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5 TAKARA, H , KAWANISHI, s , MORIOKA, T.

, MORI, K , and Design: Planar waveguides were formed in BK7 glass substrates by
SARUWATARI, M : '100Gbitk optical waveform measurement with the K+-Na+ ion-exchange process. Substrates were cleaned and
0 . 6 ~ sresolution optical sampling using supercontinuum pulses', placed in a bath of pure KNO, at 375°C for 3Sh, forming a 3 p -
Electron. Lett., 1994, 30, pp. 1152-1153 deep waveguide. Next, thin f i s of SiO,, TiO,, Au and SiO, were
sequentially deposited by electron-beam evaporation. Lastly, the
endfacets of the waveguide were polished. The complete structure
is shown in Fig. 1.
superstrate
xperimental investigation of a surface
p l a s m ~ n - ~ a s eintegrated-optic
d humidity
sensor
M.N. Weiss, R. Srivastava a n d H. Groger
input output

Indexing terms: Humidity sensors, Integrated optics, Optical in BK7 substrate


sensors
1402111
A humidity sensor has been fabricated by coating a surface Fig. 1 Surface plasmon waveguide structure
plasmon waveguide with a t h layer of Nafion fluoropolymer.
The refractive index of Nafion varies as a function of humidity,
causing a shift in the plasmon resonance wavelength. The present In this device, the lower SiO, layer serves as a buffer to control
device is able to measure relative humidity over a range of at least the magnitude of the plasmon-induced losses. The thicknesses of
20% to 50%, while exhibiting good linearity. Furthermore,
humidity-induced index changes to Nafion occur rapidly and the TiOz and upper SiOz layers control the resonance wavelength
appear to be fully reversible. of the device. Additionally, since the fragile gold layer is not in
direct contact with the surrounding environment, this configura-
tion offers a degree of ruggedness seldom found in SP sensors.
Introduction: Humidity sensors have been studied in a number of Further details of the device are reported elsewhere [7].
forms for many years. Electronic humidity sensors are well estab-
lished, but suffer from electromagnetic interference (EMI). Optical
sensors offer immunity to EM1 and have been explored using a Results and discussion: The output of a monochromator
variety of detection schemes, including humidity-induced changes (Digkrom 240) was fed through a chopper (Rolfin-Sinar) into a
in fluorescence [l], absorption [2]and refractive index [3, 41. In the multimode optical fibre. The fibre was then butt-coupled directly
first two cases, the linearity of the device response tends to be to the SP waveguide. The output signal was passed through a
poor, while in the latter case, the index change is rather small, in Glan-Thompson prism polariser to resolve the individual polarisa-
the order of 1 x l t 3 .Although index changes on this scale can be tion components and ultimately detected with a silicon photodi-
measured interferometrically, an alternative, and perhaps more ode. A lock-in amplifier was used to improve the signalhoise
robust, approach is to use a surface plasmon (SP) waveguide. In ratio.
this Letter we examine the performance of such a device, created
by coating an SP waveguide with a thin layer of a polymer whose
refractive index is moisture-sensitive.
An integrated optic (IO) SP waveguide consists of a dielectric
waveguide overlaid with a thin layer of metal and functions as a
generic refractive index sensor [5 - 71. Using the coupled mode
formalism, resonance occurs when the propagation constant of an
uncoupled TM-polarised waveguide mode matches that of an SP
mode in the metal f h and the two waves couple to form a lossy
normal mode. When this phase condition is not satisfied, propaga-
tion loss is considerably lower. SP excitation in these devices is
thus strongly polarisation- and wavelength-dependent. Changes in
the refractive index of the superstrate region alter the resonance
wavelength by producing unequal changes in the propagation con-
stants of the uncoupled waveguide and SP modes. TE-polarised
waveguide modes do not interact with the surface plasmons and
experience a relatively small, wavelength-independent loss due to
the presence of the metal layer.
The response of the 10 SP waveguide can be characterised in 1.30 1.34 1-38 1 42
terms of the polarisation extinction ratio PER), defmed at a par- wperstrate refractive index
ticular wavelength as [5] Fig. 2 Theoretically predicted and experimentally measured polarisation
extinction ratio against superstrate refractive index f o r excitation wave-
l e n d s o f 658 and 708nm
where are the propagation losses Of the TE and TM modes Theoretlcal curves have been scaled to be a factor of 10 smaller for
in dBicm. The losses are related to the normal mode propagation comnarlson DUrDoSes
constants as 0 638nm. meaiured. n 708nm. measured
658 nm, predicled (+ 10)
AT",TE = -1Olog{eXp(-2~,T",TEs)}/Z (2) ~ _ _ 708nm,
_ predicted (+ 10)
where k, = (27dh,) NE,h, is the vacuum wavelength, z is the device
length and N, is the imaginary part of the normal mode index. For To calibrate the SP waveguide, the polarisation extinction ratio
singlemodewaveguides, the PER varies linearly with device length. was measured at 658nm and 708nm as a function of superstrate
By exciting SP waveguides with circularly polarised light, the TE refractive index, as shown in Fig. 2, using Cargille index oils. For
signal can be used as an internal reference for signal normalisation each excitation wavelength, a unique value of superstrate refrac-
since its loss is relatively independent of the excitation wavelength. tive index was found which maximised the magnitude of the PER.
A transfer matrix method is used in conjunction with a A sensitivity, or minimum detectable change in refractive index, of
damped-Newton-Raphson algorithm to iteratively compute the -5 x 1 t 5had been predicted for this device, at a signalhoke ratio
complex propagation constants and field distributions for the nor- of -13dB [7].However, experimentally measured PER values were
mal modes of the SP waveguide. Eqns. 1 and 2 are used to calcu- found to be roughly an order of magnitude less than those pre-
late PER values. dicted by OUI model, most likely due to scattering caused by
842 ELECTRONICS LETTERS 25th April 1996 Vol. 32 No. 9

Authorized licensed use limited to: UNIVERSIDADE DO PORTO. Downloaded on June 15,2010 at 14:07:29 UTC from IEEE Xplore. Restrictions apply.
imperfections in the end-facet polish and grain boundary-related Acknowledgments: This work was supported in part 6y the
roughness in the metal layer. Because of this, we are only able to National Science Foundation under grant DMI-9361889 awarded
resolve index variations of 5 x 1v4 with the current device. In to the American Research Corporation of Virginia. The govern-
addition, the measured PER values peak at lower superstrate indi- ment has certain rights in these data. Support was also received
ces than predicted, which indicates that either one or both of the from the Microfabritech program at the University of Florida.
tuning layers may be slightly thicker than anticipated or that the
refractive index of the gold layer differs somewhat from the model 0 IEE 1996 17 Febvuuvy 1996
data. From Fig. 2, it is evident that the actual sensitivity of this Electronics L e t t m Online No: I9960520
device to refractive index variations depends on both the excita- M.N. Weiss and R. Srivastava (Department of Electrical and Computer
tion wavelength and the superstrate index. To uniquely determine Engineering, Lursen Hull, University of Florida, PO Box 116200,
the actual refractive index of the superstrate media, measurements Gainesville, FL 32611-6200, USA)
of the PER at two wavelengths are needed. H. Groger (American Research Corporation of Virginia, 1509 4th
Street, PO Box 3406, Radford, VA 24143-3406, USA)

References
E -4 .o
.
m
1 SADAOKA, Y., MATSUGUCHI, M., SAKAI, Y.,and MURATA, Y . : ‘Optical
humidity sensing characteristics of composite thin films of
x
._
5 -5.0 2
hydrolyzed nation-dye with a terminal N-phenyl group’, J. Mater.
Sci., 1992, 27, pp. 5095-5100
BOLTINGHOUSE, E., and ABEL, K : ‘Development of an optical
relative humidity sensor. Cobalt chloride optical absorbency sensor
study’, Anal. Chem., 1989, 61, (17), pp. 1863-1866
3 PINCENTI, J.c.,and NAYLOR, D.L.: ‘Humidity dependence of the
birefringence in poly(methy1 methacrylate) waveguides’, Appl. Opt.,
C 1994, 33, (6), pp. 1090-1094
.- 4 FRANKE, H., WAGNER, D., KLECKERS, T., REUTER, R.,
.g -7. 0
I

ROHITKUMAR, H.v., and BLECH, B.A.: ‘Measuring humidity with


-0 planar polyimide lightguides’, Appl. Opt., 1993, 32, (16), pp. 2927-
Q
0 2935
5 SLETTEN, M.A...and SESHARDI. S.R.: ‘ExDerimental investigation Of a
>.
thin-film surface polariton polarizer’, Appl. Phys., lG1, 70, (2),
pp. 57LL579
20 25 30 35 40 45 50 ~~

relative humidity ,% Lo213) 6 LAVERS, c.R., HARRIS, R.D., HAO, s., WILKINSON, J.s., O’DWYER, K.o.,
Fig. 3 Humidit.y response of surface plasmon waveguide when coated BRUST, M., and SCHIFFRIN, D.J.: ‘Electrochemically-controlled
with thin layer of Nafion fluoropolyrner waveguide-coupled surface plasmon sensing’, J. Electroanal. Chenz.,
1995, 387, pp. 11-22
0 658nm excitation wavelength 7 WEBS, M.N., SRIVASTAVA, R., GROGER, H., LO, P., and LUO, s.: ‘A
0708nm excitation wavelength theoretical investigation of environmental monitoring using surface
plasmon resonance waveguide sensors’, to be published in Sens.
Actuators A, 1996
To use the SP waveguide as a humidity sensor, it is necessary to 8 GROT, w.G.:‘Perfluorinated ion exchange polymers and their use in
coat the device with a transducing layer whose refractive index is research and industry’, Macrornol. Symp., 1994, 82, pp. 175-184
humidity-dependent. For this purpose we have used Nafion fluor-
opolymer, which swells in the presence of moisture [8]. A few
drops of Nafion fluoropolymer (Aldrich, 1% polymer solution in
alcohol) were deposited onto the surface of the SP waveguide. The
solution dried to form a film on the order of 5 p thick, covering
the entire surface of the device. Variations in the thickness of the SNR improvement in silica-based waveguide
Nafion layer do not significantly affect device performance, since Rayleigh backscattering measurement
the film thickness is always greater than the penetration depth of using a complex optical low coherence
the evanescent tail of the plasmon into the polymer [7]. The reflectometer
humidity-induced variation in the PER of the Nafion-coated SP
waveguide is shown in Fig. 3 over a range of 20% to 50% relative K. Takada and H. Yamada
humidity. Over this range, the sensor exhibits a reasonably linear
response, changing by 0.030dB/%RHcm for 658nm excitation and
-0.073dB/%RHcm for 708nm excitation. Humidity-dependent
Indexing terms: ReJectorneters, Optical waveguides
changes in the index of Nafion occur very quickly, in the order of
tens of seconds, and appear to be fully reversible. No attempt was The authors report a signal-to-noise ratio (SNR) improvement in
made to control the temperature, which varied from 22°C to 26°C the Rayleigh backscattering measurement of a silica-based
over the course of these measurements. Comparing Fig. 2 and Fig. waveguide over 20~x1,achieved by constructing a complex optical
3, we find that the refractive index of Nafion changes from low coherence reflectometer with an auxiliary interferometer. The
1.346oirO.0005 at 20% relative humidity to 1.358M.002 at 50% rel- best SNR achieved is 38, which corresponds to signal fluctuations
ative humidity. This is an order of magnitude larger than humid- of H.ldB, and the spatial resolution is 1.3cm. The measured
ity-induced refractive index changes in other polymeric materials, Rayleigh backscattering distribution clearly revealed the
waveguide loss.
such as polyimide [4].
Introduction: Coherent fading or speckle-like noise appears when
Summary: Nafion fluoropolymer has been used as a transducing the Rayleigh backscattering from silica-based waveguides is meas-
layer on a surface plasmon waveguide to allow measurement of ured with an optical low coherence reflectometer (OLCR). The
atmospheric humidity. The sensor responds rapidly and reversibly noise is reduced by averaging the signals that are obtained using
to changes in humidity and exhibits a relatively linear change in narrow band lights with different central wavelengths emitted
polarisation extinction ratio for relative humidities between 20% from a tunable narrow band source [I]. Although this method can
and 500/. Experimentally measured data agree reasonably well rapidly complete one averaging process at each waveguide point,
with our theoretical model. Through improvements in the fabrica- the signal-to-noise ratio (SNR) achieved is at most 4,owing to
tion process, namely in the characterisation of the constituent thin the finite spectral width of the source light.
films, it should be possible to optimise the sensitivity of the device The complex OLCR [2] can also perform signal averaging. This
at an operational wavelength where excitation by commercially uses the whole interference signal for a test waveguide. Signal
available red laser diodes is possible. processing enables us to generate signals obtained for narrow

ELECTRONICS LETTERS 25th April 1996 Vol. 32 No. 9 843

Authorized licensed use limited to: UNIVERSIDADE DO PORTO. Downloaded on June 15,2010 at 14:07:29 UTC from IEEE Xplore. Restrictions apply.

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