2158 Vol. 60, No.

8 / 10 March 2021 / Applied Optics Research Article

Fiber optic evanescent wave humidity sensor

based on SiO2/TiO2 bilayer films
Xixi Huang,1,2,3 Min Lai,1,2,3,5 Ziming Zhao,1,2,3 Yang Yang,1,2,3 Jinze Li,1,2,3
Huatang Song,1,2,3 Jixiang He,1,2,3 Yan Ma,1,3,4,6 AND Bo Liu2,3
1
Jiangsu Collaborative Innovation Center of Atmospheric Environment and Equipment Technology (CICAEET), Nanjing University of Information
Science & Technology, Nanjing 210044, China
2
Jiangsu Key Laboratory for Optoelectronic Detection of Atmosphere and Ocean, Nanjing University of Information Science & Technology,
Nanjing 210044, China
3
School of Physics and Optoelectronic Engineering, Nanjing University of Information Science & Technology, Nanjing 210044, China
4
NUIST Reading Academy, Nanjing University of Information Science & Technology, Nanjing 210044, China
5
e-mail: mlai@nuist.edu.cn
6
e-mail: mayan@nuist.edu.cn

Received 30 November 2020; revised 29 January 2021; accepted 9 February 2021; posted 10 February 2021 (Doc. ID 416286);
published 2 March 2021

A SiO2 /TiO2 bilayer thin-film-based fiber optic humidity sensor was fabricated via a modified dip coating proc-
ess with enhanced sensitivity. SiO2 film was coated on the surface of the fiber core, followed by deposition of the
TiO2 layer on SiO2 . The relative humidity (RH) is measured by modulation in intensity of the transmitted laser at
room temperature. The optical fiber humidity sensor based on SiO2 /TiO2 film shows two-segmented linearity in
measurement with sensitivities of 5.35 and 1.94 µW/% RH at 15%–50% RH and 50%–95% RH, respectively. The
response time and recovery time are 25 s and 50 s, respectively. To our knowledge, the superior response time and
recovery time of the sensor in our study were achieved over those fiber optic humidity sensors reported with modu-
lation in intensity. Furthermore, this fiber optic humidity sensor has a good reproducibility and long-term stabil-
ity. The sensing mechanism is attributed to effects of moisture on the refractive index and the light absorption coef-
ficient of SiO2 film and modulation in the transmission characteristic of evanescent waves in the optical fiber. ©
2021 Optical Society of America

https://doi.org/10.1364/AO.416286

1. INTRODUCTION To enhance sensing performance, the mechanical structure

Humidity is closely related to scientific research, production,
human lives, and plant growth as an important indicator [1–3].
Humidity sensing has a wide range of demands and applica-
tions in agriculture, industry, environmental monitoring, and
other fields. At present, traditional humidity sensors are mainly
based on the modulation of electrical characteristics such as
resistance, impedance, and capacitance [4–8]. In these sensors,
various inorganic and organic materials and their composite
materials are employed as sensing parts [9–14]. However, these
sensors suffer from interference in strong electromagnetic
fields. In recent years, the development of fiber optic sensors has
attracted great attention based on modulation of optical signals,
including refractive index, power, frequency, and wavelength
[15–20]. In these fiber optic sensors, modulation in evanescent
wave absorption is a widely acclaimed technique today due to
its possibility of multiplexing and miniaturization, resistivity
to electromagnetic interference, high sensitivity, and in situ
measurement [21–23].
of fiber optic evanescent wave sensors has usually been tapered
including U-shape bending fiber [24,25], flexible waveguide
tube [26], and coiled fiber sensors [27]. Alternatively, the
sensing region was modified for improvement of sensitivity,
response, and recovery [28]. Due to their unique physical and
chemical properties, metal oxides including WO3 , SnO2 ,
ZnO, and SiO2 and their composites have been widely used as
sensing elements in gas and humidity sensors [29–32]. Porous
silica film was synthesized by a sol-gel process to develop a
low-cost fiber optic humidity sensor by coating on a U-shaped
optical fiber and doping with methylene blue [33]. The sensing
mechanism is based on scattering and absorption of evanescent
waves. Estella et al. [34] prepared silica xerogel film by the solgel
method as the sensing element in a fiber optic humidity sensor
working in a reflection mode. However, these sensors, more or
less, have some limitations for application. Porous structures
delay the sensing response and recovery. Although silica is a
good candidate for light transmission as the cladding of most
low-cost optical fibers, it is limited in the capability of moisture
absorption, which results in a relatively low sensitivity.

1559-128X/21/082158-08 Journal © 2021 Optical Society of America

Corrected 8 March 2021
 Research Article
Fig. 1. (a) Schematic structure and (b) sensing process of fiber optic
evanescent wave humidity sensor.
In this work, a fiber optic evanescent wave humidity sensor
based on SiO2 /TiO2 bilayer films is designed and fabricated,
which is shown in Fig. 1. In this sensor, the SiO2 layer is used
as a new cladding for the transmission of evanescent waves. The
TiO2 layer is hydrophilic and in favor of absorbing ambient
water vapor. The humidity measurement of this type of sensor
is based on the modulation in optical intensity, which decreases
with the increase of relative humidity (RH). It is basically attrib-
uted to the adsorption of water molecules on the surface of the
TiO2 film and its facilitating diffusion of water vapor to the
internal layer, which alters the refractive index and light absorp-
tion coefficient of SiO2 film and modulates the transmission
characteristic of evanescent waves in the optical fiber.
2. EXPERIMENT
All chemical reagents used in the preparation are analytical grade
without further purification.
A. Pretreatment of Optical Fiber
Plastic coating and cladding with a length of 5 cm was
mechanically removed at the center of an optical fiber (HPCF-
1000/1100-1400-37) with a length of 25 cm. The exposed glass
core was then immersed in acetone for 15 min, after which it was
dried in air and ready for use.
B. Preparation of SiO2 Film
The SiO2 film was prepared by an improved lifting method,
which was used to fabricate TiO2 thin film [35]. The reagents
used are dilute hydrochloric acid with pH = 1 , tetraethyl
silicate, and ethanol. Hydrochloric acid ( ∼37 wt.% ) was
diluted with de-ionized water to pH = 1 . 3.896 ml of tetraethyl
orthosilicate ( Si(OCH2 CH3 )4 ) and 18.311 ml of ethanol were
mixed. The mixed solution was then stirred on a magnetic stirrer
at room temperature, while 7.792 ml of dilute hydrochloric acid
was slowly added dropwise to the mixed solution, and stirred for
30 min. The solution was sonicated to form a suspension liquid.
The bare core of the optical fiber was put into the suspension
for 2 min, after which the fiber was taken out of the suspension
at a uniform speed and was then immediately purged with
nitrogen flow. This process was repeated for the preparation of
SiO2 films with different thickness. These samples are labeled
as SiO2 -x films, where x is the total treatment times of fiber in
mixedsolution through the procedure above. Finally, the optical
Vol. 60, No. 8 / 10 March 2021 / Applied Optics 2159
fiber was dried in oven at 90o C for 2 h.
C. Preparation of TiO2 Film
The TiO2 thin film was prepared on the top of the SiO2 film by
a modified lifting method [34]. Concentrated hydrochloric acid
was diluted with equal-volume de-ionized water. The mixed
solution was then stirred on a magnetic stirrer at room temper-
ature, while 0.8 ml of tetrabutyl titanate ( Ti(OC4 H9 )4 ) was
slowly added dropwise to the mixed solution, and stirred for 30
min. The solution was then hydrothermally treated at 130o C for
4 h and then cooled down to room temperature in a Teflon-lined
stainless-steel autoclave with a capacity of 100 ml. The solution
was sonicated to form TiO2 particle suspension. The fiber
coated with SiO2 film was dropped into the suspension for 2
min, and was then pulled out at a uniform speed. After that, the
fiber was purged with nitrogen flow immediately. This process
was repeated for the preparation of TiO2 films with different
thickness. These samples are labeled as TiO2 -x films, where x is
the total treatment times of fiber in mixed solution through the
procedure above. Finally, the optical fiber was dried in an oven at
90o C for 2 h.
D. Characterization
The x-ray diffraction (XRD) pattern of the SiO2 and TiO2
thin films was recorded with an x-ray diffractometer (XRD-
6100X, Shimadzu, Japan) at 40 KV and 30 mA using Cu Kα1
radiation ( λ = 0.154056 nm ). The surface morphological
characteristics were observed using a scanning electron micro-
scope (SEM) S-4800 (Hitachi, Japan) at an operating voltage of
3.0 kV.
E. Setup for Optical Humidity Sensing Tests
The experimental setup for humidity sensing tests of the fiber
optic sensor based on TiO2 /SiO2 film is shown in Fig. 2.
A 4 mW semiconductor laser with 650 nm wavelength was
employed as an input light source. A convex lens with a focal
length of 60 mm was placed to focus the beam and to couple
the laser into the fiber. The humidity control system consists
of a glass chamber, two flow meters (LZB-2), and a hygrom-
eter (HH654); the range of the hygrometer is 10%–99% RH.
One pipe of air passes through a flow meter and then leads to
de-ionized water to realize a humid gas. The other pipe of air
is dried by passing through CaCl2 powder. By controlling the
flow ratio of dry gas and moist gas, gases with different humidity
can be obtained. The electronic hygrometer in the device is used
for calibration. The film-coated optical fiber is fixed in the glass
chamber. A suitable incident angle is set between the laser beam
and the end face of the fiber in order to satisfy total reflection.
At the output end of the optical fiber, a light detector is used to
detect the output optical power varying with humidity. The data
is recorded in the computer by an Arduino program.
 2160 Vol. 60, No. 8 / 10 March 2021 / Applied Optics Research Article

Fig. 2. Schematic diagram of a sensing device for fiber optic humidity sensor based on SiO2 /TiO2 film.

3. RESULTS AND DISCUSSION
A. XRD Analysis
The XRD diffraction pattern of the SiO2 and TiO2 films is
shown in Fig. 3. No sharp peaks were observed for the SiO2
film, which indicated that the SiO2 film prepared by the sol-gel
method was amorphous. The peaks observed at 25.3◦ , 37.8◦ ,
48.0◦ , 53.9◦ , and 62.7◦ for the TiO2 film in the figure are con-
sistent with the crystal faces of anatase TiO2 structure (101),
(004), (200), (105), and (204) (JCPDS card No. 21-1272).
B. SEM Analysis
Figure 4 shows the surface morphology and microstructures of
the fiber core, the SiO2 film coated on the core, and the TiO2
film on the SiO2 film, respectively. The bare fiber core possesses
a smooth surface, which offers benefits for coating a smooth
film on it. The SiO2 film coated on the bare core exhibits a flat
surface with a moderate amount of nanopores, which is con-
ducive to adsorption of water molecules. After coating the TiO2
film, the loss of unique structure of the SiO2 film indicated
the TiO2 film fully covered the SiO2 film. A rough surface of
TiO2 film was achieved which resulted from the aggregation of
TiO2 particles during deposition. The thicknesses of the SiO2
layer and TiO2 layer of the sensor with SiO2 -2/TiO2 -3 are
estimated to be 375 ± 34 nm and 424 ± 48 nm , respectively.

C. Humidity Sensing
Fig. 3. XRD diffraction patterns of SiO2 film and TiO2 film. Sensitivity is generally considered to be the ratio of the change in
the output signal to the input signal. In this paper, sensitivity is

Fig. 4. Side-view SEM images of (a),(b) bare fiber core; (c),(d) SiO2 film coated fiber core; and (e),(f ) TiO2 film coated SiO2 /fiber core. (g),(h)
Cross-sectional SEM images of the sensor with SiO2 -2/TiO2 -3 films. Images in (g) and (h) were taken on the same site with different focuses.
 Research Article
defined as [36–38]
1P
Sensitivity = w/%RH, (1)
1%RH
in which 1P is the change of output power of the optical fiber,
and 1%RH is the corresponding change in relative humidity.
Figure 5 shows the average sensitivity of fiber optic sensors
coated with different layered SiO2 . Sample SiO2 -2 shows
the superior sensitivity with RH varying from 15% to 95%.
Less coating was probably unable to offer a sufficient length for
penetration of evanescent waves. However, excessive coating
resulted in a decrease of the efficiency of moisture transport
from the surface to the interior. The output power change of
the optical sensors based on SiO2 -2 film and TiO2 film pre-
pared by different coating times with increasing RH and the
corresponding average sensitivity are shown in Figs. 6(a) and
6(b). The sensor with TiO2 -3 film achieved the optimal average
sensitivity of 3.41 µW/% RH, which is probably attributed
to its suitable thickness for performance both in absorbing
ambient water molecules and in further transferring to the SiO2
layer. Moreover, the sensitivity of the sensors was significantly
enhanced after coating TiO2 film, which is attributed to the
hydrophilic nature of TiO2 film, i.e., the efficient collection of
moisture. Hence, the sensor with SiO2 -2 and TiO2 -3 films was
selected for further study hereafter in this work.
Fig. 5. Average sensitivity of fiber optic sensors with SiO2 films
prepared by different coating times with RH varying from 15% to
95%.
Fig. 6. (a) Variation of output power with increasing RH from 15% to 95% and (b) average sensitivity of fiber optic humidity sensors coated with
SiO2 -2 film and TiO2 -1 , TiO2 -2 , TiO2 -3 , and TiO2 -4 films.
Vol. 60, No. 8 / 10 March 2021 / Applied Optics 2161
The moisture absorption (from 15% RH to 95% RH) and
desorption processes (from 95% RH to 15% RH) of the fiber
optic sensor with SiO2 -2/TiO2 -3 bilayer films were studied at
room temperature, which is shown in Fig. 7. The results show
that there is a slight deviation in the optical power change curves
of humidification and drying. The average relative deviation of
the round-trip measurement is less than 0.67%, indicating that
the optical humidity sensor possesses an excellent reversibility in
the processes of increasing or decreasing the relative humidity.
This hysteresis is probably ascribed to the fact that the response
of the fiber optic humidity sensor in this work was faster than
that of the hygrometer for calibration in both vapor adsorption
and desorption processes [39].
As the ambient RH increases, the output power of optical
fiber decreases. In the range of low RH (15%–50% RH), the
output power drops sharply, while in the range of high RH
(50%–95% RH), the decreasing slope of output power reduces.
Figure 8 shows the two-segment linearity of the optical fiber
humidity sensor with sensitivities of 5.35 and 1.94 µW/% RH
at high relative humidity and low relative humidity, respec-
tively. It shows that the optical fiber humidity sensor has a good
linearity in both low and high RH ranges.
Figure 9 shows the transient output power profile of the
fiber optic sensor with SiO2 -2/TiO2 -3 bilayer films with RH
variation from 15% to 95%. The response time and recovery
time are 25 s and 50 s, respectively. To illustrate that the sensor
is superior to other humidity sensors in terms of response and
recovery time, Table 1 summarizes the comparison between the
humidity sensors studied in this work and those reported. The
fiber optic humidity sensor based on SiO2 -2/TiO2 -3 bilayer
films exhibits a fast response and recovery over those reported.
Gupta et al. [21] reported a highly sensitive fiber optic humidity
sensor based on phenol red doped polymethylmethacrylate film
with a response time of ∼5 s and humidity range of 20%–80%
RH. However, the humidity-control technique for sensing
test was different from that in this work, which might result in
different measurement of response time.
In order to study the reproducibility of the fiber optic humid-
ity sensor, the sensing performance in the range of 15%–95%
RH has been successively examined for three times, as shown
in Fig. 10. The variation characteristic of optical power nearly
 2162 Vol. 60, No. 8 / 10 March 2021 / Applied Optics Research Article

[41–43]. If the transmission wave of the light beam at the inter-

face between the fiber core and the cladding and the local area
near the reflection point is approximated as a local plane wave,
the plane wave field strength along the x direction (when x > 0
) is [44]
" s #
n 21
E 2 (x ) =E 20 exp(−kn 2 x ) 2 sinθi −1 exp[ j (βz−ωt)],
n2
(2)
where E 2 is the field strength in the cladding, E 20 is the initial
value of field strength in the cladding, β is the propagation
constant, ω is the angular frequency, ω = 2π/T , and T is the
period of vibration.
In this work, the external TiO2 layer of the fiber optic evanes-
Fig. 7. Variation in output power as RH increases (i) and cent wave sensor is hydrophilic and in favor of absorbing water
decreases (ii).
molecules in ambient, as shown in Fig. 1(b). With water trans-
ferring from the TiO2 layer to the SiO2 layer, the cladding
overlap, which shows that the fiber optic humidity sensor has a of optical fiber forms with a new refractive index of n 3 , which
good repeatability. affects the transmission of evanescent waves. If the core is sup-
The stability of the fiber optic humidity sensor based on posed to be a non-absorbing medium, the ratio of the output
SiO2 /TiO2 films was investigated by keeping the sensor at power to the initial power can be described as [44]
room temperature. The sensing performance was measured h
J 12 (U )
i h 2
I1 (W)
i
2 2
at different time intervals and the test result is shown in Fig. Pt (z) n 1 1 + J 2 (U )
+ n 3 exp(−αz) I02 (W)
−1
11. The sensing performance of each measurement remained = h0 , (3)
Pt (0) 2 (U ) i h 2
(W)
i
J I
basically unchanged, which indicated a high stability owing n 21 1 + J 12 (U ) + n 23 I12 (W) −1
0 0
to the excellent physical and chemical stability of SiO2 /TiO2
films. where Pt (0) is the initial power; Pt (z) is the output power;
J 0 and J 1 are the first type of Bessel functions; I0 and I1 are
the transformed Bessel functions of the second p kind; U is the
D. Humidity Sensing Mechanism normalized lateral phase parameter and U = r k 2 n 21 −β 2 ; r
The sensing mechanism for the bilayer film-based fiber optic is the core radius; α is the power absorption coefficient of the
sensors is attributed to the transmission of evanescent waves optical fiber; n 3i is the imaginary part of the cladding refractive
weaken in moisture. Evanescent wave is an electromagnetic index n 3 , i.e., the absorption coefficient; k is the wave vector
wave whose amplitude decays exponentially with increasing in mid-air; β is the propagation constant; and Wpis the nor-
depth perpendicular to the interface between core and cladding malized lateral attenuation parameter and W = r β 2 −k 2 n 22

Fig. 8. Linearity of optical fiber humidity sensor based on SiO2 /TiO2 film with RH of (a) 15%–50% and (b) 50%–95%.

Table 1. Comparison of Response and Recovery Time of Fiber Optic Humidity Sensors
Sensing Materials Mechanism Response Time Recovery Time Humidity Range References
SiO2 /TiO2 film Intensity 25 s 50 s 15%–95% This work
Polymethyl methacrylate Intensity 27 s 168 s 35%–85% [40]
Silica sol-gel film Intensity 30 s 180 s 0.025%–16.2% [33]
Porous silica xerogel film Intensity 120 s 120 s 44%–100% [34]
 Research Article
Fig. 9. Response and recovery time of optical fiber humidity sensor
based on SiO2 /TiO2 film.
Fig. 10. Repeatability of fiber optic humidity sensor.
. Based on the physical properties of optical fiber and coat-
ings, the transmission characteristics of light in the fiber optic
fiber are shown in Fig. 12. After adsorption of water vapor, the
refractive index of SiO2 cladding decreases, which results in
the decrease of the transmission characteristic Pt (z)/Pt (0) if
the absorption coefficient n 3i is constant. In addition, light
absorption of the cladding is enhanced with the exposure to
humid air. With a constant refractive index n 3 of the cladding,
the transmission characteristic of optical power exhibits a linear
decrease with the logarithmic increase of absorption coefficient
n 3i if n 3i < 5 × 10−6 . By overall effects on the refractive index
and absorption coefficient of the cladding with the exposure
to humid air, the output power of the fiber decreases with
increasing RH, which is consistent with the test results. When
n 3i > 5 × 10−6 , the transmission characteristic Pt (z)/Pt (0)
does not change with the variation of the absorption coefficient,
i.e., the optical power remains constant, which is ascribed to the
exp(−αz) in Eq. (3) approaching zero. A high RH may lead
to a high absorption coefficient of the SiO2 layer, which has
a negligible effect on the decrease of output power. Therefore,
the sensitivity is lowered compared to that in the low RH range,
which probably generate two-segment linearity of sensing.
Vol. 60, No. 8 / 10 March 2021 / Applied Optics 2163
Fig. 11. Stability of fiber optic humidity sensor.
Fig. 12. Relationship between transmission characteristic
Pt (z)/Pt (0) and the absorption coefficient n 3i . In the simula-
tion, the light wavelength, fiber radius, fiber length, and core refractive
index are 650 nm, 500 µm, 25 cm, and 1.52, respectively.
4. CONCLUSIONS
A fiber optic evanescent wave humidity sensor based on
SiO2 /TiO2 bilayer films has been fabricated by modulating
the intensity of laser transmitted. SiO2 film and TiO2 film
are employed as the optical fiber cladding and the humidity
sensitive material, respectively. Anatase TiO2 thin film was
coated by a modified dip coating method after deposition of an
amorphous SiO2 layer on the fiber core. The output power of
the transmitted beam decreased with increasing RH. Sensors
based on SiO2 /TiO2 bilayer films were superior on sensitivity
over those based on pure SiO2 films. The fiber optic humidity
sensor based on SiO2 /TiO2 film shows linearity in two seg-
ments in the whole measurement range of RH. The sensitivity
is determined to be 5.35 µW/% RH ( R 2 = 0.995 ) in the RH
range of 15%–50%, and 1.94 µW/% RH ( R 2 = 0.993 ) in
the RH range of 50%–95%. The response and recovery times
were determined to be 25 s and 50 s, respectively. In addition,
this fiber optic humidity sensor possessed a good repeatability
and long-term stability after aging. The sensing mechanism is
based on the absorption of moisture on the TiO2 film and also
 2164 Vol. 60, No. 8 / 10 March 2021 / Applied Optics
diffusion of water molecules promoted by the TiO2 film, which
leads to the change of the refractive index and light absorption
coefficient of the SiO2 film. The transmission characteristics
of evanescent waves in the optical fiber are modulated corre-
spondingly. The fiber optic humidity sensor may be applicable
in many sites such as remote online observation stations.
Funding. National Natural Science Foundation of China (41975172,
51472123, 51502143).
Acknowledgment. The authors thank J. Zhao for the discussion on
humidity test setup.
Disclosures. The authors declare no conflicts of interest.
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