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AbstractA hollow-core photonic bandgap (PBG) fiber sensing the inlet of the fiber relative to the outlet pressure at the distal
configuration for optical absorption spectroscopy of multiple-com- end. The filling gas displaces the resident gas in a piston-like
ponent gas samples absent of a vacuum environment is presented. fashion without the assistance of a vacuum. The measured filling
Pressure-driven sensor response times that are shorter in dura-
tion compared to diffusion-limited filling times for fiber lengths times for a 2 m length of PBG fiber were in good agreement with
1 m are reported. Reduced filling times that approach the sub- the estimated filling times. The filling times were significantly
minute regime are possible for a 2 meter length of commercially enhanced by the pressure differential along the length of the
available PBG fiber with a 12.5 micron core diameter at a pres- fiber. For a pressure differential of 14.7 Psi, the filling time for
sure 15 Psi. The spectroscopy measurements were limited to the 2 m of fiber was approximately 120 s, whereas diffusion filling
near-IR region for sample gases that include acetylene and carbon
dioxide. Using the techniques presented, the detection of concen- would take 120 000 s.
trations 100 ppm for acetylene gas at pressures 15 Psi is pos- A PBG fiber based spectroscopic sensor that simultaneously
sible. detects multiple-component gases is presented in this paper.
Index TermsGas sensing, hollow-core photonic bandgap fiber, The fiber system was loaded via a pressure-driven gas-filling
spectroscopy. method with acetylene, C H and carbon dioxide, CO gases at
varied concentrations. These gases were selected because they
possessed spectral absorption characteristics that are compat-
I. INTRODUCTION ible with light sources that were used in the proposed sensing
arrangement. Gas-loading techniques are described that demon-
XAMPLES of optical absorption spectroscopy for the
E sensing of gases [1] and detection of biomolecules in
liquids [2] using microstructured optical fibers have previ-
strated sub-minute filling times for PBG fiber lengths
allows access to the filled fiber for manipulation and compact
m and
packaging. The strong overlap of the optical field with the gas,
ously been reported. Potential applications for gas sensing
which were both confined to the hollow-core region with the gas
hollow- core photonic bandgap (PBG) fibers include moni-
was exploited to enhance detector sensitivity over long lengths
toring methane in hazardous environments [3], sensing low
with a 27 m PBG fiber.
concentrations of ammonia for the semiconductor manufac-
Evidence of simultaneous detection of a mixture of two
turing industry [4] and for absolute wavelength referencing
gases (50%CO and 5%C H ), demonstrated the selectivity
with acetylene [5], [6]. Early fiber gas-loading techniques
capacity of the configuration. Enhanced sensor response-times
involved filling methods that operate at pressures that rely on
that are a function of filling-pressure, fiber length and gas
diffusion and vacuum conditions to fill the fiber which leads to
viscosity are presented in this article. Filling times that are
limited response times on the order of minutes for lengths
practical for sensing applications are also emphasized. The
m [4], [7], [8].
peak broadening characteristics of the absorption lines were
The pressure-driven method reported here is proposed as an
investigated to determine the pressure limitations that must be
alternative approach for filling PBG fibers at a much higher rate
considered for enhanced sensitivity and spectroscopic resolu-
than the diffusion method. In the present method, the sample
tion. The measurements from our sensing scheme are reported
gas fills the PBG fiber as a result of the increased pressure at
and are in agreement with standard spectroscopic information
on acetylene and carbon dioxide absorption characteristics [6],
Manuscript received October 30, 2008; revised March 17, 2009. Current ver- [9], [10], [11].
sion published May 20, 2009. This work was supported in part by the U.S. Office
of Naval Research Award No. N00014-06-1-0479.
R. M. Wynne is with the Department of Electrical and Computer En-
gineering, Villanova University, Villanova, PA 19085-1681 USA (e-mail: II. PRINCIPLE OF OPERATION
rosalind.wynne@villanova.edu, rwynne@ece.villanova.edu).
B. Barabadi was with Department of Mechanical Engineering, Villanova Uni-
versity, Villanova, PA 19085-1681 USA. She is now with the Department of A. Absorption Spectroscopy
Mechanical Engineering, Georgia Institute of Technology, Atlanta, GA 30332
USA (e-mail: banafsheh.barabadi@villanova.edu). Absorption spectroscopy exploits the characteristic absorp-
K. J. Creedon was with Department of Electrical and Computer Engineering,
Villanova University, Villanova, PA 19085-1681 USA. He is now with Lincoln
tion of radiation that corresponds to the wavelengths associated
Laboratory at MIT, Lexington, MA 02420 USA. (e-mail: kevin.creedon@vil- with the excitation of atoms in the sample. The characteristic ab-
lanova.edu). sorption spectra are usually well defined making the detection
A. Ortega is with James R. Birle Professor of Energy Technology, Associate method highly selective. The sensitivity of wavelength selective
Dean for Graduate Studies and Research, Villanova University, College of En-
gineering, Villanova, PA 19085 USA (e-mail: alfonso.ortega@villanova.edu). spectroscopy is dependent on the path length of the absorption
Digital Object Identifier 10.1109/JLT.2009.2019258 process in the sample, concentration of the sample and the line
0733-8724/$25.00 2009 IEEE
WYNNE et al.: HOLLOW-CORE PHOTONIC BANDGAP FIBER GAS SENSOR 1591
B. Spectroscopic Measurements
Spectroscopic data were collected for the different fiber con-
figurations. The normalized absorption peaks of the character-
Fig. 2. PBG fiber gas loading system is shown where one of the gas housing istic spectra were monitored to observe the filling times, pres-
components is connected to a gas cylinder for filling the PBG fiber. (Single mode
optical fiber: SMF and Multi-mode optical fiber: MMF.). sure broadening of peaks and bend sensitivity of the gas-filled
fiber.
Simultaneous detection of individual gases in a mixture using
are similar,the filling time is linearly dependent on viscosity. a 27 m length of PBG fiber was spectroscopically confirmed.
Similarly, increased viscosity results in longer filling times. The measured spectra are consistent with existing reference
Also, depends inversely on the pressure difference and fiber spectra for the sample gases [11]. The 27 m PBG fiber was
core diameter. It is strongly dependent on the fiber length such assembled in the arrangement described in Section III.A.
that the length and the core diameter of the fiber are significant The gas mixture consisted of 5% C H and 50% CO with a
factors in the filling time. balance of nitrogen. The absorption line strengths of CO are
significantly less (by nearly 3 orders of magnitude) than C H
III. EXPERIMENTAL TECHNIQUE in the spectral region of interest. The absorption behavior is
highlighted by the growth rate of the absorption peaks as the
A. Fiber Filling Apparatus fiber was filled with the gas mixture. Initially, the C H peaks
Sections of PBG fiber (Corning PBG-1550) with a were pronounced and then mostly disappeared into the noise
transmission window between 1480-nm and 1640-nm were region by the time the CO peaks were fully realized. (See
prepared and inserted into the gas system. The coating of Fig. 3.) Not only can the two gases be identified spectroscop-
the fiber was mechanically stripped and was cleaved using a ically but the concentration of each gas can be estimated by
Fujikara CT-04 cleaver. Initially, the prepared fiber ends comparing absorbance measurements to a calibrated reference.
were placed into two separate hermetically sealed aluminum For example, the absorbance of a normalized CO peak at
housing components with a gas-filling or evacuation port. (See 1571.12 nm for a 50% concentration is dB. When this
Fig. 2) A light source was launched into the PBG fiber via a value is compared to an absorbance of dB for a 100%
butt-coupled conventional single mode fiber. The transmitted concentration, a ratio of 0.461 is produced that is consistent
light was coupled out of the PBG fiber through to a butt-cou- with the ratio of 0.5 for the two concentrations.
pled conventional multi-mode fiber. The output light was then Considerations should be made for pressure limitations that
transmitted to an optical spectrum analyzer (OSA). A small are important for spectroscopic accuracy in terms of peak
gap ( m) was formed between the butt-coupled fiber width. It was apparent that the filling dynamics were a function
ends to allow gas to enter/exit the hollow core of the fiber. of pressure. Absorption peaks typically experience linewidth
Losses due to the butt-coupled PBG fiber were less than dB broadening at relatively high pressures ( 15 Psi). The pres-
relative to the transmission baseline of an unfilled system for sure broadening was determined by fitting the peak data to a
each configuration [22]. Lorenztian lineshape and measuring the change in the linewidth
Light from a broadband source centered at 1550 nm wave- due to increased pressure. The peak broadening measurements
length was directed into and out of the hollow core of the and linewidth expansion as a function of pressure are listed in
fiber. The alignment conditions were monitored using a camera Table I
system to image the hollow core region at the fiber output and The broadened absorption peaks for acetylene exhibited rel-
verify that the light was launched into the hollow core at the atively wide linewidths. Measurement standards approximate
fiber input. typical linewidths to be 140 pm for tunable laser schemes [10]
The gas-loading procedure required that the fiber be purged at 1528.03 nm for pressures near 15 Psi (above atmospheric
with nitrogen to remove residual gases in the PBG fiber and pressure). Detection schemes that use broadband light sources
to obtain a spectroscopic baseline reading for comparative pur- typically produce wide linewidths in comparison to schemes
poses. The gas sample was then admitted to the gas housing at that use tunable laser diodes. The relative absorption based
a designated pressure that was monitored by a pressure trans- on broadband light sources is usually low compared to laser
ducer. Pressures were measured above ambient pressure at room sources. In order to have a sufficient signal-to-noise ratio the
temperature. The sample gas flowed through the PBG fiber and spectrometer resolution was sacrificed. The measured linewidth
vented to atmospheric pressure at the second butt-coupled sec- of the peaks is usually governed by the spectral resolution of
tion. The transmitted output was measured by the OSA at 0.2 the spectrometer [23]. The optical spectrum analyzer that was
nm resolution. The spectral information was recorded at regular employed in this study had a resolution of 0.2 nm in order to
WYNNE et al.: HOLLOW-CORE PHOTONIC BANDGAP FIBER GAS SENSOR 1593
TABLE I
LINEWIDTH MEASUREMENTS AS A FUNCTION OF PRESSURE
TABLE II
3
COMPARISON OF AVERAGE GAS-FILLING TIME, , AS A FUNCTION OF
CONCENTRATION FOR (A) 0.3 M FIBER LENGTH AT A PRESSURE OF 15 PSI,
(B) 0.7 M FIBER LENGTH AT A PRESSURE OF 14.5 PSI, AND (C) 27 M FIBER
LENGTH AT A PRESSURE OF 17 PSI
TABLE III of the filling gas molecules into the gas resident in the fiber, usu-
THEORETICAL MINIMUM DETECTABLE CONCENTRATIONS ally air at ambient conditions. In [1] the authors measured the
filling rate of acetylene into air, in a microstructured fiber with
a length of 10 cm and diameter of 10.5 m. From simple diffu-
sion theory [15], the characteristic diffusion time scale can be
estimated as the fiber length squared divided by the diffusion
coefficient. The length and diffusion coefficient used in [1] are
respectively 10 cm and 0.17552 cm s . Their experimentally
measured filling time was approximately 300 s, which is very
much in line with the order of magnitude of the characteristic
diffusion time scale.
In the gas regimes of interest, the filling rates are governed
by a classical laminar but unsteady fluid dynamics theory, in
which the filling gas displaces the resident gas in a piston-like
fashion. With the viscosity of acetylene taken as Ns
m ; flowing in a tube with diameter 12.5 m and length of 10
cm (as in [1]), the time scale for filling is calculated to be three
orders of magnitude smaller than that observed by reference [1]
in diffusion driven filling. For the parameters of the experiment
in [1] where acetylene gas was introduced to the system at 15
psi above the ambient pressure, pressure filling would take 0.3
s, as compared to 300 s using diffusion.
Fig. 8. Trends of absorption versus fiber length for different concentrations of V. CONCLUSION
C H .
Optical absorption spectroscopy based on a hollow-core PBG
fiber was demonstrated on fiber lengths as long as 27 m and
minimum concentration levels of 120 ppm for C H . Detec- while presenting relatively short gas-filling periods. Detection
tion sensitivity is typically limited by source fluctuations in ad- of concentrations as low as 50 ppm C H were observed for a
dition to the detector noise with detectable absorption limits at 27 m hollow-core PBG fiber. The gas loading system was filled
relative absorptions on the order of to [23]. These with acetylene and carbon dioxide gases at pressures ranging
detection limits can be enhanced by adopting a narrow band- from 2 Psi to 17 Psi (above atmospheric pressure). Absorption
width light source (e.g., laser) such that as the source linewidth spectra were observed to be consistent with the 1550 nm region
decreases the detection limits are reduced and the smallest ob- characteristic peaks of acetylene and carbon dioxide. The pre-
servable signal is significantly larger than limits based on con- sented results reveal sub-minute filling times that are conducive
ventional broadband source spectroscopy. Lasers with relatively to fast detector response times for fiber lengths m for pres-
high intensities can increase the signal-to-noise ratio to suppress sures Psi. Multiple gas components in a mixture were si-
the detector noise that restricts sensitivity. multaneous sensed in a 27 m PBG fiber demonstrating inherent
The relationship between PBG fiber length and measured ab- selectivity qualities of sensing systems that are based on optical
sorbance was examined and compared for C H at gas concen- absorption spectroscopy.
trations of 100%, 50% and 5% (in mixture). The data followed These promising results show that pressure-driven filling is
linear trends which is an indication that Beers law from (1) gov- significantly faster than diffusion methods. It is recommended
erned the absorption process for the PBG fiber configuration. that the initial pressure-driven model be modified to be a
(See Fig. 8.) The sensor was calibrated with specific concentra- more accurate model considering actual viscosities for the
tions of the sample gases. The calibration verified that the de- initial gas and the filling gas. The dynamic nature of the pres-
vice absorbance levels are proportional to the gas concentration sure-driven gas-filling process may cause uncharacteristically
levels. The linear fit of the data produced slopes that are propor- wide linewidths. It is possible to reduce the gas pressure of the
tional to the concentration of the sample C H gas. system ( Psi) after the fiber length has been completely filled
Bend losses for a 27 m gas-filled PBG fiber appeared to be to reduce the pressure broadening effects. A pressure reduction
negligible. The losses are negligible and independent of bend post filling with a relative change of 10 may increase the overall
radii, in general, for Corning PBG-1550. Measurements were sensor response time by a factor of 2 which is still significantly
obtained for bend loss were dB per millimeter of bend faster than diffusion rates. A modified pressure-driven process
radius for radii in the range of 5 mm to 75 mm. that will address these recommendations will be presented in
Based on the initial findings of pressure-driven fiber filling re- future work. The findings in this paper may contribute to the
ported here, several early observations can be made with regard advancement of PBG fiber based absorption spectroscopy. PBG
to its practical application, especially in comparison to tradi- fiber devices that can demonstrate fast response times, high
tional diffusion filling methods. The traditional diffusion filling sensitivity and high selectivity detection in a compact rugged
method, as for example reported in [1], depends on the diffusion device may be an improvement on existing schemes.
1596 JOURNAL OF LIGHTWAVE TECHNOLOGY, VOL. 27, NO. 11, JUNE 1, 2009
REFERENCES
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fiber, Opt. Eng., vol. 41, no. 1, pp. 89, 2002. Rosalind M. Wynne (M04) received the B.S. degree in physics from Norfolk
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[3] . Kornaszewski et al., Mid-infrared methane detection in a photonic She recently received a tenure-track Assistant Professor position at Villanova
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139204, 2005. He currently holds an assistant staff position in the Laser Technology and
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ened detection of C H in the parts per trillion range, J. Opt. Soc. Alfonso Ortega received the B.S. degree in mechanical engineering from the
Amer. B, vol. 24, no. 6, 2007. University of Texas at El Paso in 1976, and the M.S. and Ph.D. degrees in me-
[15] R. B. Bird, Transport Phenomena. New York: Wiley, 1960. chanical engineering from Stanford University, Stanford, CA, in 1978 and 1986,
[16] P. K. Kundu et al., Mechanics of Fluids. Amsterdam, Netherlands: respectively.
Elsevier Academic Press, 2004, vol. ED-3. He is the Associate Dean for Graduate Studies and Research for the College
[17] I. H. Shames, Mechanics of Fluids. New York: McGraw Hill, 1982, of Engineering at Villanova University, Villanova, PA and the James R. Birle
vol. ED-2. Professor of Energy Technology in the Department of Mechanical Engineering.
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[19] D. Seibet et al., Viscosity measurements on nitrogen, J. Chem. Eng. of turbo-machinery. He has published extensively on air-cooling of electronics,
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[20] R. Fox and A. McDonald, Introduction to Fluid Mechanics. New surements in the thermal sciences.
York: Wiley, 1998. Dr. Ortega is a Fellow of the ASME. He is the former Chairman of the
[21] S. C. Saxena and R. S. Gambhir, The viscosity and translational ASME/IEEE ITHERM Symposium (1994), the IEEE SEMITHERM Sym-
thermal conductivity of gas mixtures, Brit. J. Appl. Phys., vol. 14, posium (1994), and recipient of the 2002 IEEE SEMITHERM Significant
1963. Contributor Award.