materials

Article
Fiber-Optic Thermal Sensor for TiN Film
Crack Monitoring
Hsiang-Chang Hsu 1 , Tso-Sheng Hsieh 2 , Yi-Chian Chen 1 , Hung-En Chen 3 , Liren Tsai 1 and
Chia-Chin Chiang 1, * ID
1 Department of Mechanical Engineering, National Kaohsiung University of Applied Sciences, Kaohsiung 807,
Taiwan; gn1204774@gmail.com (H.-C.H.); al11062000@gmail.com (Y.-C.C.); liren@kuas.edu.tw (L.T.)
2 Department of Industrial Engineering and Management, Fortune Institute of Technology, Kaohsiung 831,
Taiwan; srcx2s904@gmail.com
3 Department of Mechanical Engineering, Wu Feng University, Chiayi County 62153, Taiwan;
2954883@gmail.com
* Correspondence: ccchiang@kuas.edu.tw; Tel.: +886-07-381-4526 (ext. 5340)

Received: 29 September 2017; Accepted: 7 November 2017; Published: 11 November 2017

Abstract: The study focuses on the thermal and temperature sensitivity behavior of an optical
fiber sensor device. In this article, a titanium nitride (TiN)-coated fiber Bragg grating (FBG) sensor
fabricated using an ion beam sputtering system was investigated. The reflection spectra of the FBG
sensor were tested using R-soft optical software to simulate the refractive index sensitivity. In these
experiments, the temperature sensitivity of the TiN FBG was measured at temperatures ranging from
100 to 500 ◦ C using an optical spectrum analyzer (OSA). The results showed that the temperature
sensitivity of the proposed TiN FBG sensor reached 12.8 pm/◦ C for the temperature range of 100 to
300 ◦ C and 20.8 pm/◦ C for the temperature range of 300 to 500 ◦ C. Additionally, we found that the
produced oxidation at temperatures of 400–500 ◦ C caused a crack, with the crack becoming more and
more obvious at higher and higher temperatures.

Keywords: fiber Bragg grating (FBG); temperature sensitivity; TiN-coated FBG sensor; refractive
index sensitivity

1. Introduction
The safety-related resistance temperature detectors (RTDs) used in nuclear power plants (NPP)
require fast dynamic performance [1]. In order to achieve dynamic performance sensor monitoring
and diagnostics, the associated response times can be estimated in situ by noise analysis techniques [2].
RTDs are sensors that are used to measure temperature by directly registering electrical resistance [3],
the resistive value of which changes simultaneously with temperature changes, and these sensors can
be used to measure wide ranges of temperature, including temperatures from −50 to 500 ◦ C for the
thin film variety and temperatures from −200 to 850 ◦ C for the wire-wound variety [4]. When using
RTDs, the biggest of which are self-heating, the test current could result in measurement inaccuracy.
Optic fibers are typically small in size, passive, immune to electromagnetic interference, resistant to
harsh environments, and are capable of performing distributed sensing [5–7]. In a study conducted
by Rajini-Kumar et al. [8], different types of metal-coated FBGs were tested for their temperature
characteristics, and a CrN-coated FBG sensor exhibited a 14.0 pm/◦ C greater temperature sensitivity
than a bare FBG [9]. Relatedly, in studies by the Zhang group regarding the design and analyses of
periodic dielectric Bragg grating and associated waveguide temperatures [10,11], germanium-oxygen
(Ge-O) bonds were found to play an important role during the index change process of FBG fabrication.
The mathematical modeling of fiber grating is generally accomplished using the coupled mode
theory of wave propagation and the transfer matrix method [12–14]. Chiang et al. conducted a

Materials 2017, 10, 1297; doi:10.3390/ma10111297 www.mdpi.com/journal/materials

Materials 2017, 10, 1297 2 of 10
Materials 2017, 10, 1297 2 of 10
The mathematical modeling of fiber grating is generally accomplished using the coupled mode
theory of wave propagation and the transfer matrix method [12–14]. Chiang et al. conducted a
simulation
simulation study
study ofof coated
coated FBG
FBG used
used as
as aa temperature
temperature sensor
sensor using
using the
the GratingMOD
GratingMOD of of the
the RSoft
RSoft
Photonics computer-aided design (CAD) Suite (version 2016.19, Synopsys,
Photonics computer-aided design (CAD) Suite (version 2016.19, Synopsys, Mountain View, Mountain View, CA, USA),
CA,
according to the literature, where α was the thermal expansion coefficient of silica
USA), according to the literature, where α was the thermal expansion coefficient of silica and was and was equal to
0.55 × 10 −6 , while ξ was the thermo-optic coefficient of the fiber material and was equal to 7.18 × 10−6
equal to 0.55 × 10 , while ξ was the thermo-optic coefficient of the fiber material and was equal to
−6

for
7.18photosensitive (PS) 1250/1500
× 10−6 for photosensitive (Fibercore)(Fibercore)
(PS) 1250/1500 fiber [15]. fiber [15].
The
The present study sought
present study soughttotodevelop
developa simple
a simple method
method forfor making
making a temperature
a temperature modelmodel of
of TiN-
TiN-coated FBG, and to study the role of such metal coating in promoting the temperature
coated FBG, and to study the role of such metal coating in promoting the temperature sensitivity and sensitivity
and the crack
the crack characteristics
characteristics of TiN-coated
of TiN-coated film of filmFBGof in
FBG in high-temperature
high-temperature environments.
environments. In thisIn this
study,
study, the TiN-coated FBG were analyzed applied to monitoring the temperature
the TiN-coated FBG were analyzed applied to monitoring the temperature in the environment sensor. in the environment
sensor. An experimental
An experimental metal coating
metal coating was developed,
was developed, and theand
TiNtheFBGTiN FBG sensor
sensor was investigated
was investigated with
with regard
regard to its temperature
to its temperature sensitivity
sensitivity and crack
and crack characteristics.
characteristics. The measurement
The measurement results,
results, suchsuch as strain
as strain rate
rate
and other information, were detected by the response of the reflected spectrum of the TiN FBG.FBG.
and other information, were detected by the response of the reflected spectrum of the TiN The
The results
results show show
thatthat
thetheTiNTiN
FBGFBG sensor
sensor hasa abetter
has bettersensing
sensingcapability
capability and
and monitoring
monitoring response
response at at
higher temperatures than the bare
higher temperatures than the bare FBG. FBG.

2. Working Principle of TiN-Coated FBG Temperature Sensors

2. Working Principle of TiN-Coated FBG Temperature Sensors
2.1. Fabrication of TiN-Coated FBG Temperature Sensors
2.1. Fabrication of TiN-Coated FBG Temperature Sensors
In this study, the fiber studied was procured from commercial sources, was specially fabricated,
In this study, the fiber studied was procured from commercial sources, was specially fabricated,
and consisted of boron/germanium co-doped fiber (fiber type: photosensitive) 1250/1500, inner core
and consisted of boron/germanium co-doped fiber (fiber type: photosensitive) 1250/1500, inner core
diameter of 9.6 µm, and outer glass (SiO2 ) cladding diameter of 124.9 µm, supplied by Fibercore Ltd.
diameter of 9.6 μm, and outer glass (SiO2) cladding diameter of 124.9 μm, supplied by Fibercore Ltd.
(Southampton, UK). Bragg grating was written into the fiber by using a pulsed KrF-excimer laser at
(Southampton, UK). Bragg grating was written into the fiber by using a pulsed KrF-excimer laser at
248 nm wavelength (Coherent Xantos XS, 248 nm wavelength, 12 mJ/cm2 , Coherent, Palo Alto, CA,
248 nm wavelength (Coherent Xantos XS, 248 nm wavelength, 12 mJ/cm2, Coherent, Palo Alto, CA,
USA). The grating region of the optical fiber was 5 mm in length, and was etched to a diameter of
USA). The grating region of the optical fiber was 5 mm in length, and was etched to a diameter of 60
60 µm in a buffered oxide etchant (BOE) solution, and then placed and fixed on a holder in order to be
μm in a buffered oxide etchant (BOE) solution, and then placed and fixed on a holder in order to be
accurately sputtered.
accurately sputtered.
In this sputtering, a form of physical vapor deposition (PVD), the material was deposited with
In this sputtering, a form of physical vapor deposition (PVD), the material was deposited with
high energy ions from a plasma. Argon (Ar) was used to facilitate the deposition and did not react with
high energy ions from a plasma. Argon (Ar) was used to facilitate the deposition and did not react
the deposited material. The metal thin film was coated onto the FBG, and its reaction with nitrogen gas
with the deposited material. The metal thin film was coated onto the FBG, and its reaction with
caused the formation of TiN. An ion beam sputtering system was used to deposit a uniform TiN film
nitrogen gas caused the formation of TiN. An ion beam sputtering system was used to deposit a
by rotating the substrate and holder in a vacuum chamber, as illustrated in Figure 1. Pre-sputtering
uniform TiN film by rotating the substrate and holder in a vacuum chamber, as illustrated in Figure
was first conducted for 30 min to eliminate any vacuum chamber contamination. The Ar to N2 gas
1. Pre-sputtering was first conducted for 30 min to eliminate any vacuum chamber contamination.
ratio was 80:20. The sputtering process pressure of the system was 6 × 10−3 Torr, and the power of
The Ar to N2 gas ratio was 80:20. The sputtering process pressure of the system was 6 × 10−3 Torr, and
the Ti target material was 70 W. The film was deposited for 15 min to approximate a film thickness of
the power of the Ti target material was 70 W. The film was deposited for 15 min to approximate a
0.82 µm.
film thickness of 0.82 μm.

Figure 1.
Figure 1. Rotating
Rotating the
the FBG
FBG sensor
sensor holder
holder in
in the
the vacuum
vacuum chamber.
chamber.
2
Materials 2017, 10, 1297 3 of 10

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Materials 2017,10,
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1297 33of
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The composition of the TiN film was characterized by a scanning electron microscope equipped
Thecomposition
The compositionofofthe
theTiN
TiNfilm
filmwaswas characterizedby by a scanningelectron
electronmicroscope
microscopeequipped
equipped
with energy dispersive spectroscopy (EDS).characterized
Figure 2 showsaascanning
spectrogram of the EDS analysis results
withenergy
with energydispersive
dispersivespectroscopy
spectroscopy(EDS).
(EDS).Figure
Figure22shows
showsaaspectrogram
spectrogramofofthe
theEDS
EDSanalysis
analysisresults
results
of the
of TiN-coated
the TiN-coatedFBG
FBGsensor,
sensor,which
which indicate
indicatethat
that titanium
titanium and nitrogen
and nitrogenwere
weredetected
detected
onon the
the FBG.
FBG.
of the TiN-coated FBG sensor, which indicate that titanium and nitrogen were detected on the FBG.
TheTheTi content
Ticontentwas
contentwas about
wasabout 72.38
about72.38 wt
72.38wt %,
wt%, and
%,and the
andthe N
theN content
Ncontent was
contentwas about
wasabout 27.62
about27.62 wt
27.62wt
wt%.%. The
%.The
TheFBGFBG
FBGand and
andthe the
theTiNTiN
TiN
The Ti
filmfilm
coating are
coatingareshown
areshown in
shownin Figure
inFigure 3.
Figure3.
3.
film coating

Figure2.2.2.EDS
Figure
Figure EDSanalysis
EDS analysisresults
analysis
of
resultsof
results
the
ofthe TiN-coated
theTiN-coated FBGsensor.
TiN-coatedFBG
FBG sensor.
sensor.

Figure3.3.Photographic
Figure Photographicview
viewof
ofTiN-coated
TiN-coatedFBG.
FBG.
Figure 3. Photographic view of TiN-coated FBG.
2.2.Principle
2.2. PrincipleofofTiN-Coated
TiN-CoatedFBG FBGTemperature
TemperatureSensors
Sensors
2.2. Principle of TiN-Coated FBG Temperature Sensors
TheFBG
The FBGcan canbebecharacterized
characterizedby byits
itsBragg
Braggwavelength,
wavelength,which whichisisthethereflected
reflectedwavelength
wavelengthof oflight
light
from
Thethe
from the
FBGgrating.
can beThe
grating. The Bragg wavelength
characterized
Bragg wavelength isis wavelength,
by its Bragg ,, where
where
which is is is the
the the effective
reflected
effective refractive index
wavelength
refractive index
of light
fromof the fiber core
grating. and
The Λ
Braggis the grating
wavelength
of the fiber core and Λ is the grating period.B period.
is λ = 2n eff , where n eff is the effective refractive index of the
fiber core If the
and
If the Λ is the grating
temperature
temperature is equal
is equal to
period.zero, the Bragg wavelength of bare FBG
to zero, the Bragg wavelength of bare FBG sensor is given by sensor is given by

∆∆
If the temperature is equal to zero, the Bragg wavelength of bare FBG sensor is given by
(1)
(1)
∆λB
= [αs + ξ ]∆T (1)
where ΔT=T−T00 isis the
where ΔT=T−T the change
change in in temperature,
temperature,
λB isis the
the thermal
thermal expansion
expansion coefficient
coefficient ofof silica
silica equal
equal
to 0.55
0.55 ×× 10
10−6−6, and
and / ⁄ is is the
the thermo-optic
thermo-optic coefficient
coefficient of of the
the fiber
fiber equal
equal to to 7.18
7.18 ××
to
where ∆T = T ,− T 0 is the/change in ⁄temperature, αs is the thermal expansion coefficient of silica
10−6 [15].
10
−6 [15].
equal to 0.55 × 10−6 , and ξ = (1/neff )(∂neff /∂T) is the thermo-optic coefficient of the fiber equal to
According
According to the literature [9,16], for a temperature change ΔT, the thermal expansion
−6 [15]. to the literature [9,16], for a temperature change ΔT, the thermal expansion
× 10
7.18coefficients and the refractiveindex
indexcancanbebedefined
definedas as
coefficients and the refractive
According to the literature [9,16], for a temperature change ∆T, the thermal expansion coefficients
and the refractive index can∆∆be defined as
(2)
(2)
∆λB
= [αs + (1 − Pe )(αTiN − αS )η + ξ ]∆T (2)
λB
   //   (3)
(3)
ATiN ATiN
η= (ETiN ) / (ETiN ) + ES (3)
AS AS
33
Materials 2017, 10, 1297 4 of 10

where PMaterials 2017, 10, 1297

e is the photoelastic constant of the fiber and αTiN is the thermal expansion coefficient of TiN
4 of 10

material, ETiN and

where ES are
is the the Young’s
photoelastic moduli
constant of theoffiber
the and
TiN material
is theand the expansion
thermal silica glass, respectively,
coefficient of
and ATiN
TiN and AS are the cross-sectional
material, and are theareas of themoduli
Young’s TiN material
of the and
TiN the silica and
material glass,
therespectively.
silica glass,
Forrespectively,
FBG coated and with TiN,
and a change
are thein the temperature
cross-sectional areas causes a change
of the TiN materialin thethe
and grating period
silica glass,
due to respectively.
the thermal expansion of the fiber and the strain induced by thermal expansion of the TiN
For FBG
coating material. Incoated with the
addition, TiN,refractive
a change inindex
the temperature
of the corecauses
changesa change
due toin the
the grating period due
thermo-optic effect.
to the thermal
The temperature expansion
sensitivity ofof the fiber and
TiN-coated theis
FBG strain
given induced
by by thermal expansion of the TiN coating
material. In addition, the refractive index of the core changes due to the thermo-optic effect. The
∆λB FBG is given by
temperature sensitivity of TiN-coated
= [(1 − Pe )αTiN + ξ ]∆T (4)
λ∆B
(4)
where Pe is the photoelastic constant of the fiber and αTiN is the thermal expansion coefficient of the
TiN material.
where Theistheoretical temperature
the photoelastic constantsensitivity
of the fibercan
andthus beisdetermined by calculating
the thermal expansion that ofofthe
coefficient
metal film combined
the TiN with
material. Thethe FBG. The
theoretical metal film
temperature deposition
sensitivity cantechnique can be effectively
thus be determined utilized
by calculating that to
of the metal film combined with the FBG. The metal film deposition technique can be effectively
deposit TiN coating, and by adding this coating, the temperature sensitivity of the FBG sensor in high
utilized
temperature to deposit TiNwas
environments coating, and by adding this coating, the temperature sensitivity of the FBG
increased.
sensor in high temperature environments was increased.
3. Experiment
3. Experiment
3.1. Measurement of TiN-Coated FBG Sensor
3.1. Measurement of TiN-Coated FBG Sensor
The high temperature sensor was fabricated by using a DC magnetron to sputter physical
The high temperature sensor was fabricated by using a DC magnetron to sputter physical vapor
vapor deposition (PVD) TiN onto the surface cladding of the FBG sensor. The resulting novel
deposition (PVD) TiN onto the surface cladding of the FBG sensor. The resulting novel metal-coated
metal-coated nitrogen-doped
nitrogen-doped high temperature
high temperature sensor wassensor was then
then studied studied
using using the experimental
the experimental framework
framework illustrated
illustrated in Figure
in Figure 4. A broadband
4. A broadband light
light ray was ray was
injected injected
using a superusing a superdiode
luminescent luminescent
(SLD,
diode (SLD, DL-BP1-1501A,
DL-BP1-1501A, POET Technologies
POET Technologies Inc, Singapore,
Inc, Singapore, Singapore)Singapore) broadband
broadband light source. light source.
A jumper
A jumperwire wire
waswas connected
connected to one
to one of aof1 a× 12×
endend 2 optical
optical coupler,
coupler, and and the other
the other end end
was was connected
connected to a to
superfluorescent fiber source with a spectrum analysis instrument. The reflected spectra
a superfluorescent fiber source with a spectrum analysis instrument. The reflected spectra of the FBG of the FBG
sensor sensor
were thenwerescanned
then scanned and stored
and stored via via an optical
an optical spectrumanalyzer
spectrum analyzer (OSA,
(OSA, MS9740A,
MS9740A,ANRITSU
ANRITSU
EMEA Ltd, Luton, UK).
EMEA Ltd, Luton, UK).
The TiN-coated FBG sensor (1551.00 nm 23 °C) was placed in the heating oven, which was
The TiN-coated FBG sensor (1551.00 nm 23 ◦ C) was placed in the heating oven, which was
certainly capable of influencing the data quality of the test experiments in terms of the signals
certainly capable of influencing the data quality of the test experiments in terms of the signals emitted.
emitted. The temperature of the oven was raised from 100 to 500 °C. Data were recorded once every
The temperature
50 °C increaseof the oven was raised
in temperature. Every from
individual 500 ◦ C. Data
100 totemperature were
point wasrecorded
maintained once
for every
10 min50
◦
in C
increaseorder
in temperature.
to record theEvery individual
reflective spectrum temperature point wasbetween
of the relationship maintained for 10 min in
the wavelength order
and the to
record the reflective
temperature. spectrum of the relationship between the wavelength and the temperature.

4
Figure 4. The experimental setup of the temperature sensing test.
Materials 2017, 10, 1297 5 of 10

Materials 2017, 10, 1297 5 of 10

Figure 4. The experimental setup of the temperature sensing test.

3.2. Simulation
3.2. Simulation of
of TiN-Coated
TiN-Coated FBG
FBG Sensor
Sensor

3.2.1. Thermal-Structure
3.2.1. Thermal-Structure Interaction
Interaction of
of TiN-Coated
TiN-CoatedFBG
FBG
Thedesign
The designof ofthethe optical
optical fiber fiber temperature
temperature sensor wassensor wastoproven
proven to be by
be reasonable reasonable by the
the experimental
experimental
results. results. The
The schematic schematic
of the of the design
experimental experimental
is showndesign is shown
in Figure in COMSOL
5. The Figure 5. The COMSOL
Multiphysics
Multiphysics
5.1 (v5.1.0.180,5.1 (v5.1.0.180,
Pitotech Co. Ltd, Pitotech
Changhua,Co. Taiwan)
Ltd, Changhua,
and opticalTaiwan)
software and
Rsoftoptical software
(v2015.09, Rsoft
Cybernet
(v2015.09,
Systems Cybernet
Taiwan Systems
Co. Ltd, Taiwan
Hsinchu, Co. Ltd, Hsinchu,
Taiwan)were then usedTaiwan)were then used
for a temperature testfor a temperature
simulation, with test
the
simulation, with
temperature the temperature
variation ranging from variation 500 ◦ C with
100 toranging from steps
100 toof
500 ◦ C.
50°C with steps of 50
A complete °C. Aconsisting
mesh complete
mesh
of consisting
50,742 domainofelements,
50,742 domain
14,798elements,
boundary14,798 boundary
elements, andelements,
1372 edge and 1372 edge
elements elements
was computed,was
computed,
and exhibited andcomplete
exhibited complete convergence.
convergence. The TiN films TheandTiNoptical
films and
fiberoptical
materialfiber materialare
properties properties
shown
areTable
in shown in TableThe
1 [17,18]. 1 [17,18]. The heatinterface
heat transfer transfer interface of the TiN-coated
of the TiN-coated FBG at temperatures
FBG at temperatures from 100 from
to
500 ◦
100 to C500
was°C was calculated
calculated with
with the the COMSOL
COMSOL software.
software. A linear
A linear relationship
relationship was was obtained
obtained between
between the
the temperature
temperature loading
loading and and
strainstrain
of theofTiN-coated
the TiN-coated
FBG,FBG,
withwith a thermal
a thermal sensitivity
sensitivity of ×
of 2.31 10×−610
2.31 . −6.

Figure 5. The
Figure 5. The schematic
schematic of
of the
the experimental
experimental design
design of
of the
the simulation
simulation study.
study.

Table 1. TiN
Table 1. TiN films
films and
and optical
opticalfiber
fibermaterial
materialproperties
propertiestable
table[17,18].
[17,18].

Material Elastic Coefficient of Thermal

Material Elastic Poisson’s Coefficient of Thermal
Poisson’s Expansion
−6 Expansion
TiN films 390 GPa 0.25 5.85 × 10
FBG
TiN films 73 GPa
390 GPa 0.165 0.25 0.55 × 10−6 5.85 × 10−6

FBG 73 GPa 0.165 0.55 × 10−6

3.2.2. Numerical Modeling of Spectral Amplitude Response in FBG
3.2.2.The
Numerical Modeling
Rsoft software was of Spectral
then Amplitude
employed to analyze Response in FBG sensitivity of the FBG at various
the temperature
surrounding temperatures.
The Rsoft software was Forthen
experimentation,
employed tothe Rsoft software
analyze was initially
the temperature employed
sensitivity to confirm
of the FBG at
the temperature sensitivity values measured by the FBG for the various surrounding
various surrounding temperatures. For experimentation, the Rsoft software was initially employed temperatures
by
to comparing
confirm thethe FBG changesensitivity
temperature results with the Bragg
values measuredwavelength
by the shifts at the
FBG for thevarious
varioustemperatures.
surrounding
The results were then used to analyze the thermal expansion coefficient and the
temperatures by comparing the FBG change results with the Bragg wavelength shifts at the thermo-optic coefficient
various
of the FBG temperature sensor.
temperatures. The results were then used to analyze the thermal expansion coefficient and the
Default waveguide
thermo-optic settings
coefficient of the FBGwere set in order
temperature to produce a standard single mode fiber with a
sensor.
diameter of 9.6 µm, a cladding index of 1.466,
Default waveguide settings were set in order to and a core indexa of
produce 1.474. This
standard corresponded
single to thea
mode fiber with
following
diameter of CAD9.6 parameters (as shown
μm, a cladding indexinofTable
1.466,2):and
index difference
a core = 0.008,
index of 1.474.background index = to
This corresponded 1.466,
the
and component width = component height = 9.6 µm. A typical free-space wavelength of 1551.78 nm
5
Materials 2017, 10, 1297 6 of 10

Materials 2017, 10, 1297 6 of 10

following CAD parameters (as shown in Table 2): index difference = 0.008, background index = 1.466,
and component width = component height = 9.6 μm. A typical free-space wavelength of 1551.78 nm
was used at
was used at 100
100 ◦°C, while the
C, while the simulation
simulation test
test temperature
temperature ranged
ranged from
from 100
100 to 500 ◦°C.
to 500 C. The
The grating
grating
perturbation,
perturbation, defined
defined asas the
the way
way the
the waveguide
waveguide parameters
parameters vary
vary along
along the
the propagation
propagation direction,
direction,
was 0.0003. The
was 0.0003. The thermo-optic
thermo-optic coefficient
coefficient ξξ and
and thermal
thermal expansion
expansion coefficient
coefficient αα of
of the
the fiber
fiber were
were
defined as Dn/dt
defined as Dn/dt andand DΛ/dt
DΛ/dtininthe
theRSoft
RSoftCAD
CADlayout
layoutparameters,
parameters,and
andthe
thesimulation
simulation was
was performed
performed
as
as GratingMOD.
GratingMOD.

Table
Table 2.
2. The
The simulation
simulation parameters
parameters of
of TiN-coated FBG.
TiN-coated FBG.

Simulation Tool GratingMOD Simulation Tool GratingMOD

Simulation Tool GratingMOD Simulation Tool GratingMOD
Grating type Volume index Width 9.6 μm
StructureGrating
type type Volume index
Fiber Width
ModDelta 9.6 µm
0.0003
Structure type Fiber ModDelta 0.0003
Index profile
Index profile Step index
Step index Delta
Delta 0.008 0.008
Length Length 5000 μmµm
5000 Dn/dt
Dn/dt (ξ)( ) 7.18 × 107.18
−6 × 10−6
−6
2.31 × 102.31
Height Height 9.6 9.6
μmµm DΛ/dt
DΛ/dt (α)(α) × 10−6

4.
4. Results
Results and
and Discussion
Discussion

Temperature Test
4.1. Temperature Test of
of the
the TiN-Coated
TiN-CoatedFBG
FBGSensor
Sensor
temperature sensitivity
The temperature sensitivity and
and responsivity
responsivity of of the
the TiN-coated
TiN-coated FBG
FBG sensor
sensor in the oven was
measured as
measured as light
lightwas
wasinjected
injectedinto
intoitsitsfiber
fibercore
corebyby
thethe broadband
broadband laser.
laser. As the
As the test test proceeded,
proceeded, the
the thermal
thermal expansion
expansion coefficient
coefficient andand refractive
refractive index
index in in
thethegrating
gratingofofthe
theTiN-coated
TiN-coated FBG FBG sensor
changed. TheThechanges
changesininthethe
temperature
temperature itself, meanwhile,
itself, meanwhile,couldcould
be observed via thevia
be observed reflection spectra
the reflection
of the FBG,
spectra of thewhich
FBG,were
which themselves the result
were themselves theof perturbations
result in the grating
of perturbations resulting
in the grating in shifts
resulting in in the
shifts
Bragg
in the wavelength. Figure 6Figure
Bragg wavelength. shows 6the intensity
shows the spectra
intensityresults of TiN-coated
spectra FBG as the temperature
results of TiN-coated FBG as the
was increased.
temperature was increased.

Figure
Figure 6.
6. The
The online
online monitoring
monitoring diagram
diagram of
of the
the highly
highly reflective
reflective TiN-coated FBG.
TiN-coated FBG.

The temperature characteristics of the TiN-coated FBG sensor showed that, under increasing
The temperature characteristics of the TiN-coated FBG sensor showed that, under increasing
temperature, the intensity spectrum of the TiN-coated FBG at 100 °C was measured to be 1551.78 nm,
temperature, the intensity spectrum of the TiN-coated FBG at 100 ◦ C was measured to be 1551.78 nm,
as shown in Figure 7. The results also showed that the shift in the Bragg wavelength for the TiN-
as shown in Figure 7. The results also showed that the shift in the Bragg wavelength for the TiN-coated
coated FBG was 2.57 nm over the temperature range from 100◦to 300 °C, while it was 4.18 nm for the
FBG was 2.57 nm over the temperature range from 100 to 300 C, while it was 4.18 nm for the higher
higher temperature range from 300◦to 500 °C.
temperature range from 300 to 500 C.
6
Materials 2017, 10, 1297 7 of 10
Materials 2017, 10, 1297 7 of 10

Specifically,
Materials 2017, 10, the
Specifically, 1297
theresponses
responses ofofthethe
TiN-coated
TiN-coated FBGFBG ininterms
termsofofthe
theshift
shiftininthe
theBragg
Braggwavelength7 of 10for
wavelength
each degree of change in the temperature were calculated. The responsivity
for each degree of change in the temperature were calculated. The responsivity of the TiN-coated of the TiN-coated FBG
was Specifically,
about the
◦ responses of the TiN-coated FBG in terms
◦ of the shift in the Bragg wavelength
◦
FBG was12.8
aboutpm/ 12.8Cpm/°C
for the
fortemperatures
the temperaturesfromfrom
100 to100300 C, °C,
to 300 while it was
while about
it was about20.8 pm/
20.8 pm/°CC for
for
thefor eachrange
higher degreeofof change in the
temperatures temperature
from 300 to were calculated.
◦ C. Below ◦The responsivity of the TiN-coated
the higher range of temperatures from 300500
to 500 °C. Below 300300C,°C,
the temperature
the temperature coefficient
coefficientofofthe
FBG was about 12.8 pm/°C for the temperatures from 100 to 300 °C, while it was about 20.8 pm/°C
TiN-coated FBG exhibited
the TiN-coated a 7.6%
FBG exhibited improvement
a 7.6% improvementoverover
thatthat
of the barebare
of the FBG FBG(|11.9–12.8|/11.9)
(|11.9–12.8|/11.9)[9].
[9].
for the higher range of temperatures from 300 to 500 °C. Below 300 °C, the temperature coefficient of
the TiN-coated FBG exhibited a 7.6% improvement over that of the bare FBG (|11.9–12.8|/11.9) [9].

Figure 7. Temperature characteristics of the TiN-coated FBG sensor and bare FBG sensor.
Figure 7. Temperature characteristics of the TiN-coated FBG sensor and bare FBG sensor.

The onsetFigureof 7. Temperature

oxidation characteristics
occurred at 400 toof the°C,
500 TiN-coated FBG sensor
and a change in the and bare FBGof
mechanism sensor.
TiN oxidation
The onset ofwith oxidation occurred at 400 toRapid
500 C,◦ and a change in the mechanism of TiN oxidation
was observed increasing temperature. oxidation occurred at 500 °C, and with increasing
was The onset
observed withof increasing
oxidation occurred
temperature.at 400 to 500 °C,
Rapid and a change
oxidation in the mechanism
occurred ◦ C, andof with
TiN oxidation
oxidation time, the growth and strain of the small crystallites arising at 500 the
from volume increasing
expansion
was observed with increasing temperature. Rapid oxidation occurred at 500 °C, and with increasing
oxidation time, the growth
caused intergranular andThe
fracture. strain of thecrack
oxidation small crystallitescharacteristics
propagation arising fromofthe thevolume
TiN-coated expansion
FBG
oxidation time, the growth and strain of the small crystallites arising from the volume expansion
at 500intergranular
caused °C, with t0 ~ fracture.
t3 ≈ 90 sec,Theare schematically
oxidation crack illustrated
propagation in characteristics
Figure 8, whereoft1the indicates
TiN-coatedthe crack
FBG at
caused
◦ C, withintergranular fracture. The oxidation crack propagation characteristics of the TiN-coated FBG
500initiation phase,
t0~t3 ≈ t290
indicates the crack propagation
s, are schematically illustratedphase, and8,t3where
in Figure indicates the ultimate
t1 indicates catastrophic
the crack initiation
at 500 °C, with t0 ~ t3 ≈ 90 sec, are schematically illustrated in Figure 8, where t1 indicates the crack
failure
phase, phase. Optical
t2 indicates spectra
the crack and SEM phase,
propagation imagesand of the experimental
t3 indicates results for
the ultimate these different
catastrophic phases
failure phase.
initiation phase, t2 indicates the crack propagation phase, and t3 indicates the ultimate catastrophic
of
Opticaloxidation
spectra time
and in
SEMthe oven
images areof shown
the in Figure
experimental 9. The crystallographic
results for these characteristics
different phases ofand intensity
oxidation time
failure phase. Optical spectra and SEM images of the experimental results for these different phases
in spectrum
the oven of the
are shownTiN-coated
in Figure FBG9. filmcrystallographic
The showed that oxidation crack propagation
characteristics and intensity
of oxidation time in the oven are shown in Figure 9. The crystallographic characteristics and intensity
occurred
spectrum at of
thethe
maximumFBG
TiN-coated temperature of 500
filmTiN-coated
showed °C.oxidation
that The spectra of the
crack TiN-coatedoccurred
propagation FBG exhibited two peaks (at
at the maximum 1557.86
temperature
spectrum of the FBG film showed that oxidation crack propagation occurred at the
nm
of 500 and
◦ 1559.12
C. The nm) for
spectra of of two different
the500
TiN-coated periods
FBG ofof crack
exhibited initiation,
two peaksthree peaks (at 1557.80 nm, 1558.06
maximum temperature °C. The spectra the TiN-coated FBG (at 1557.86two
exhibited nmpeaks
and 1559.12
(at 1557.86 nm)
nm, and 1558.34 nm) for three different periods of crack propagation, and then one peak (at 1557.32
for nm
twoanddifferent periods of crack initiation, three peaks (at 1557.80 nm, 1558.06
1559.12 nm) for two different periods of crack initiation, three peaks (at 1557.80 nm, 1558.06 nm, and 1558.34 nm)
nm) for one period of ultimate catastrophic failure.
for nm,
three different
and 1558.34periods
nm) for of crack
three propagation,
different periods and thenpropagation,
of crack one peak (atand 1557.32
then nm) for one
one peak (at period
1557.32of
ultimate
nm) for catastrophic
one period of failure.
ultimate catastrophic failure.

Figure 8. Schematic of crack characteristics of the TiN-coated FBG. (t0~t3 ≈ 90 s at 500 °C).

Figure
Figure 8. Schematic
8. Schematic of of crack
crack characteristicsofofthe
characteristics theTiN-coated
TiN-coatedFBG. ~t33≈≈9090
FBG. (t(t00~t s at 500
s at ◦ C).
°C).
500

7
Materials 2017, 10, 1297 8 of 10
Materials 2017, 10, 1297 8 of 10

Materials 2017, 10, 1297 8 of 10

Figure 9. The optical spectra and SEM images of TiN-coated FBG at 500 °C: (a) crack initiation; (b)
Figure 9. The optical spectra and SEM images of TiN-coated FBG at 500 ◦ C: (a) crack initiation; (b) crack
crack propagation, and (c) ultimate catastrophic failure.
propagation, andoptical
Figure 9. The (c) ultimate
spectracatastrophic failure.
and SEM images of TiN-coated FBG at 500 °C: (a) crack initiation; (b)
crack propagation, and (c) ultimate catastrophic failure.
4.2. Analysis Using the FEM
4.2. Analysis Using the FEM
The temperature
4.2. Analysis Using the characteristics
FEM of the TiN-coated FBG sensor indicated by the Rsoft simulation
andThe temperature
experiment characteristics
are shown in Figureof10. theThe
TiN-coated FBG sensor
values measured by the indicated
TiN-coated by the Rsoft
FBG simulation
temperature
and The temperature
experiment are characteristics
shown in Figure of
10. the
TheTiN-coated
values FBG sensor
measured by indicated
the by the Rsoft
TiN-coated FBG simulation
temperature
sensor were for loadings of 0 to 500 °C, and were verified by experimental measurement. As can be
and experiment
sensor are shown in Figure
500 ◦ C,10.and Thewere
values measuredexperimental
by the TiN-coated FBG temperature
seen were
from for loadings
Figure 10a,b, of
the0 to
wavelength strength verified
variationby was 4.30 nm, and measurement.
the sensitivityAs of can
this be
sensor
seen were
from Figure for loadings
10a,b, of 0 to 500 °C, and were verified by experimental measurement. As canofbe
temperature sensor wasthe14.2wavelength
pm/°C for the strength variation
experimental was 4.30 nm,
measurements, theand the sensitivity
wavelength variation this
of
seen from Figure 10a,b, the wavelength ◦ C for thestrength variation was 4.30 nm, and the sensitivity of this
temperature
3.71 nm and sensor was 14.2 pm/
the sensitivity of 12.8 pm/°C, as experimental
indicated bymeasurements,
the Rsoft software the wavelength variation
simulation analysis,
temperature sensor was 14.2 pm/°C for the◦ experimental measurements, the wavelength variation of
of were
3.71 nm and the sensitivity
proportional of 12.8 pm/
to the temperature changes C, as fromindicated by°C.
100 to 400 theThese
Rsoftexperimental
software simulation analysis,
results indicate
3.71 nm and the sensitivity of 12.8 pm/°C, as indicated by the ◦ Rsoft software simulation analysis,
thatproportional
were the Bragg wavelength shift of the
to the temperature TiN-coated
changes from FBG100 toas 400
the temperature changed was
C. These experimental a parabolic
results indicate
were proportional to the temperature changes from 100 to 400 °C. These experimental results indicate
relation,
that the Bragg caused by the oxygen
wavelength shift of in the
the TiN-coated
natural environmentFBG as the diffusing into the
temperature TiN-coated
changed was films and
a parabolic
that the Bragg wavelength shift of the TiN-coated FBG as the temperature changed was a parabolic
then
relation, diffusing
caused through
bybythethe the
oxygengrainin inboundary
thethe
natural of the TiN-coated
environment films
diffusing into the
into SiO
thethe , at
TiN-coated
2 temperatures
films from
and then
relation, caused oxygen natural environment diffusing into TiN-coated films and
150 to 400
diffusing °C. Additionally, a large part of the wavelength variation was observed at temperatures
then diffusing through the grain boundary of the TiN-coated films into the SiO2, at temperatures from150
through the grain boundary of the TiN-coated films into the SiO 2 , at temperatures from
to from
400 to
150
400Additionally,
◦ C. to 500 °C, where
400 °C. Additionally,
the temperature
a large a part
largeof
sensitivity (24.5
theofwavelength
part the wavelength
pm/°C)
variation was
variation
forobserved
the experiment
was observed
measurement
at temperatures
at temperatures from
was
400from higher
to 500 ◦ than
C, 500
wherethe simulation result, as oxidation occurred ◦at that temperature range with formation
400 to °C, the
wheretemperature
the temperature sensitivity (24.5 (24.5
sensitivity pm/ pm/°C)
C) for the experiment
for the experiment measurement
measurement was
of oxide
higher thanlayer
the of rutile-TiOresult,
simulation 2[19].
as oxidation occurred at that temperature
was higher than the simulation result, as oxidation occurred at that temperaturerange rangewith
withformation
formation of
oxide layerlayer
of oxide of rutile-TiO 2 [19].
of rutile-TiO 2[19].

Figure 10. Temperature characteristics of the TiN-coated FBG sensor according to the Rsoft simulation
and experiment. (a) Intensity-Wavelength graph for Rsoft simulation; (b) Wavelength-Temperature
Figure 10. Temperature characteristics of the TiN-coated FBG sensor according to the Rsoft simulation
graph.
Figure 10. Temperature characteristics of the TiN-coated FBG sensor according to the Rsoft simulation
and experiment. (a) Intensity-Wavelength graph for Rsoft simulation; (b) Wavelength-Temperature
and experiment. (a) Intensity-Wavelength graph for Rsoft simulation; (b) Wavelength-Temperature graph.
graph.
5. Conclusions
5. Conclusions
This study proposed and investigated TiN-coated FBG applied as a sensor to monitor
5. Conclusions
environmental
This temperatures. The sensor was fabricated by depositing a TiN as
film on FBG using PVD
Thisstudy
studyproposed
proposed and and investigated
investigated TiN-coated
TiN-coated FBGFBG applied
applied as a asensor
sensor totomonitor
monitor
method. Simulations of this TiN-coated FBG were then conducted using the COMSOL and optical
environmental
environmental temperatures.
temperatures.TheThesensor
sensor was
was fabricated bydepositing
fabricated by depositingaaTiN
TiNfilm
filmononFBG
FBG using
using PVDPVD
method.
method.Simulations of of
Simulations this TiN-coated
this TiN-coatedFBG were
FBG were8 then
then conducted using
conducted thethe
using COMSOL
COMSOL andand
optical Rsoft
optical
8
Materials 2017, 10, 1297 9 of 10

software in order to obtain the temperature sensitivity, responsivity of the reflected spectrum, thermal
expansion coefficient, and thermo-optic coefficient of the FBG temperature sensor. The experimental
results indicated that the metal film of the TiN-coated FBG sensor had suitable temperature sensitivity
and behavioral processes for the monitoring of crack growth, but it was found that the nonlinear
part generated by the oxidation phenomenon could not be analyzed using the simulation software.
This aspect is worthy of further investigation in an in-depth study. Moreover, the results indicated
that the TiN-coated FBG sensor effectively achieved temperature sensitivity and responsivity for
higher-temperature sensing at temperature ranges from 100 to 400 ◦ C, with the sensitivity of the
temperature sensor being 14.2 pm/◦ C for the experimental measurements; at temperatures from 400
to 500 ◦ C, the temperature sensitivity 24.5 pm/◦ C for the experiment measurement.

Acknowledgments: This work was supported by the Ministry of Science and Technology, Taiwan (grant number
MOST 106-2221-E-51-023).
Author Contributions: Chia-Chin Chiang designed the study methods and experiments, analyzed the data,
and wrote the paper. Hsiang-Chang Hsu, Tso-Sheng Hsieh, Yi-Chian Chen, Hung-En Chen, and Liren Tsai
conducted the experiments and analyzed the experimental data.
Conflicts of Interest: The authors declare no conflicts of interest.

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