Sensors and Actuators B 134 (2008) 687693

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Sensors and Actuators B: Chemical

journal homepage: www.elsevier.com/locate/snb

Nano-structured Pd-long period ber gratings integrated optical sensor

for hydrogen detection
Xiaotong Wei a , Tao Wei b , Hai Xiao b , Y.S. Lin a,
a
b

Department of Chemical Engineering, Arizona State University, Tempe, AZ 85287, United States
Department of Electrical and Computer Engineering, Missouri University of Science and Technology, MO 65409, United States

a r t i c l e

i n f o

Article history:
Received 5 February 2008
Received in revised form 8 June 2008
Accepted 11 June 2008
Available online 22 June 2008
Keywords:
Long period ber gratings
Pd
Hydrogen sensor
Response time
Stability

a b s t r a c t
A ber-optic sensor for detecting hydrogen at various temperatures (30200 C) is reported in this paper.
The sensor is composed of a long period ber gratings coated with a nano-structured Pd thin layer as the
sensing material. The sensing principle of the designed sensor is based on the change of the refractive
index of the Pd thin layer upon exposure to hydrogen, which causes the resonance wavelength shift of
the long period ber gratings. The Pd layer prepared by sputter deposition has nanograins of 3040 nm
in size. The resonance wavelength of the long period ber gratings coated with Pd decreases as hydrogen
concentration increases from 0% to 16% at all temperatures. There is a signicant wavelength shift of the
sensor when the Pd lm goes through the phase transition between and phases. The sensor has a
short response time with a relatively slower recovery rate. The sensor maintains its functionality after
several cycles of hydrogen detection and recovery.
2008 Elsevier B.V. All rights reserved.

1. Introduction
Fossil fuels will remain to be a dominant energy source in the
near future. The US Department of Energy predicts that by 2020,
90% of the energy needs rely on fossil fuels [1]. As compared to
the traditional fossil fuel power plant with 3540% efciency, the
integrated gasication combined cycle (IGCC) power plant which
was introduced in the last ten years possesses a higher efciency of
50% [2]. Hydrogen is one of the gas components of the syngas produced during the coal gasication in IGCC. Therefore, introducing
a high temperature hydrogen sensor into the IGCC for the in-situ
hydrogen monitoring is important for process control, efciency
improvement and safe operation of the IGCC process.
In the last 20 years, great efforts have been devoted to developing and commercializing electrical based hydrogen sensors [3,4].
Even though some of them exhibit high sensitivity and fast response
at either room temperature or elevated temperatures, a main drawback of this type of sensor is that the use of electricity may lead to
sparks at the sensing point. As an alternative, optical techniques are
more attractive due to the lack of sparking possibilities. Recently,
development of optical type hydrogen sensors based on optical
bers [510], switchable mirrors [11] and other techniques [12]
has been reported by several research groups. Typically, an opti-

Corresponding author. Tel.: +1 480 965 7769.

E-mail address: Jerry.Lin@asu.edu (Y.S. Lin).
0925-4005/$ see front matter 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2008.06.018

cal type hydrogen sensor consists of an optical signal generation

and transmission component and a layer of sensing material. The
hydrogen can be detected upon the interaction with the sensing
material which causes the change in the optical properties. Among
these sensors, the ones based on optical bers are more attractive since the optical ber can help realize the remote control of
processes.
Because of the fast absorption kinetics, high hydrogen solubility and selectivity towards hydrogen absorption at relative low
temperature, Pd and Pd alloys have been used as the hydrogen
sensing material in many optical sensors. For instance, Butler [13]
coated one end of the optical ber with Pd and the hydrogen
can be detected based on the reectance change of the Pd due
to the hydrogen absorption. Later on, Tabib-Azar et al. [14] coated
the outside of a multimode optical ber with Pd. The change in
the refractive index of Pd caused by the absorption of hydrogen
resulted in changes in both the phase and the absorption of the
guided light. Bvenot et al. [6] coated an optical ber with Pd
to develop a surface plasmon resonance sensor and the sensing
signal was caused by the Pd complex permittivity change due to
the hydrogen absorption. In the last 23 years, Pd-coating of a
modied optical ber such as ber-taper [8,9] and ber Bragg gratings (FBGs) [15] was reported to develop hydrogen sensors. Up
to now, most of the work reported on Pd-based optical hydrogen
sensors is aimed at the leak detection or hydrogen concentration monitoring at low temperature. High temperature sensors
impose a more stringent requirement on sensing materials and

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Fig. 1. Schematic of the Pd-LPFGs hydrogen sensor.

other sensor components, and therefore are more difcult to

develop.
Recently, long period ber gratings (LPFGs) gained many interests due to the improved sensitivity to many parameters such as
temperature, strain, and environmental refractive index as compared to the FBGs. Once coated with sensing material on the
cladding at the grating region, upon the change of refractive index,
the LPFGs can serve as a gas or liquid sensor and show very good
sensitivity towards the target materials [1619]. In 2006, Trouillet
et al. [16] reported the use of the Pd-coated LPFGs as a hydrogen sensor. In their work, Pd was deposited on one side of the
optical ber, which was modied into LPFGs. The sensor shows
improved response as compared to the Pd-coated ber Bragg grating. However, in their work [16] the sensor was only tested at room
temperature, and the response time and sensor stability were not
reported in detail.
The structure of the hydrogen sensor developed in the current
work is schematically shown in Fig. 1. The sensor consists of a LPFGs
as the optical signal generation and transmission component and a
thin layer of Pd as the sensing material. The application of this sensor to measure hydrogen concentration in the temperature range of
30250 C was studied. The objective is to evaluate the functionality of this type of sensor to monitor hydrogen at high temperatures
and the potential of using LPFGs as an optical gas sensing component in the IGCC process. The kinetics of hydrogen absorption
and desorption by the Pd thin lm was also analyzed based on the
response and recovery times of this sensor.
2. Principle of operation
A LPFGs is a device with induced periodic change in the refractive
index of the ber with a period in the range of 0.11 mm, which is
many times higher than the light wavelength in the ber. In a LPFGs,
a fundamental core mode and multiple cladding modes exist and
propagate in the same direction. The energy propagating in the fundamental core mode to the discrete cladding modes results in the
transmission spectrum of the ber which contains a series of attenuation bands centered at discrete wavelengths, namely resonance
wavelength R (wavelength at minimum transmission). The light
is coupled effectively following the phase match conditions:
1 2 =

2
2
(ne1 ne2 ) =
R


(1)

where 1 and 2 are the propagation constant of the core and

cladding, respectively, ne1 and ne2 are the core and cladding mode
effective refractive indices, respectively, and  is the period of the
grating. When a sensing layer is coated outside the cladding area,

changes in the refractive index of the sensing layer could result in

the change in the effective refractive index of the cladding (ne2 ),
which leads to the shift of resonance wavelength.
The sensor designed in this work uses Pd as the sensing material. When Pd is exposed to hydrogen, hydrogen dissociates into
two hydrogen atoms at the Pd surface with an efcient rate. The
hydrogen atoms then diffuse into the bulk Pd, leading to formation
of palladium hydride (PdH). The ratio between Pd and hydrogen
atoms, which is characterized by the existence of two different
crystallographic phases, and , depends on the hydrogen partial pressure and temperature [20]. In phase, hydrogen is slightly
absorbed into the lattice, which leads to a slight increase in the
lattice parameter (within 0.4% in length). As the hydrogen partial
pressure increases, the transition from to phase occurs, resulting in a drastic lattice parameter increase (around 3% in length). The
increase in the lattice parameters consequently causes a decrease
in the volume density of free electrons. This, therefore, causes a
change in the electrical and optical properties [21].
To date, many of the hydrogen sensors reported relied on the
phase transition into phase at room temperature or even lower.
However, when temperature is higher than 100 C, the phase transition will not occur unless the metal is exposed to the environment
with relatively high hydrogen partial pressure. This causes the poor
sensitivity of these sensors at elevated temperatures. Therefore,
deposition of Pd onto a platform which has higher resolution is
necessary for development of a Pd-based hydrogen sensor for high
temperature application. In the current work, a thin layer of Pd is
coated on the cladding at the grating section of a LPFGs. A change
in the refractive index of Pd upon exposure to hydrogen results in a
shift of the resonance wavelength of the LPFGs. The sensor is based
on measuring the resonance wavelength shift which is a function
of hydrogen concentration.

3. Experimental
LPFGs inscription was performed by the method adopted from
the literature [22,23]. Briey, the focused CO2 laser line was transversely loaded onto a single mode optical ber (Corning SMF-28)
which was moved by a computer-controlled precise translation
stage with a period (around 500 m) between two shots. An
online monitoring system containing a tunable laser source (Agilent 8164A) with a step of 1 nm scanning from 1510 nm to 1640 nm
and a spectrometer (Agilent 81618A) was applied to take the LPFGs
transmission spectrum during fabrication.
A Pd thin layer was deposited on the cladding area of the ber
grating (6 cm long) by DC magnetron sputtering. A Pd foil (Alfa
Aesar, 99.9%) was used as the target. The distance between the target and the ber was kept at 10 cm. Prior to the deposition, the
chamber was evacuated to a pressure in the range of 106 Torr
and then back lled with ultra high purity argon at a pressure of
5 103 Torr. Pd was sputtered at a power of 10 W for 10 min at
room temperature. The deposition rate was about 7 nm/min. During the deposition, the ber was rotated periodically in order to
acquire the thin layer with relatively uniform thickness. The whole
lm morphology and Pd grain size were characterized by SEM and
the composition was analyzed by EDS. The spectra of the LPFGs
before and after Pd coating were recorded prior to the sensor test.
The experimental setup used to test the sensor performance
under various conditions is shown in Fig. 2. The LPFGs coated
with Pd was sealed in a 1/4 inch stainless steel tube and placed
in a furnace (LINDBERG UP150). The ends of the ber were connected to a light source and a detector by a splicer (SUMITOMO
TYPE-36), respectively. The light source is a combination of C band
and L band light source, which has a broadband from 1510 nm to

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689

Fig. 2. Apparatus of the hydrogen sensing test setup.

1620 nm totally. An HP 70952 B optical spectrum analyzer was used

as the detector. The resolution of the HP 70952 B is 10 pm. During the data analysis process, the collected data was tted by a
polynomial of four orders to obtain the moving trend of the peak
instead of the lowest point, which dramatically increased the measurement accuracy. The resonance wavelength of the attenuation
band with the highest energy loss was selected as the sensing signal. Before the experiment, the ber was pretreated in 4% H2 /He
for 4 h at 300 C to remove the gas molecules such as CO, CO2
and O2 adsorbed on the Pd surface which might affect the hydrogen absorption rate. During the experiment, the Pd-LPFGs was
preheated at a desired temperature in helium. The hydrogen and
helium ow rates were monitored by mass ow controllers. When
the gas environment was switched between He and a H2 /He mixture, it took about 30 s to reach a desired gas composition in the
stainless steel tube. The transmission spectra were recorded around
every 13 s.

attenuation band decreases and the peak becomes broader. Pd is a

metal with a higher refractive index than air. Therefore, Pd-coating
of LPFGs results in the changes of the boundary conditions of the
cladding modes and the Bragg diffraction. Consequently, the resonance quality is reduced because the coupling condition is not as
critical as the one without any coating.

4. Results and discussion

Fig. 3(a) and (b) shows scanning electronic micrographs of the
Pd-coated LPFGs (Pd-LPFGs). The Pd lm thickness is estimated at
about 70 nm from the deposition time and growth rate. The particles shown in Fig. 3(a) are dirt from the atmosphere. There are some
very minor defects observed on this image. The nano-structured Pd
has the grain size distributed in the range of 3040 nm, as shown
in Fig. 3(b). The nanoparticles agglomerate and form a continuous lm. In order to estimate uniformity of the Pd lm around the
ber, EDS line analysis was carried out at a random spot along
and across the ber, respectively. As seen in Fig. 4, the intensity of the signal for Pd shows a plateau in both directions; along
(Fig. 4(a)) and across (Fig. 4(b)) the ber. The intensity of silicon is
also shown as a reference. Both the SEM images and the EDS line
analysis conrm the high quality of the Pd lm deposited on the
ber.
The transmission spectra of the LPFGs before and after Pd coating are shown in Fig. 5. Each measured transmission spectrum was
t with a polynomial of four orders in order to obtain the accurate
resonance wavelength of the Pd-LPFGs. Without the Pd coating, the
spectrum exhibits several attenuation bands among which the one
centered at 1564 nm has an energy loss up to approximately 24 dB.
For LPFGs, the resolution is higher with a larger energy loss. Therefore, the high energy loss indicates the high quality of the LPFGs
prepared in this work. With Pd coating, the energy loss of the same

Fig. 3. SEM images of (a) an optical ber coated with Pd and (b) Pd grains and
agglomerates.

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X. Wei et al. / Sensors and Actuators B 134 (2008) 687693

Fig. 6. (a) Spectra of LPFGs coated with Pd in 8% H2 and H2 free atmosphere at 30 C.

(b) Resonance wavelength of LPFGs coated with Pd in 8% H2 and H2 free atmosphere
as a function of temperature.
Fig. 4. Elemental analysis on LPFGs coated with Pd by EDS line scan; (a) along and
(b) across the ber (white line on the SEM image indicates the direction along which
the line scan was carried out).

Fig. 5. Transmission spectra of LPFGs before and after Pd coating.

The Pd-LPFGs sensor was tested in the temperature range of

30250 C under various hydrogen concentrations. The transmission spectra of Pd-LPFGs in He and 8% hydrogen at 30 C are shown
in Fig. 6(a). After hydrogen was introduced into the system, the
shift of the resonance wavelength towards the lower wavelength
can be observed. Fig. 6(b) shows the resonance wavelength of the
Pd-LPFGs in He and 8% H2 /He as a function of temperature. In our
work, the shift of resonance wavelength is found to be +35 pm/ C
in He, as shown in Fig. 6(b). When tested in the temperature range
of 30200 C, the resonance wavelength of the Pd-LPFGs shifted
towards the lower wavelength in 8% H2 /He as compared to He.
At 250 C, the amount of hydrogen dissolved into Pd is too small
to cause any observable and reproducible wavelength shift in the
hydrogen concentration range studied in this work (016%).
The dependence of the resonance wavelength shift on the hydrogen concentration at different temperatures is shown in Fig. 7. It
can be seen that the resonance wavelength decreases as the hydrogen concentration increases at all temperatures. At 30 C, there
is a sharp decrease in the resonance wavelength when hydrogen
concentration increases from 1% to 2%. This is due to a jump in
hydrogen concentration (and lattice parameter) in Pd as a result
of to phase transition. These changes cause drastic changes
in refractive index, resulting in the pronounced shift of the resonance wavelength. Further increasing the hydrogen concentration
from 2% to 16% leads to a much less signicant wavelength shift

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691

the completely stabilized point. At 100 C, the recovery time is

shorter.
The response and recovery time of the sensor is mainly determined by the surface reaction and hydrogen diffusion process
in Pd. The transport of hydrogen through the Pd layer involves
three steps. Once the Pd thin layer is exposed to hydrogen,
hydrogen is dissociated into two hydrogen atoms or forms protons and then the atoms diffuse into the bulk metal. In the
bulk, there is a net transport of hydrogen atoms driven by the
hydrogen concentration gradient. The hydrogen atoms recombine
and form hydrogen molecules again during the desorption process.
Ideally, the dissociation of hydrogen on a clean Pd surface is a
barrierless process [24], followed by the diffusion of the surface H
atoms into the Pd lms. Hence, the diffusion of hydrogen atoms
through the Pd layer is the rate limiting step. In our work, the
hydrogen transport through the Pd layer with a very small thickness
(70 nm) with the corresponding diffusivity of 107 cm2 /s in phase
and 106 cm2 /s in phase [25]. At 30 C, the / phase boundary
movement rate is reported to be around 3550 nm/s [25]. Therefore, the response time of the sensor developed in this work can
be expected to be less than 3 s. The actual response time is longer
than the estimated one. This is likely due to the adsorption of certain amounts of oxygen, carbon monoxide and other compounds
which are known to interfere with the absorption of hydrogen [26]
since the sensor device was not kept under a special care to preserve
an atomically clean surface.

Fig. 7. Resonance wavelength shift as a function of H2 concentration at (a) 30 C and

(b) 100 C, 150 C and 200 C (the line was added for visual guide).

because PdH is in the phase, in which hydrogen concentration

increases continuously with the gas phase hydrogen concentration. The extent of resonance wavelength shift highly depends
on the temperature. As explained in the principle, the hydrogen
absorption capacity of Pd decreases signicantly as the temperature increases, causing a less change in the refractive index of Pd
at higher temperatures. It should be noted that at 200 C a shift
of 11 pm in the resonance wavelength can be observed when
exposed to 4% H2 even though the ratio between H and Pd is
smaller than 0.01 in PdHx [20]. This indicates the high resolution of this technique for hydrogen sensing up to 200 C. However,
the change is smaller than the response induced by 1 C temperature variation. Therefore, it is necessary to take into account
the gas temperature variations in the operation of such a sensor.
Fig. 8 shows the response and recovery rates of the Pd-LPFGs
sensor subjected to an increase in hydrogen concentration in the
gas stream between 0% (in pure helium) and 4% (hydrogen in
helium) at 30 C and 100 C, respectively. The time taken for the
resonance wavelength to reach complete equilibrium after hydrogen partial changes is considered as the response/recovery time.
At each temperature, the response time to the increase of hydrogen concentration is less than 70 s. Compared to the hydrogen
uptake process, the recovery time is longer. At 30 C, it takes about
5 min to get 90% of the total resonance wavelength shift back
to the one in helium. However, it takes about 14 min to reach

Fig. 8. Response and recover times of LPFGs in 4% H2 at (a) 30 C and (b) 100 C.

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X. Wei et al. / Sensors and Actuators B 134 (2008) 687693

The recovery time is longer than the response time at lower

temperatures. This indicates a slower hydrogen desorption rate
corresponding the phase change from to . This hysteresis for
hydrogen transport in the PdH system was reported by other
researchers [24,27]. It is attributed to the macroscopic energy barrier between the transforming phases arising from the coherent
strains, which opposes both the forward and reverse isostructural
hydriding transformations [24,28,29]. At elevated temperatures,
the recovery time is much faster for the sensor without going
through the phase change.
Fig. 9 shows the changes of the resonance wavelength of the
Pd-LPFGs sensor subjected to multiple cycles of hydrogen concentration change in the gas stream between pure helium and 4%
hydrogen in helium, at 30 C and 100 C, respectively. At 30 C, the
resonance wavelength could not return completely to the initial
point during the rst two cycles. After the rst cycle, there is a
18 pm wavelength shift while after the second cycle, a shift of
about 7 pm is observed. Beginning with the third cycle, no wavelength shift is observed. As mentioned before, the Pd lm goes
through phase transition when exposed to 4% hydrogen at 30 C.
In phase, there is a signicant increase in the lattice parameter of
Pd as compared to pure Pd or PdH in phase. When hydrogen desorbs from the Pd lattice, due to the lattice swelling effect, the strain
in the lm may lead to a variation in the Pd lm morphology, which
causes a slight change in the ne2 compared to the fresh lm. After
several cycles, the change in the lm morphology becomes negligible. At 100 C, the resonance wavelength can return to the starting

line after each cycle. This is because the Pd lm does not go through
the phase change during the cycles at this temperature, so that
it can maintain the original properties.
5. Conclusions
The use of Pd-coated LPFGs as a hydrogen sensor in the temperature range of 30200 C is demonstrated in this work. The
exposure of the sensor to hydrogen leads the attenuation band
of the transmission spectrum of LPFGs to shift towards the lower
wavelength at all the temperatures. The resonance wavelength
decreases as the hydrogen concentration increases in the range
from 0% to 16%. There is a signicant wavelength shift of the sensor when the Pd lm goes through the to phase change. The
sensor has short response time with relatively long recovery time
at low temperatures. Multiple cycle test conrms the stability of
the sensor for hydrogen detection. The results show feasibility of
using LPFGs, when coated with an appropriate sensing material,
offering the potential for sensing hydrogen at high temperatures in
the IGCC streams. Future work will focus on exploration of other
sensing materials with improved sensitivity and chemical stability
for detection of hydrogen and other gases in IGCC streams
Acknowledgement
The project was supported by Department of Energy through
grant (DE-FC26-O5NT42439).
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Fig. 9. Stability test of LPFGs coated with Pd at (a) 30 C and (b) 100 C.

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Biographies
Xiaotong Wei received his B.S. (2003) from Tsinghua University in China, and M.S.
from University of Cincinnati (2005) in the U.S., both in chemical engineering.
Presently, he is working towards the Ph.D. degree in the Materials for Separation
Lab, Department of Chemical Engineering, Arizona State University. His research
interests include development of novel inorganic materials for high temperature
gas sensing and gas separation.
Tao Wei received the M.S. degree from Electrical and Computer Engineering
Department, Missouri University of Science and Technology (formerly University
of Missouri Rolla), MO, in 2008. He is currently working towards the Ph.D. degree
in electrical engineering at Missouri University of Science and Technology. His current research interests include development of ber Fabry-Perot devices and the
optimization of long period ber gratings.
Dr. Hai Xiao received his Ph.D. in electrical engineering from Virginia Polytechnic
Institute and State University (Virginia Tech), Blacksburg, Virginia, in 2000. He is currently an associate professor of Electrical Engineering at the Missouri University of
Science and Technology. His research interests include novel photonic device design
and fabrication, sensors for harsh environments, nanomaterials and nanostructures
for chemical sensing, optical spectroscopy, and computer vision.
Dr. Jerry Y.S. Lin received his B.S. (1982) from Zhejiang University in China and
M.S. (1985), and Ph.D. (1988) from Worcester Polytechnic Institute in the U.S., all
in chemical engineering. He was a post-doctoral staff member at the University of
Twente in the Netherlands (19881991). Currently, he is a professor and department
chair of Chemical Engineering at Arizona State University. His research interest is in
inorganic membrane science and adsorption separation.