Optical Sensing:

Microstructured
Fibers, Fiber
Micromachining,
and Functional
Coatings
Minghong Yang, Dongwen Lee,
and Yutang Dai

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 Optical Sensing:
Microstructured Fibers, Fiber Micromachining,
and Functional Coatings
by Minghong Yang, Dongwen Lee, and Yutang Dai
doi: http://dx.doi.org/10.1117/3.2195943
PDF ISBN: 9781628416718
epub ISBN: 9781628417937
mobi ISBN: 9781628417944

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Spotlight vol. SL03

Last updated 30 April 2015

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 Table of Contents
1 Introduction 1
2 Fiber-Optic Sensing Concepts Using Functional Coatings on a Fiber Tip 2
2.1 Porous oxide coating with Fabry–Perot structure on fiber tip for
relative-humidity sensing 2
2.2 Multilayer coating on sapphire fiber tip for high-temperature sensing 10
3 Integration of Functional Materials with Fiber Micromachining for
Advanced Sensing Applications 15
4 Microstructured Fiber with Functional Materials for Optical Sensing
Engineering 20
4.1 Microstructured fiber with functional materials for hydrogen sensing 20
4.2 Integration of Pt/WO3 hydrogen-sensitive material with selectively
infiltrated PCF for hydrogen sensing 26
5 Conclusion 30
References 30

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 SPIE Spotlight Series

Welcome to SPIE Spotlight eBooks! This series of tutorials is designed to educate

readers about a wide range of topics in optics and photonics. I like to think that
these books address subjects that are too broad for journal articles but too concise
for textbooks. We hope you enjoy this eBook, and we encourage you to submit
your ideas for future Spotlights online.

Robert D. Fiete, Series Editor

Exelis Geospatial Systems

Editorial Board Members

Aerospace and Defense Technologies Rick Kendrick (Lockheed Martin)

Biomedical Optics/Medical Imaging Brian Sorg (National Cancer Institute)

Electronic Imaging and Signal Majid Rabbani (Kodak)

Processing

Energy and the Environment Paul Lane (US Naval Research Lab)

Optical Design and Engineering Rich Youngworth (Riyo, LLC)

Semiconductor Technology Stefan Preble (Rochester Institute of Technology)

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 Yang, Lee, and Dai: Optical Sensing 1

1 Introduction
In optical sensing, the most recent and important enabling technologies are based
on either the longitudinal or transverse structuring of fibers. Bragg gratings are a
typical example of the longitudinal structuring of fibers, while microstructured
fibers [e.g., photonic crystal fibers (PCFs)] are the promising enabling technology
in terms of transverse structuring of fibers. Microstructured fibers provide materi-
als with dispersion characteristics unattainable with conventional materials, as
well as otherwise unfeasible physical characteristics that can be tailored to spe-
cific sensing applications.
Functional materials can be realized on the side- or end-face of fiber with
many techniques, including sputtering, thermal evaporation, spin-coating, and so
on. The combination of fiber optics with nanostructure technologies and func-
tional materials offers great potential for the realization of novel sensor concepts.
Miniature optical fiber sensors with functional coatings and thin films as sensitive
elements could open new fields for optical fiber sensing applications. Functional
coatings work as sensitive elements and transducers to get response and feedback
from the environment, while optical fibers are employed here as carriers of sens-
ing signals.
This Spotlight presents a general overview of the integration of microstruc-
tured fiber, fiber micromachining, and functional coatings for optical sensing engi-
neering. The structure of this Spotlight is designed as follows: Section 1 gives a
short introduction to these specific fiber sensor concepts and the outline of this
Spotlight. Section 2 introduces the integration of optical fibers with functional
coatings on the fiber tip for optical sensing applications, and two concrete exam-
ples including an optical fiber humidity sensor and sapphire fiber high-tempera-
ture sensor are given. A multilayer coating of TiO2 ∕SiO2 ∕TiO2 can be deposited
on the fiber tip for a relative-humidity (RH) sensing application, or one
can deposit a multilayer of ZrO2 ∕Al2 O3 ∕ZrO2 on a sapphire fiber tip for high-
temperature sensing up to 1000°C. Section 3 introduces the integration of fiber
micromachining with functional materials for optical sensing. Using femtosecond
laser micromachining, different microstructures can be generated on fiber. When
functional materials are deposited on such a microstructured fiber, an advanced
performance can be expected, especially for fiber-optic sensing engineering. As
an example, microstructured fiber coated with a TbDyFe magnetostrictive can
greatly improve magnetic field sensing. Section 4 introduces the integration of a
microstructured fiber with functional coatings for optical sensing applications.
PCF is one of the very enabling technologies in terms of transverse structuring
of fibers, and when it is integrated with functional coatings, new directions for
sensing applications can be expected, including hydrogen sensing by combining
hydrogen-sensitive materials (such as a Pt-doped WO3 coating and a Pd-alloy thin
film). An example of such an integration is demonstrated in this Spotlight.
Section 5 is a short conclusion.

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 2 Yang, Lee, and Dai: Optical Sensing

2 Fiber-Optic Sensing Concepts Using Functional Coatings

on a Fiber Tip
Fiber-optic sensors have many distinctive characteristics, such as small size, flex-
ibility, and immunity to electromagnetic interference.1–3 For example, there
already exists a fiber-optic temperature sensor—a fiber Bragg grating (FBG)—
that enables temperature measurement with a sensitivity of 0.1°C. Several optical
fiber RH sensors based on different configurations have also been reported, such
as long-period gratings (LPGs), 4 tilted fiber Bragg gratings, 5 U-bend, 6 and
hetero-core optical fibers.7,8 These sensors rely on the fiber’s response to the sur-
rounding environment, and to generate secondary effects such as refractive index
(RI) change or strain on the sensing fiber that result in a shift of output spectra or
change in intensity. Alternatively, one can use functional materials for fiber-optic
sensing; in these cases, functional materials sense changes of the surrounding
environments such as humidity, temperature, and gas concentrations. As FBGs
can only be used for temperature or stress sensors, the applications of such intrin-
sic fiber-optic sensors are limited. Combining fiber optics with functional materi-
als has the potential to open many new applications for fiber-optic sensing. In this
Spotlight, fiber-optic sensors for RH and high-temperature sensing are presented
as examples of fiber-optic sensing concepts with functional coatings on the
fiber tip.

2.1 Porous oxide coating with Fabry–Perot structure on fiber tip for
relative-humidity sensing
Using functional coatings on the fiber tip as sensitive elements, a fiber-optic sen-
sor enabling simultaneous measurement of humidity and temperature is proposed
and demonstrated. The sensing probes are a porous oxide multilayer deposited on
the fiber tip, which is realized by e-beam evaporation without ion-source assis-
tance, to form a thin-film Fabry–Perot interferometer (FPI). FPI sensors are
extremely sensitive to perturbations that affect the optical path difference (OPD)
between two reflective mirrors, and the sensing region can be very compact to
ensure the miniature size of the sensor. There are two sensing probes in the sys-
tem; one is sensitive to environmental humidity changes, and the other is sealed
in a glass tube for temperature measurement.
The RH of an air-water mixture is defined as the ratio of the partial pressure
of water vapor (H2 O) in the mixture to the saturated vapor pressure of water at
a given temperature. Here, the saturated vapor pressure of water is correlated with
temperature; the correlation presented by Buck9 is commonly encountered in the
literature and provides a reasonable balance between complexity and accuracy:

eðT Þ ¼ ð1.0007 þ 3.46 × 10−6 PÞ × ð6.1121Þeð240.97þT Þ ;

17.502T

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 Yang, Lee, and Dai: Optical Sensing 3

Figure 1 Schematic diagram of the TiO2 ∕SiO2 ∕TiO2 multilayer sensor for relative-humidity
(RH) measurement [(a) unsealed probe] and temperature measurement [(b) sealed probe].

where T is the air temperature expressed in degrees Celsius (°C) and P is the
absolute pressure expressed in hectopascals. In this way, the RH can be correlated
with the changing temperature.
The miniature optical fiber humidity sensing probe consists of three-layer
optical thin films deposited on a multimode fiber (MMF: 62.5 nm∕125 nm) tip
as shown in Fig. 1. The first and third layers are TiO2 coatings that are employed
as mirror layers. A very thick SiO2 coating is used as a cavity layer in the F–P
structure. The coatings are deposited by evaporation technology where a porous
microstructure in the coating is realized. The sensing mechanism is based on the
change of the reflected interference spectrum when water molecules are absorbed
in the porous oxide coating, which means the change of the effective RI; as a
result, this will shift the interference fringes. Therefore, the drift of the FPI fringes
is correlated with the variation of humidity level.
The dielectric thin films manufactured by e-beam evaporation without ion-
source assistance have columnar and porous structures.10 When the TiO2 and
SiO2 porous coatings absorb water molecules from the environment as the result
of capillary condensation,11–13 their effective RI will change. In this way, the cor-
relation of the humidity level with the effective RI of the films is maintained.
Variations in the RI of dielectric films affect the propagation of light in the
element, which in turn leads to a phase change. Figure 2(a) shows the theoretical
simulation of the interference fringe shift of the proposed three-layer F–P struc-
ture when the effective RI has a 1% and 2% increase. The third interference fringe
dips are located at 526.6, 530.9, and 535.4 nm, respectively, in the case of the
original fringe, and correlate with a 1% and 2% increase in the effective RI
increase. The means 4.3 and 8.8 nm of characteristic wavelength drift exists when
the effective RI increases 1% and 2% when compared to the original fringe.
As mentioned above, RH in a sealed system varies with the change of envi-
ronmental temperature. This can be employed for the principle of temperature
sensing. Figure 2(b) plots the change of RH in a sealed system with a changing
temperature under different original levels of RH. It can be concluded that RH

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 4 Yang, Lee, and Dai: Optical Sensing

70
2% Neff increase
60 1% Neff increase
Orginal fringe
50
Reflectance (%)

40

30

20

10

0
450 500 550 600 650 700 750
Wavelength (nm)

(a) (b)

Figure 2 (a) Simulated spectral drift of the multilayer sensor with 1% and 2% effective
refractive index change and (b) calculated RH shift with temperature change in a sealed
system.

inside the sealed F–P sensor decreases with an increase of the surrounding tem-
perature. As for the temperature measurement in the work, the sensing probe with
a similar porous thin film coating is sealed in a glass tube, thus it is isolated from
the environmental humidity change. However, when the environmental tempera-
ture changes, the RH in the sealed tube will change. In this way, the interference
fringe drift is correlated with the RH change in the sealed metal tube and is also
correlated to the environmental temperature change.
A three-layer FPI structure was realized on an MMF tip by e-beam evapora-
tion, by which it is possible to control the structural and morphological properties
of the deposited thin film by optimization of the deposition process parame-
ters.14,15 In this experiment, the basic vacuum pressure of the coating chamber is
set at 0.01 Pa, oxygen (O2 ) with a velocity of 100 sccm is supplied as procedure
gas, and the fiber sample baking temperature is set at 100°C. The first and third
layers are 168.55 nm TiO2 film with a deposition rate of 0.2 nm∕s, while the
second layer is a 1621.34 nm SiO2 film with a deposition rate of 0.5 nm∕s.
The dielectric coatings are realized without ion-source assistance, which enables
the porous structure.
The multilayer dielectric thin films were deposited on fibers using physical
vapor deposition, and adhesion between dielectric thin films is fine due to the
continuous physical deposition; in some cases, ion-source assistance is employed
for a better adhesion between thin films. The adhesion between thin films and
fiber can also be optimized by changing deposition parameters such as the tem-
perature and so on. The proposed sensor can still work well after 1 year, which
shows the good performance of the multilayer thin film attachment to the fiber.
The experimental setup shown in Fig. 3 consists of a broadband light source
(BBS; HL-2000 Tungsten Halogen Light Sources from Ocean Optics, wavelength

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 Yang, Lee, and Dai: Optical Sensing 5

Figure 3 Experimental configuration for simultaneous measurement of humidity and

temperature.

range: 360 to 2500 nm), miniature fiber spectrometer (S3000-VIS Micro

Spectrometer made by Seeman Technology, wavelength range: 320 to 1050 nm,
wavelength resolution: 0.3 nm), multimode optical fiber coupler, and the pro-
posed F–P sensor probe working in the reflection mode. During sensing charac-
terization experiments, the light emitted from the Tungsten Halogen BBS goes
to the optical coupler, and one output port is connected to the optical spectrum
analyzer (OSA) for measuring the reflected optical spectrum, while the second
output port is fusion spliced with the fabricated RH sensor. The two sensors are
connected to the system with an optical switch; one sensor is used for RH meas-
urement and the other is sealed in a glass tube for temperature measurement.
Considering its flow ability and rapid solidification, the ultraviolet curing adhe-
sive was used to seal the temperature sensing probe into the glass tube (the pack-
aging was finished in the room environment, about 50%RH, 25°C).
The fiber-optic humidity sensor was enclosed in an accurate humidity gener-
ator (Model SRH-1 made by SHINYEI, Japan) with a high performance dew
point hygrometer for calibration. The RH can be varied from 1.6 to 90%RH with
a control accuracy of 0.1%RH. Figure 4(a) shows the packed sensor in a sealed
glass tube for temperature measurement; both sensors have the same multilayer
coating as the sensitive elements. A key issue to the manufacture of the fiber-optic
humidity and temperature sensor is to realize and control the porous structure in
the oxide films. The microstructure of the deposited multilayer samples was
investigated by the scanned TEM as shown in Fig. 4(b). It can be clearly demon-
strated that the coating is porous in microstructure, and the pore size is between
20 and 50 μm, depending on the deposition process.
Figure 5(a) shows the actual spectrum in the wavelength region of 450 to
750 nm measured by the miniature fiber spectrometer (time of exposure 510 ms,
time sampling interval 5 ms) under 10, 30, and 70%RH, respectively. There exist
several spectral dips of minimum reflectivity in the spectral region. Since the
wavelength position of minimum reflectance will drift due to the effective RI
change of the coating material because of the absorption and desorption of water
molecules, each spectral peak can be regarded as a characteristic wavelength of

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 6 Yang, Lee, and Dai: Optical Sensing

Figure 4 (a) Schematic diagram of the packed temperature sensor and (b) scanning elec-
tron microscope image of the sensing coating.

the humidity sensing measurement. It can be observed that the interference fringe
shows a redshift when the RH increases, which corresponds to an increase in the
effective RI of the sensing films. This can be explained as follows: when the RH
increases, the dielectric coating absorbs more water molecules from the atmos-
phere, and the increase in the number of water molecules (RI ¼ 1.33) filling air
pores (RI ¼ 1) in the coating will lead to an increase in the effective RI in the
sensing films.
The measurement results were analyzed, the shift of the characteristic wave-
length to different RH levels is fitted and plotted in Fig. 5(b), and it can be
found that the average humidity sensitivity of the proposed sensor is approxi-
mately 0.43 nm/%RH. Moreover, it should be mentioned that the spectrum shift
reaches 8.2 nm in the RH level ranging from 1.8 to 14.3%RH (humidity sensing
test lower than 1.8%RH is not available because of the limit of the experimental
device), which means an RH sensitivity of 0.66 nm/%RH. It can be concluded
that the fiber-optic humidity sensor is more sensitive at lower RH levels,

Figure 5 (a) Reflection spectra of the porous-film sensor at different RH levels and (b) the
shift of the characteristic wavelength in response to different RH levels.

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 Yang, Lee, and Dai: Optical Sensing 7

Figure 6 (a) Cross-sensitivity to temperature of the proposed unsealed humidity senor and
(b) characteristic dip wavelength of the sealed temperature sensing probe under different
RH levels.

whereas its wavelength shift at higher RH levels is not apparent. This can be
understood by the fact that the micropore easily absorbs water molecules due
to the capillary condensation effect, while at higher RH levels, the micropore is
easily saturated.
Temperature cross-sensitivity is a main concern for the unsealed RH sensor,
therefore, cross-sensitivity to temperature was investigated as for the proposed
F–P fiber-optic humidity sensor. Characteristic wavelength shifts of the fiber sam-
ple at different RH levels were tested at 15°C, 25°C, and 35°C, respectively.
Figure 6(a) shows the relation of the temperature effect to the humidity measure-
ment. It can be concluded that the temperature cross-sensitivity is rather low, with
a characteristic wavelength shift of less than 2 nm within 20°C of temperature
change, while the change is typically more than 20 nm when the RH level
changes from 20 to 80%RH. As for the proposed F–P temperature sensor, the sen-
sor head is packed in a sealed system. Cross-sensitivity to an environmental
RH change should be avoided to ensure accurate temperature measurement.
Figure 6(b) shows the stability of the characteristic dip wavelength of the sealed
F–P temperature sensor under different environmental RH levels, while the
temperature is kept at 20°C. It can be concluded that the sealed F–P sensor
head is insensitive to RH, which means the sealing of the sensor by ultraviolet
curing adhesive is good and the cross-sensitivity to the RH of the sealed sensor
can be ignored.
Temperature response of the sealed F–P sensor is observed and the spectral
shift under different temperatures from 21.4°C to 38.8°C is plotted and shown
in Fig. 7(a); it is found that the characteristic dip wavelength presents a blueshift
with the increase of temperature. The correlation of the wavelength shift to tem-
perature is generated as shown in Fig. 7(b). Compared to the unsealed RH sensor
that shows a redshift with the increase of the RH level, the sealed temperature

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 8 Yang, Lee, and Dai: Optical Sensing

Figure 7 (a) Reflection spectra of the sealed multilayer sensor at different temperature lev-
els and (b) the shift of the characteristic wavelength with different temperatures.

presents a blueshift with the increase in temperature. The blueshift caused by tem-
perature can be explained by Kelvin’s equation
2M γ cos θ
rK ¼
RρT × ln H
where rK is a Kelvin radius, H is the RH, γ is the surface tension, R is the univer-
sal gas constant, T is the temperature in Kelvin, ρ and M are the density and
molecular weight of water, respectively, and q is the contact angle. The capillary
condensation can take place in pores with a radius less than rK at a particular RH
and temperature. rK decreases when the temperature increases or RH decreases,
and the adhesion of the vapor molecules in the coating is reduced, which results
in the decrease of the effective RI.
Experiments for sensing repeatability, response time, and stability are also
studied; the sensing experiments have been repeated four times in order to inves-
tigate the measurement repeatability. Wavelength shifts of the proposed sensor
under different humidity and temperature levels in the both ascending and
descending phases are shown in Fig. 8. The measurement results are quite stable
at each humidity and temperature reading, taking into account the reading error
of 0.3 nm. The sensor can still function even if it is over saturated; the sensor
was immersed in water or alcohol several times and it could still function nor-
mally after drying in air.
The response time of the sensor was also evaluated. The sensor was placed in
14.3 and 60.5%RH moisture conditions supplied by saturated salt solutions of
LiCl and NaBr in bottles. A few cycles were performed to determine the repeat-
ability, rise time, decay time, and hysteresis of the sensor. The spectrum move-
ment was recorded with a rate of 1 frame∕s, and the peak shift is plotted as
shown in Fig. 9. Experimental results show that the sensor has a response/recover

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 Yang, Lee, and Dai: Optical Sensing 9

Figure 8 Repeatability tests of (a) the unsealed RH sensor and (b) the sealed temperature
sensor.

time of 5 s between 14.3 and 60.5%RH. As to the sealed temperature sensor, the
response time is more than 20 s from 20°C to 40°C because of the delay of heat
transfer. Furthermore, the stability of the proposed sensor was also examined.
Figure 9 shows the characteristic wavelength shift when the unsealed RH sensor
was held at 41%RH and the sealed temperature was held at 26°C for 12 h. The
data were recorded at 3-min intervals. Only small fluctuations are observed,
which demonstrates the good stability of the proposed fiber-optic RH and temper-
ature sensor. The small random errors displayed in Fig. 9 can be attributed to a
slight instability of the microspectrometer and temperature change during
recordings.
Using a multilayer oxide thin film as the RH functional coating on an optical
fiber tip, a fiber-optic sensor enabling simultaneous measurement of humidity and
temperature is proposed and demonstrated. The sensing elements are multilayer

Figure 9 (a) Time response of the unsealed RH sensor and (b) the shift of the characteristic
wavelength over time for 12 h when the unsealed RH sensor was held at 41%RH and the
sealed temperature was held at 26°C.

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 10 Yang, Lee, and Dai: Optical Sensing

porous films deposited on the fiber tip by e-beam evaporation. RH sensing is cor-
related with the shift of the interference fringe due to the change of the effective
RI of the porous coatings when exposed to different RH environments. In the case
of temperature measurement, the sensor is sealed in a glass tube. Experimental
results show that the average sensitivity is 0.43 nm/%RH and 0.63 nm∕°C,
respectively, when the environmental RH changes from 1.8 to 74.7%RH and tem-
perature changes from 21.4 to 38.8°C. The cross-sensitivity to temperature change
for the RH sensor and to humidity change for the temperature sensor is low.

2.2 Multilayer coating on sapphire fiber tip for high-temperature

sensing
Similar to the structure of the fiber-optic RH sensor mentioned above, a three-
layer F–P cavity structure with dielectric oxide coatings is realized on a sapphire
fiber tip as the high-temperature-sensing element. However, the sensing principle
is somewhat different. The RH sensor works based on the effective RI change due
to the absorption and desorption of water content, while in the case of the fiber-
optic high-temperature sensor, the effective RI change is caused by the thermo-
optic efficiency, which is associated with the temperature change.
Due to its advantages including miniature design, electromagnetic immunity,
and durability to harsh environments, numerous optical fiber high-temperature
sensors have been developed in the past decades. High-temperature sensors using
FBG and LPG inscribed in special optical fibers are proposed,16–20 and fiber-optic
temperature sensing schemes based on fluorescence detection are demon-
strated.21,22 Recently, optical fiber high-temperature sensors based on FPI have
been proposed for their unique advantages of high resolution, simple configura-
tion, and low cost. FPI high-temperature sensors created by micromachining and
microstructured fibers23–25 are reported. However, all of the above mentioned
components have problems for practical applications such as complex fabrication
processes and fragile structures. With a functional high-temperature coating as the
sensitive element, a novel sensor with a multilayer thin film deposited on the tip
of a sapphire fiber as an extrinsic FPI for temperature measurement is proposed.
Sapphire fiber is well-accepted for its long-term stability at high temperatures up
to 1800°C, and a dielectric oxide multilayer is coated on the sapphire fiber tip
as the sensitive elements; therefore, the proposed sensor has the miniature size
of the sapphire fiber itself. The proposed sensing component is simple in physical
structure and robust in mechanical stability. Such a sensor is also capable of batch
fabrication and has potential in industrial applications.
The schematic diagram of the sensing head is shown in Fig. 10. Three layers
of ZrO2 ∕Al2 O3 ∕ZrO2 (ZAZ) dielectric materials were deposited on the tip of
a sapphire fiber to generate an extrinsic FPI. Alumina (Al2 O3 ) and zirconium
dioxide (ZrO2 ) were selected as the lower and higher RI materials, because this
kind of RI combination provides high temperature stability, a thermal expansion

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 Yang, Lee, and Dai: Optical Sensing 11

Input light

Reflected light

ZrO2/Al2O3/ZrO2
Sapphire fiber multilayer

Figure 10 Schematic diagram of a thin film temperature sensor.

coefficient similar to sapphire, and a higher RI contrast.26,27 The sensing principle

is that RI and the thickness of the deposited oxide films will increase with the
increase in the surrounding temperature due to the thermo-optic and elastic-optic
effects. This will change the OPD of the thin-film interferometer, which results
in shift of the interference spectra. When the surrounding temperature changes
from T 0 to T , the OPD change of the thin film cavity can be expressed by
ΔOPD ≈ ðan þ ad ÞðT − T 0 Þ. Here, an and ad are the first-order coefficients of
the thermo-optic effect and the thermal expansion, respectively. In this way, a
correlation of the temperature change with the interference spectra shift is main-
tained. By monitoring the drift of the reflected interference fringe at different
temperature levels, the environmental temperature under test can be extracted.
Normally, a single layer on a sapphire fiber can also present an interference
spectrum, but it is not possible to optimize the interference effect in such a case.
Instead of a single layer, a three-layer structure is employed to enhance the
intensity and visibility of the reflected spectrum. Figure 11 shows the simulated
reflections of a 300 nm single ZrO2 layer, 300 nm Al2 O3 layer, and 283 nm
ZrO2 ∕1396 nm Al2 O3 ∕283 nm ZrO2 three-layer structure, respectively. It is clear
that the ZrO2 ∕Al2 O3 ∕ZrO2 structure has better visibility than the single layer.

Figure 11 Theoretical interference fringes of sensors.

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 12 Yang, Lee, and Dai: Optical Sensing

Figure 12 Sapphire fiber tip with as-deposited multilayer.

Figure 12 shows the image of a sapphire fiber tip with the deposited multi-
layer of 283 nm ZrO2 ∕1396 nm Al2 O3 ∕283 nm ZrO2 . It can be concluded that
the coating on the sapphire fiber is smooth and free of cracks. The sample was
annealed at 1000°C three times with a temperature increase speed of 2°C∕ min.
Following that, it was kept at 1000°C for 10 h for thermal stability and then
cooled down to room temperature. For contrast, Fig. 13 shows the image of the
annealed samples of the sapphire fiber tip with multilayer coatings. It can be
found that the coating is still stable even after baking at 1000°C three times. It
should also be pointed out that the surface changes roughly compared to the as-
deposited sample. But this is acceptable since there is still an interference fringe
even with such a rough surface. Additionally, no clear crack can be detected,
and only a few contaminations can be found on the surface.
The experimental temperature increase was monitored by a standard B-type
thermocouple, and the thermocouple was collocated at exactly the same position
as the multilayer-coated sapphire fiber tip to avoid a temperature difference due
to the nonuniform thermal distribution in the furnace. The experimental curve of

Figure 13 Multilayer on sapphire fiber after 1000°C annealing.

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 Yang, Lee, and Dai: Optical Sensing 13

Figure 14 Experimental curve of temperature increase.

the temperature increase was recorded as shown in Fig. 14, which demonstrates
that the OPD of the thin-film interferometer on a sapphire fiber tip has a correla-
tion with temperature change as mentioned above. Figure 15 shows the recorded
OPD during the temperature increase up to 1000°C. It can be gleaned from
Figs. 14 and 15 that the OPD has a very similar evolution trend as its status
changes, including a temperature increase, holding, and decrease. This has

Figure 15 Experimental optical path difference (OPD) curve during temperature increase.

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 14 Yang, Lee, and Dai: Optical Sensing

Figure 16 Recorded reflection spectrum of sapphire fiber with coating.

demonstrated that such a proposed sapphire fiber with a multilayer coated on the
fiber tip can be suitable for high-temperature measurements up to 1000°C.
Figure 16 shows the measured reflection spectrum of the sapphire fiber with a
multilayer coating as the sensitive elements. The spectrum will shift with the
temperature change. Figure 17 shows the repeated measurement of the sensing
calibration. It is clear that the two curves match well at a temperature above
400°C.

Figure 17 OPD versus temperature of two thermal cycles.

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 Yang, Lee, and Dai: Optical Sensing 15

3 Integration of Functional Materials with Fiber Micromachining

for Advanced Sensing Applications
Laser ablation is an efficient fabrication technology and a promising microma-
chining technique for many hard and brittle materials.28–31 Due to its high peak
power, short pulse, and other excellent properties, femtosecond laser processing
has been widely applied in many fields including fiber-optic sensing.32,33 This
Spotlight introduces a novel device for a static magnetic field through microma-
chining a spiral microgroove into the FBG cladding and then sputtering a
Terfenol-D functional coating into the microgrooves. Femtosecond laser process-
ing was employed to ablate the microgrooves. The schematic of the microstruc-
ture is shown below.
From Fig. 18, it can be found that a certain thread L0 is manufactured by the
femtosecond laser. Two kinds of pitches were realized with femtosecond-laser
micromachining, namely 60 and 80 μm. The diameter of cladding D is 125 μm,
and a TbDyFe film was directly coated in the microgrooves, thus, a primarily
new type of magnetic sensing probe was successfully made.
In order to achieve the three-dimensional (3-D) microstructure on the clad-
ding, a femtosecond laser, as shown in Fig. 19, was applied during fabrication.
The laser system is based on a 180 fs titanium-sapphire regenerative amplifier
system, which has a maximum single pulse energy of 1.1 mJ and repetition rates
between 1 and 1000 Hz. The 3-D moving stage has a movement range of 100,
100, and 25 mm in the X -, Y -, and Z-direction, respectively. All three stages
were driven by linear direct current motors. The laser beam (a Gaussian mode
beam) would finally be focused on the targets by the objective lens with a focal
length of 60 mm. A high-resolution CCD camera connected to a computer was
also used to monitor the real-time process of micromachining.
Two types of 3-D microstructures were ablated on the cladding of the optical
fiber, namely single-thread and double-thread, as shown in Fig. 20.
The pitch was controlled by special control of the rotating fixture and the feed
speed of the Y axis. The rotary speed was set as 15 rpm, and the pitch is decided
by the following equation:

Figure 18 Schematic of fiber Bragg grating (FBG) magnetic sensing probe.

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 16 Yang, Lee, and Dai: Optical Sensing

Figure 19 Schematic of femtosecond-laser micromachining system.

F
S¼ ;
R
where S represents the pitch, and F is the feed speed, which is decided by the pro-
gram set in the operation stage. As for the double thread, 60 and 80 μm of thread
pitches were made separately. Moreover, all the 3-D microstructures were made
under the energies of 18, 20, and 22 mW. Finally, nine samples were successfully
realized. The single thread is denoted as S-1 to S-3 and the double thread is
SS-1 to SS-6. Meanwhile, the original standard optical fiber grating was also used
for comparison (O-1). All the microstructured fiber gratings are listed in Table 1.
The functional coating of the TbDyFe magnetostrictive materials was depos-
ited in a magnetron sputtering machine. During the process, the rotation fixture
was applied to gain a uniform thin film on the surface of the cladding. The start
power was set as 50 W and the coating power stabilized at a level of 90 W, thus
the average speed of sputtering was almost 0.15 nm∕s. The TbDyFe target and
the microstructured fiber are kept at a distance of 50 mm.

Figure 20 Two types of microstructures for magnetic field sensing. (a) Single thread
(pitch ¼ 60 μm). (b) Double thread (pitch ¼ 60 μm, 80 μm, respectively).

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 Yang, Lee, and Dai: Optical Sensing 17

Table 1 Parameters of microstructured fibers.

Sample O-1 S-1 S-2 S-3 SS-1 SS-2 SS-3 SS-4 SS-5 SS-6
Pitch (μm) ∞ 60 60 60 60 60 60 80 80 80
Energy (mW) 0 18 20 22 18 20 22 18 20 22

Finally, an experimental system for testing the magnetic field was set up as
shown in Fig. 21, and the sensing probe coated with TbDyFe materials is also
shown. The magnetic field was supplied by a permanent magnet instead of an
electric spiral coil in order to eliminate the thermal effect. The value of the mag-
netic field can be measured by a gauss meter. It depends on the distance D from
the magnetic source (the magnetic field range: 0 to 150 mT). The magnet was
fixed on a special nonmagnetic fixture. Additionally, the demodulator (SM130,
Micron Optics) was used to detect the change of the center wavelength by an opti-
cal fiber grating which has a resolution of 1 pm. The magnetic field sensing probe
was protected in a glass tube to avoid breakdown and the N-S orientation of the
permanent magnets was set as parallel to the fiber axis in order to remain at the
uniaxial stress state.
Taking the sample SS-5 as an example, the reflected center wavelength spec-
trum of the FBG (1294.6 nm) by using an OSA was traced as shown in Fig. 22. It
was found that there was no optical reflection peak loss as the peak remained the
same after the ablation; however, the center wavelength permanently shifted about
1 nm due to the broadened grating caused by the thermal effect. When a certain
magnetic field was added, the shift would be traced by OSA, and it would return
to the original spectrum when the magnetic field was moved away.
Using the optical demodulator, the wavelength shifts of the double thread
sample SS-6 when changing the static magnetic strength were recorded and com-
pared with the standard FBG sample O-1. As shown in Fig. 23, the red line
depicts the wavelength changing trend of the most remarkable sensitivity sample
SS-6, while the black line plots the trend of the standard sample.

Figure 21 Schematic of magnetic field sensing device and microstructured sensing probe.

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 18 Yang, Lee, and Dai: Optical Sensing

Figure 22 Spectrum of FBG under different situations.

From Fig. 23, it can be clearly found that the FBG magnetic field sensing
probe with double thread and 80-μm pitch has a much more notable wavelength
shift than the original one. The sensitivity of sample SS-6 can be calculated as
about 1.1 pm∕mT, while the original sample without micromachining is about
0.2 pm∕mT. At the same time, as the magnetic field force is strengthening to a
certain extent about 150 mT, the center wavelength shift of the FBG will increase
slowly due to the limited elongation of the TbDyFe coating. The center wave-
length of FBG magnetic sensing probe can return to the original value when the
magnetic field is removed.
Figure 24 depicts the relationship between the FBG wavelength shifts and
magnetic field strength under different ablation energies. It is obvious that the
value of the energy has a significant influence on the sensitivity according to
the magnetic field. The greater the energy, the deeper the groove it obtains. As
a result, the cross-sectional area of the optical fiber cladding will tend to become

Figure 23 Wavelength shift of sensing probe (sample SS-6 and O-1).

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 Yang, Lee, and Dai: Optical Sensing 19

Figure 24 Wavelength shift of double thread magnetic sensing probe. (a) Thread pitch
80 μm. (b) Fitted line, thread pitch 60 μm.

smaller, thus more magnetostrictive material (TbDyFe) will coat the surface as
well as in the groove. The magnetostrictive effect, therefore, will be more appar-
ent and the strain ε along the axis gets larger under the same magnetic field. So
the microstructures with 22 mW have the highest sensitivity to the magnetic field,
with 1.1 pm∕mT (SS-6) and 0.81 pm∕mT (SS-3, fitted line), respectively.
Additionally, the larger thread pitch can promote the sensitivity to the magnetic
field.
According to Fig. 25(a), an FBG magnetic field sensing probe with a single
thread also responds better to a magnetic field than the standard version. The maxi-
mum wavelength shift can reach approximately 70 pm under the 150-mT magnetic
field, while the standard optical fiber grating only produces a 20-pm wavelength
shift under the same conditions.
In Fig. 25(b), the tested results of three types of microstructures with different
pitches are shown. Apparently, the microstructure with 80 μm is more sensitive to

Figure 25 Center wavelength shift referring to magnetic field. (a) Single thread with pitch
60 μm. (b) Histogram of wavelength shift of different types and pitches.

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 20 Yang, Lee, and Dai: Optical Sensing

the magnetic field compared to that with 60 μm. When the pitch is bigger, the
axial component dominates along the optical fiber, so it will produce a marked
deformation along the axial direction. What is more, the double thread is more
sensitive to the magnetic field in comparison with the single thread as the double
thread has more axial components as well as a smaller cross-sectional area. As a
whole, the double thread is obviously the most effective and suitable microstruc-
ture manufactured on the cladding of optical fiber, which shows great prospects
for magnetic field sensing.
In conclusion, the integration of functional materials with fiber micro-
machining shows promise for advanced sensing technologies. As a demonstrative
example, a new method of magnetic field sensing probe has been proposed and
successfully manufactured in the cladding of an optical fiber. The microstructures
were finally fabricated under the appropriate parameters of femtosecond laser and
a special rotation fixture. The functional magnetostrictive materials of TbDyFe
were coated on the cladding of the fiber grating magnetron sputtering technology.
Experimental results of such an integration of functional materials with fiber
micromachining show that micromachining on fiber can greatly improve the sens-
ing performance in detecting the magnetic field change.

4 Microstructured Fiber with Functional Materials for Optical

Sensing Engineering
PCF, or microstructured fiber, is a new class of optical fiber based on the proper-
ties of photonic crystals. Because of its ability to confine light in hollow cores or
with confinement characteristics not possible in conventional optical fibers, PCF
is now finding applications in fiber-optic communications, fiber lasers, nonlinear
devices, high-power transmission, highly sensitive gas sensors, and other
areas.34–37 More specific categories of PCF include photonic-bandgap fibers
(PCFs that confine light with bandgap effects), holey fibers (PCFs using air holes
in their cross sections), hole-assisted fiber (PCFs guiding light by a conventional
higher-index core modified by the presence of air holes), and Bragg fibers
(photonic-bandgap fibers formed by concentric rings of multilayer film).
Integration of this kind of microstructured fiber with functional materials will
open new fields and directions for high-performance fiber sensing applications.
Microstructured fiber with hydrogen-sensitive materials, i.e., Pt-doped WO3 coat-
ings and Pd-alloy thin film, are proposed and demonstrated as examples of such a
platform for technology.

4.1 Microstructured fiber with functional materials for

hydrogen sensing
Hydrogen has many superior characteristics as an alternative energy resource to
fossil fuels, such as cleanness, sustainability, and high efficiency. However,

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 Yang, Lee, and Dai: Optical Sensing 21

hydrogen easily leaks out and can explode. Therefore, monitoring of hydrogen
concentration is essential for its safe use. Optical fiber sensors have been attrac-
tive for hydrogen measurement because of their intrinsic safety, distributed remote
sensing capability, and stability. Most of these fiber-optic hydrogen sensors are
based on varieties of smart structures combined with sensitive materials, such as
side-polished fibers,38–40 tapered fibers, 41,42 etched fibers, 43,44 and fiber gra-
tings.45,46 Hydrogen sensor based on optical fiber interferometers are of particular
interest due to their high sensitivity. Yang et al.47 reported an extrinsic FPI fiber-
optic hydrogen sensor. Kim et al. 48 reported a Mach-Zehnder interferometric
(MZI) fiber-optic hydrogen sensor. However, both are based on the Pd or
Pd–Ag film, the response and recovery times are relatively long, and the Pd
or Pd–Ag film easily suffer from the risk of delamination, especially when
exposed to a higher hydrogen concentration.49 At present, a fast response fiber-
grating hydrogen sensor was reported,50 where the Pt∕WO3 film was used as a
hydrogen gas sensitive layer. However, the measurement accuracy of the LPG is
limited because of the larger full width at half maximum of the resonance peak
and cross-sensitivity to the change of the environmental temperature and RI.
Microstructured fiber with functional materials for hydrogen sensing is dem-
onstrated as a new platform for optical engineering. A simple but very effective
method to measure hydrogen concentration is proposed by combining a micro-
structured fiber with hydrogen-sensitive functional materials of Pt∕WO3 . A fiber
inline MZI is fabricated by fusion splicing a short section of ethanol-filled PCF
with two single-mode fibers (SMFs). The PCF is coated with sol-gel Pt∕WO3 .
Utilizing the MZI as a temperature-sensing element and with the Pt∕WO3 coat-
ing undergoing an exothermic reaction in a hydrogen atmosphere, a fiber-optic
hydrogen sensor is prepared. Then we can determine the hydrogen concentration
by monitoring the transmission spectrum shift of the interference fringe. The
experimental results demonstrate that the sensor has high sensitivity, fast
response time, and is easily constructed with a low cost.
Figure 26 shows the schematic diagram of the device. Light propagating in
the structure is divided into two parts: in the first collapsed region, the cladding
mode is excited, and then the core mode and the cladding mode propagate along
the ethanol-filled PCF with different effective RIs (denoted by neff eff
core and nclad );
in the second collapsed region, the cladding mode recouples back into the fiber

Figure 26 Schematic diagram of the hydrogen-sensing device proposed.

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 22 Yang, Lee, and Dai: Optical Sensing

core and interferes with the core mode. The interference depends on the optical
path length difference between the core mode and the cladding mode. Therefore,
the MZI output intensity (I) is given by
 
pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi 2πL eff
I ¼ I core þ I clad þ 2 I core I clad cos ðncore − nclad Þ ;
eff
λ

where I core and I clad are the light intensities of the core mode and cladding mode,
respectively, L is the length of the PCF, and λ is the wavelength of the incident
light. According to the previous equation, the interference peak or dip wavelength
(λm ) of the transmission spectrum is denoted as

2πL eff
ðn − neff
clad Þ ¼ mπ m ¼ 1; 2; 3: : : :
λm core

Due to the thermo-optic effect and the thermoexpansion effect, the shift of λm
induced by temperature variation can be derived from Eq. (2) as
  eff 
dλm 1 dL 1 dncore dneff
¼ λm · · þ − clad
¼ λm · ðα þ βÞ;
dT L dT ðneff
core − nclad Þ
eff dT dT

where α is the thermoexpansion coefficient of the ethanol-filled PCF and its value
is taken as about 5.5 × 10−7 ∕°C, and β is the temperature coefficient difference
between the effective RIs of the core mode and the cladding mode, which is deter-
mined by the thermo-optic coefficient (3.9 × 10−4 ∕°C) of ethanol. The parameter
β is calculated to be about −2.6 × 10−4 ∕°C, which is almost three orders larger
than the thermoexpansion coefficient of the ethanol-filled PCF. Therefore, the
dip wavelength shift of the MZI is mainly attributed to the thermo-optic effect.
Assuming the transmission dip wavelength at 1300 nm, the calculated value of
the temperature sensitivity is −0.338 nm∕°C.
In the presence of hydrogen, by utilizing Pt as catalyst, WO3 can react with
hydrogen, and heat will be generated during this chemical reaction. When there
is no hydrogen, the reaction can be recovered in air. Since the Pt∕WO3 layer is
coated on the ethanol-filled PCF, the reaction heat can raise the temperature of
the PCF. Based on Eq. (3), as the temperature increases, the interference fringe
yields a subsequent blueshift of the peak or a dip wavelength. Hence, the hydro-
gen concentration can be obtained by measuring the wavelength shift.
In the device fabrication, a FITEL S177 splicer with a semiautomatic splice
mode was employed to fabricate a fiber MZI. The interferometer had a fraction
of spliced PCF (length of ∼15 mm) between two well cleaved SMFs. The micro-
scope image of the cross-section view of PCF is displayed in Fig. 27(a). Before
fusion splicing, ethanol was filled into the air holes in PCF cladding by capillary

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 Yang, Lee, and Dai: Optical Sensing 23

Figure 27 (a) Microscope image of PCF cross section. (b) Microscope image of ethanol-
filled PCF. (c) The composition of Pt∕WO3 coating. (d) The morphology of Pt∕WO3 coating.

force. The ethanol flow was clearly observed by the digital microscope (VHX-
100). Figure 27(b) shows the microscope image of the ethanol-filled PCF. After
the fabrication of the MZI, the hydrogen-sensitive material (Pt∕WO3 ) was pre-
pared using the sol-gel method. 51 First, an aqueous sol-gel of H2 WO4 was
obtained from Na2 WO4 with a cation-exchange resin. The solution was washed
and centrifuged several times with deionized water. Then appropriate amounts
of H2 PtCl6 · 6H2 O were mixed with the above obtained solution and stirred sev-
eral hours by magnetic stirrer. Finally, the mixture was annealed at 400°C for
1 h, and the Pt-loaded WO3 powder was prepared. To obtain the Pt∕WO3 coating,
the powder was mixed with an appropriate deionized water, and then uniformly
coated on the ethanol-filled PCF of the MZI. The composition and morphology
of the Pt∕WO3 coating were characterized using a field emission scanning elec-
tron microscope (FE-SEM S-4800, Hitachi, Japan), as shown in Figs. 27(c) and
27(d). It can be seen that Pt∕WO3 exists in the coating and there are many porous
structures in the Pt∕WO3 coating.
The experimental setup used for the demonstration of the proposed hydrogen
sensing is illustrated in Fig. 28(a). A superluminescent light-emitting diode

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 24 Yang, Lee, and Dai: Optical Sensing

Figure 28 (a) Scheme of the experimental setup used to test the proposed hydrogen sen-
sor. (b) Transmission spectrum before and after coating treatments.

(SLED) light source was used to illuminate the system, and the transmission spec-
trum was in situ monitored by an OSA (YOKOGAWA, AQ6370B) with a wave-
length resolution of 0.02 nm and a scanning range of 1250 to 1350 nm,
respectively. The hydrogen-sensing performance of the proposed device was
implemented in a gas chamber at room temperature (about 28°C). The gas cham-
ber consists of an inlet and an outlet to allow the dynamic flow of hydrogen and
air. A mass flow controller was used to provide a mixture of hydrogen and air
with the variable hydrogen concentration ranging from 0% to 4%. Figure 28(b)
shows the transmission spectrum variation before and after the Pt∕WO3 coating
treatment. It was observed that after the coating treatment, the fringe visibility
increases, the output intensity decreases, and a number of small peaks almost dis-
appear. This could be explained by the fact that the higher-order cladding modes
are excited into the radiation modes due to the change of the environmental RI.20
In this experiment, the system response to the hydrogen concentration
variation was investigated. A certain volume of hydrogen in air (0%, 1%, 2%,
3%, and 4%) was injected into the gas chamber. The transmission spectrum cor-
responding to each hydrogen concentration was recorded by an OSA, as shown
in Fig. 29(a). The measurements were performed in equilibrium and the response
time was less than 1 min for the spectrum to reach its equilibrium. A clear dip
wavelength shift was observed immediately after hydrogen was introduced.
When the hydrogen concentration increases from 0% to 4%, the location of
the dip wavelength shows a total blueshift of 1.96 nm. According to the discus-
sion in Sec. 2 (the calculated temperature sensitivity of −0.338 nm∕°C), this
means that the temperature of the MZI device increases more than 5°C. The
dip wavelength shift of the interference fringe with the hydrogen volume con-
centration is plotted in Fig. 29(b), in which a good linear fit of the experimental
data is implemented. The obtained hydrogen sensitivity is −0.508 nm∕%
(R2 > 0.99), which is a great improvement in comparison to the previous
report in Ref. 51. In this experiment, the OSA works at a resolution of

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 Yang, Lee, and Dai: Optical Sensing 25

Figure 29 (a) Transmission spectrum response to the hydrogen concentration change rang-
ing from 0% to 4%. (b) Dip wavelength shift versus hydrogen concentration.

0.02 nm; therefore, the hydrogen concentration resolution can be estimated to be

around 0.04%.
After a measurement cycle including each individual hydrogen concentration,
the gas chamber was opened to the ambient environment. Then the hydrogen was
vented and the dip wavelength went back to its original location. The recovery
time was about 2 min after the gas chamber was opened. To investigate the sens-
ing reliability of the proposed hydrogen sensor, the measurement cycle was
repeated three times. It can be concluded from Fig. 30 that there is a measuring
error between each measurement cycle, which mainly resulted from the ambient
temperature fluctuation, the nonuniformity of the Pt∕WO3 coating and hydrogen
concentration error during the experiment. The maximum deviation between the
experimental data and linear fitted data is  0.18 nm, which corresponds to a

Figure 30 Performance measurement of the Mach-Zehnder interferometric device.

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 26 Yang, Lee, and Dai: Optical Sensing

0.35% measurement error of the hydrogen volume concentration. No crack can be

found in the Pt∕WO3 coating after the repeatability test. Further efforts should be
made to enhance the device stability by optimizing the performance of the
Pt∕WO3 coating and stabilizing the ambient temperature.

4.2 Integration of Pt∕WO3 hydrogen-sensitive material with

selectively infiltrated pcf for hydrogen sensing
Another example of such a microstructured fiber with functional materials for
optical sensing engineering is the combination of a Pt∕WO3 hydrogen-sensitive
material with selectively infiltrated PCF for hydrogen sensing.
Most optical fiber hydrogen sensors exploit the optical or elastic property
changes of hydrogen-sensitive materials exposed to hydrogen gas mixtures.
Numerous wavelength-sensitive hydrogen optical fiber sensors have been demon-
strated based on palladium (Pd) films. Sensitivities of the hydrogen sensors men-
tioned above are mainly limited by the intrinsically low strain and/or RI responses
of the fiber-optic devices. To achieve a high sensitivity, hydrogen sensors that
utilize the thermal responses of fiber-optic devices have been proposed, where
exothermic materials, such as WO3 and its compounds, are generally coated on
the fiber surface to change its local temperature through a heat release process
in the hydrogen atmosphere. By coating a Pt-doped WO3 film, FBG exhibits a
sensitivity of up to 1.98 nm/%(v/v) H2 within the range of 0.6 to 4%(v/v) H2
in air.
WO3 can drastically react to hydrogen with a thermal release process, and
then WO3−x can be oxidized to form WO3 again in air. These processes determine
the thermal equilibriums of the hydrogen-sensitive materials under constant
hydrogen concentrations. This Spotlight highlights a highly sensitive fiber device
based on a selectively infiltrated PCF with a Pt-loaded WO3 coating for hydrogen
sensing. The selectively infiltrated PCF device exhibits extremely high sensitivity
to temperature change, and a highly sensitive hydrogen sensor can be achieved
via a Pt-loaded WO3 coating. A 10-mm long sensor exhibits the maximum wave-
length shift of ∼98.5 nm, a response time of ∼78 s for 4%(v/v) H2 , and a sensi-
tivity of up to 32.3 nm/%(v/v) H2 within the range of 1 to 4%(v/v) H2 in air at
room temperature.
In this experiment, one air hole of an endlessly single-mode PCF (LMA-10,
NKT Photonics) was filled with standard RI liquid (RI ¼ 1.508, Cargille
Laboratory Inc.) through the femtosecond-laser-assisted selective infiltration tech-
nique. Figure 31(a) shows the cross-section view of the filled PCF. The liquid-
filled waveguide forms an embedded coupler together with the fiber core based
on the light coupling between the core LP01 and the liquid-waveguide LP11 -like
modes at resonant wavelengths. The resonant wavelength is extremely sensitive
to temperature due to the weak cross-sensitivity effect and the high thermal-optic
coefficient of the RI liquid. A 10-mm long selectively infiltrated PCF was fusion

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 Yang, Lee, and Dai: Optical Sensing 27

Figure 31 (a) Cross-section view of the selectively infiltrated PCF (the white spot near the
fiber core indicates the liquid-filled waveguide); (b) schematic diagram of the proposed
hydrogen sensor, the gray rendering represents the Pt-loaded WO3 coating, the red rod rep-
resents the liquid-filled waveguide, and the rightmost gray rod represents the fiber core of
the single-mode fiber, respectively.

spliced to a standard SMF at both ends and then the PCF section was coated with
Pt-loaded WO3 for the hydrogen sensing test, as depicted in Fig. 31(b). The
hydrogen-sensitive material was prepared using the sol-gel method. First, an aque-
ous sol-gel of H2 WO4 was obtained from Na2 WO4 with a cation-exchange resin.
The solution was washed and centrifuged several times with deionized water.
Then appropriate amounts of H2 PtCl6 · 6H2 O were mixed with the previously
obtained solution and stirred several hours by a magnetic stirrer. Finally, the
PCF device was coated with a Pt-loaded WO3 with the dip-coating technique with
an estimated coating thickness of a few microns.
Before the hydrogen concentration test, the temperature response of the PCF
device was investigated with a high precision column oven (with an accuracy of
 0.1°C). The transmission spectra were recorded by a BBS and an OSA from
room temperature (21.3°C) to 30°C, as shown in Fig. 32(a). The resonant or dip
wavelength change with temperature variation is plotted in Fig. 32(b), where a
linear fitting shows that the temperature sensitivity of the device is ∼7.69 nm∕°C.
For hydrogen sensing, the PCF device was put into a tubular gas cell with a
diameter of 1 cm and a length of 12 cm. The transmission spectrum was moni-
tored in real time by use of a BBS and an OSA. The sample was exposed to
hydrogen concentrations ranging from 0 to 4%(v/v) H2 in air at a temperature of
18.6 °C. Three rounds of hydrogen concentration tests were conducted with a
rising/falling step of 1%(v/v), and the corresponding resonant wavelengths are
plotted in Fig. 33. The resonant wavelength shifts to the shorter wavelength with
the increase in hydrogen concentration and the total wavelength shifts at 4%(v/v)
H2 in air are 52.95, 50.22, and 51.88 nm, respectively. However, the wavelength
shifts at 1%(v/v) H2 in air are only 0.81, 0.91, and 0.83 nm, respectively, for the
rising process of each test. The hydrogen sensitivity can be estimated to be larger

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 28 Yang, Lee, and Dai: Optical Sensing

0
1540
Mearsurement data
Linear fit
o
Temperature sensitivity: 7.69 nm/ C
1520
Transmission (dB)

Dip wavelength (nm)

-10

1500

-20 21.3 C
o

o
1480
25.0 C
o
30.0 C
1460
-30
1440 1470 1500 1530 1560 1590 20 22 24 26 28 30
o
Wavelength (nm) Temperature ( C)
(a) (b)

Figure 32 (a) Transmission spectra at 21.3°C, 25°C, and 30°C and (b) resonant wavelength
shift versus temperature of the selectively infiltrated photonic crystal fiber device.

than 16.7 nm/%(v/v) H2 within the range of 1 to 4%(v/v) H2 in air at room tem-
perature. In the decreasing processes of hydrogen concentration from 4 to 0%(v/v)
H2 in air, the resonant wavelength shifts approximately linearly to longer wave-
lengths and returns to the original values with a fluctuation of less than 100 pm.
Thus, there is hysteresis between the rising and falling processes of hydrogen con-
centrations. The hysteresis in the first test is plotted in Fig. 33 and the contrasts
are 6.09 and 4.62 nm for hydrogen concentrations of 1 and 2%(v/v) H2 in air,
respectively. For the subsequent rounds of tests, the hysteresis can still be
observed; however, the contrasts are found to be slightly reduced.
Temporal response to hydrogen concentrations of the PCF device is also
investigated. Figure 34 displays the resonant wavelength response of the device

st nd rd
1 Test 2 Test 3 Test
1560
0% 0% 0% 0%
1% 1% 1%
1%
1% 1%
Wavelength (nm)

1540
2%
2% 2% 2% 2% 2%

1520 3% 3% 3% 3% 3% 3%

1500 4% 4% 4%
0 20 40 60 80 100
Time (min)

Figure 33 Wavelength shifts of the hydrogen sensor in successive hydrogenation cycles

(between 0% and 4% H2 in air).

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 Yang, Lee, and Dai: Optical Sensing 29

0% 0% 0% 0%
1550

Wavelength (nm) 1525

1500

1475

1450 4% 4% 4%
0 10 20 30 40
Time (min)

Figure 34 Response of the Pt-loaded WO3 coated hydrogen sensor in successive hydrog-
enation cycles (at 0% and 4% H2 in air).

to different hydrogen concentrations. Note that a new sample with more coating
materials (Pt-loaded WO3 ) is used here. However, the amount of the coated
materials used with the dip-coating technique has not been quantified and should
be evaluated in future work. It can be concluded from Fig. 34 that the
device responses are repeatable for the hydrogen concentration ranging from
0 to 4%(v/v) H2 in air. The resonant wavelength can be restored to its initial value
with a fluctuation of less than 100 pm. The average rising (from 0% to 4%) and
falling (from 4% to 0%) response times are measured as 78 and 82 s, respectively.
The total wavelength shifts [from 0 to 4%(v/v) H2 in air] of the device exceed
90 nm in all three cycles of the hydrogen concentration test. The maximum reso-
nant wavelength shift from 1 to 4%(v/v) H2 in air is measured to be 97.0 nm,
which gives an average hydrogen sensitivity of 32.3 nm/%(v/v) H2 in air,
which corresponds to a hydrogen resolution of 3.1 ppm within the range of
1 to 4%(v/v) H2 in air, by assuming a 10-pm optical spectral resolution.
It should be noted that the proposed hydrogen sensor exhibits a large
temperature cross-sensitivity since the selectively infiltrated PCF device is
extremely sensitive to temperature. For example, the temperature cross-sensitivity
can be estimated to be 2378 ppm∕°C for the sensor with a sensitivity of
32.3 nm∕%(v/v) within the range of 1 to 4%(v/v) H2 in air, according to the tem-
perature sensitivity of the PCF device. Thus, temperature calibration should be
included in practical applications to maintain a reasonably high resolution of
hydrogen concentration. One of the possible solutions is to simultaneously mea-
sure H2 concentration and temperature with cascaded fiber-optic temperature
sensors such as FBG, long-period fiber grating, and selectively infiltrated PCF
devices.
In conclusion, a highly sensitive hydrogen sensor based on a selective liquid
infiltrated PCF with Pt-loaded WO3 coating is demonstrated. The hydrogen

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 30 Yang, Lee, and Dai: Optical Sensing

sensitive coating undergoes an exothermic reaction when the sensor is exposed to

gas mixtures of air and hydrogen and thus, induces a local temperature change,
which results in a large resonant wavelength shift of the PCF device. The maxi-
mum wavelength shift of 98.5 nm is observed under 4%(v/v) H2 in air and a
hydrogen sensitivity of 32.3 nm/%(v/v) H2 within the range of 1 to 4%(v/v) H2
in air is obtained. The proposed idea for the integration of a microstructured fiber
with functional materials for hydrogen sensing engineering has high potential in
highly sensitive hydrogen leakage detection.

5 Conclusion
Integration of a novel functional material with fiber-optic components is one of
the new trends for novel sensing technologies. Functional coatings work as sensi-
tive elements and transducers to get response and feedback from the environment.
The integration of functional materials with micromachined or microstructured
fiber means adding a new dimension for optical engineering. Functional materials
can be realized on the side- or end-face of a fiber with many techniques including
sputtering, thermal evaporation, spin-coating, and so on. This Spotlight demon-
strates some examples of such work. Functional coatings on a fiber tip is one such
example. Multilayer coatings of TiO2 ∕SiO2 ∕TiO2 can be deposited on a fiber tip
for an RH sensing application, or one can deposit a multilayer of
ZrO2 ∕Al2 O3 ∕ZrO2 on a sapphire fiber tip for high-temperature sensing up to
1000°C. Using femtosecond-laser micromachining, different microstructures can
be generated on the fiber. When functional materials are deposited on such a
microstructured fiber, an advanced performance can be expected, especially for
fiber-optic sensing engineering. As an example, a microstructured fiber coated
with a TbDyFe magnetostrictive material can greatly improve the effect of magnet
field sensing. PCF is one of the very enabling technologies in terms of the trans-
verse structuring of fibers; when it is integrated with functional coatings, new
directions of sensing applications can be expected including hydrogen sensing
by combining hydrogen-sensitive materials (Pt-doped WO3 coating and Pd-alloy
thin film).

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 Yang, Lee, and Dai: Optical Sensing 33

Minghong Yang is a professor and head of the optical materials and components
division at the National Engineering Laboratory for Fiber Optic Sensing
Technology, Wuhan University of Technology, China. He is a TPC member of
the International Conference of Optical Fiber Sensors. As a conference chair, he
organized the fourth Asia-Pacific Optical Sensors in 2013 (SPIE). His research
interests include thin film materials and optical fiber sensors.

Dongwen Lee received his master’s degree in electronic engineering from

Southeast University, Nanjing, China, in 2006. Currently, he is a doctoral candi-
date with a research interest in optical fiber sensors at the National Engineering
Laboratory for Optical Fiber Sensors, Wuhan University of Technology, China.

Yutang Dai is currently a professor at the National Engineering Laboratory of

Fiber Optical Sensing Technology, Wuhan University of Technology, China. He
received his PhD from the Nippon Institute of Technology, Japan, in 2001.
Afterward, he studied ultra-precision machining techniques for four years at the
Institute of Physical and Chemical Research in Japan. His current interests include
femtosecond-laser micromachining of optoelectronic materials and the develop-
ment of new-type fiber optical sensors.

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