targets for the proposed antenna sensor, such as
mucous particles or other industrial chemicals. This would be
necessary as other solutions have varying permittivity and
dielectric properties when compared to water. Moreover,
modifications can be made to the antenna sensor to facilitate
gas sensing on PPE such that the antenna sensor would be
applicable to a wider range of applications and environments.
Finally, an investigation can be performed on the selectivity of
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the sensor within possible high-frequency ranges, where the
microwave signal can also resonate with the target aqueous
hazardous liquid samples.
■ AUTHOR INFORMATION
Corresponding Authors
Kevin Golovin − Okanagan Polymer Engineering Research &
Applications Laboratory, School of Engineering, University of
British Columbia, Kelowna V1V 1V7 British Columbia,
Canada; orcid.org/0000-0001-8309-7458;
Email: kevin.golovin@ubc.ca
Mohammad H. Zarifi − Okanagan MicroElectronics and
Gigahertz Applications Laboratory, School of Engineering,
University of British Columbia, Kelowna V1V 1V7 British
Columbia, Canada; orcid.org/0000-0001-5544-3966;
Email: mohammad.zarifi@ubc.ca
Authors
Kasra Khorsand Kazemi − Okanagan MicroElectronics and
Gigahertz Applications Laboratory, School of Engineering,
University of British Columbia, Kelowna V1V 1V7 British
Columbia, Canada; orcid.org/0000-0002-9385-4173
Telnaz Zarifi − Okanagan Polymer Engineering Research &
Applications Laboratory, School of Engineering, University of
British Columbia, Kelowna V1V 1V7 British Columbia,
Canada; orcid.org/0000-0003-4376-7087
Majid Mohseni − Okanagan Polymer Engineering Research &
Applications Laboratory, School of Engineering, University of
British Columbia, Kelowna V1V 1V7 British Columbia,
Canada; orcid.org/0000-0003-0976-4771
Rakesh Narang − Okanagan MicroElectronics and Gigahertz
Applications Laboratory, School of Engineering, University of
British Columbia, Kelowna V1V 1V7 British Columbia,
Canada; orcid.org/0000-0001-5690-6379
Complete contact information is available at:
https://pubs.acs.org/10.1021/acsami.1c07880
Notes
The authors declare no competing financial interest.
■ ACKNOWLEDGMENTS
The authors acknowledge the Syilx Okanagan Nation for use of
their unceded territory, the land on which the research was
conducted. We acknowledge support from the Natural
Sciences and Engineering Research Council of Canada
(NSERC) through grant RGPIN-2018-04288. The authors
thank The Mathematics of Information Technology and
Complex Systems (Mitacs) Accelerate program through
grant no. IT16812. The authors thank the Canada Foundation
for Innovation (CFI) through grants nos. 38148 and 37904, as
well as CMC Microelectronics for their software licenses. The
authors acknowledge Brad Field at PRE Labs Inc. for
generously providing the fabric samples. The authors acknowl-
edge the financial support of the Department of National
Defense (contract nos. W7714-196839 and W7714-186568).
■
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