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Sensors and Actuators B 145 (2010) 265–271

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Sensors and Actuators B: Chemical


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

Characterization of a fiber optic liquid refractive index sensor


Arunava Mukherjee a , Debanjan Munsi a , Vishal Saxena b , Ramaswarup Rajput a , Paramhans Tewari b ,
Vandana Singh a , Anjan Kumar Ghosh b , Joseph John b , Harshwardhan Wanare a , Pinaki Gupta-Bhaya c,∗
a
Department of Physics, Indian Institute of Technology Kanpur, Kanpur 208016, India
b
Department of Electrical Engineering, Indian Institute of Technology Kanpur, Kanpur 208016, India
c
Department of Chemistry, Indian Institute of Technology Kanpur, Kanpur 208016, India

a r t i c l e i n f o a b s t r a c t

Article history: The intensity of light signal transmitted through an optical fiber, whose cladding over a finite length is
Received 31 July 2009 removed, is used as a sensor of refractive index of liquids, in which the fiber is immersed. The transmitted
Received in revised form light intensity is measured as a function of liquid refractive index for different lengths of the unclad
28 November 2009
section of the fiber and at each unclad length its sensitivity to change in refractive index of liquid is
Accepted 4 December 2009
monitored. The liquid refractive index studied ranges from below the refractive index of the cladding
Available online 16 December 2009
to above that of the core. A plot of normalized light intensity as a function of liquid refractive index
for a short unclad length shows a local maximum at a liquid refractive index equal to the refractive
Keywords:
Liquid refractive index sensor
index of the fiber core. This maximum becomes less prominent as length of unclad region increases and
Fiber optic refractive index sensor finally disappears. These observations are interpreted in terms of frustrated total internal reflection of
Frustrated total internal reflection light rays. Sensitivity to refractive index differential, of the sensor response, increases with increase in
FTIR refractive index of the liquid pair, below that of the fiber core. In this range of refractive index, we observe
a maximum in this sensitivity at an intermediate unclad length of the fiber. When liquid refractive index
equals core refractive index, at the rising edge of the local maximum observed in sensors of shorter unclad
length, the sensitivity maximum disappears. The sensitivity to refractive index differential diminishes
as liquid refractive index exceeds fiber core refractive index. Measurements have been performed with
five different unclad sensor lengths and a core diameter of 400 and 800 ␮m. The results for the two core
diameters show similar qualitative features.
© 2009 Elsevier B.V. All rights reserved.

1. Introduction teristic of a partially unclad fiber as a liquid RI sensor [23]. In this


paper we observe that RI sensitivity of this sensor is dependent
Fiber-based refractive index (RI) sensors have been widely used. on the cladding thickness that remains after the fiber is partially
They can be very compact in size, need only a small sample volume, uncladded over a fixed length and is maximum at an intermediate
can be used in remote sensing, for liquids or polymer composites unclad length. The role of cladding in RI sensing is further explicitly
and can be adapted as chemical sensors. Optical fiber has been used demonstrated in experiments using a mode scrambler. A few other
as a sensor of absorption [1–4]. Metal-coated fibers using surface reports also refer to the significance of the cladding of a fiber in the
plasmon resonance [5,6] and in-fiber Bragg grating (FBG) [7,8] have context of its use as a sensor [24–30].
been used as highly sensitive RI sensing devices. Tapering of fiber Brown et al. [31] in an interesting experiment use two fibers
and stripping of the fiber cladding have been used to make opti- which are perfectly aligned with an intervening liquid medium,
cal fiber a sensitive sensor of RI [9–13]. Untapered, fully clad fibers through which light passes from one fiber to another and whose
with thin films deposited on them have been used as RI sensors refractive index it senses. Theoretical analysis using Fresnel equa-
[14,15]. A fiber stripped of cladding has been layered with adsor- tion is given and a non-monotonic dependence of light intensity
bent material deposited by sol–gel technique to make it a sensor incident in the second fiber on the distance separating the two
of chemicals that get adsorbed on the adsorbent layer and modify fiber fragments is predicted in one model. Our experiments are
its RI [16–22]. We have reported in a detailed paper the charac- inspired by Brown’s work. We however modify Brown’s experi-
mental set-up by keeping the unconnected fiber segments of Brown
connected by the unclad fiber core, vary the length of the unclad
∗ Corresponding author. Tel.: +91 945 2959798; fax: +91 512 2598337. region and investigate dependence of RI sensitivity on unclad
E-mail address: pinaki@iitk.ac.in (P. Gupta-Bhaya). length.

0925-4005/$ – see front matter © 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2009.12.009
266 A. Mukherjee et al. / Sensors and Actuators B 145 (2010) 265–271

Fig. 1. Schematic experimental arrangement.

2. Methods a result a magnification of 10 is used. The ratio of the diameter of


the fully clad fiber whose thickness is manufacturer specified and
2.1. Measurement system the unclad fiber is used to calculate the degree of uncladding. The
uncertainty in manufacture specified fiber diameters (Section 2.2)
The experimental set-up is shown in Fig. 1. A laser beam is the maximum uncertainty over large fiber lengths. Our expe-
( = 633 nm) from Melles-Griot (25LHP-213230) Helium Neon rience is that this uncertainty over small fiber lengths does not
Laser is chopped by a Stanford Research System (SR540) optical significantly increase the uncertainty in the unclad fiber diameter.
chopper. The chopped light beam falls on a beam splitter (Melles The fiber diameter we measure is 400 ␮m and 800 ␮m within error
Griot) which splits the beam into a reference and a sample beam. margin cited above, i.e., all of cladding is etched out by Sulphuric
The two beams emerge in perpendicular directions. The sample acid treatment. We have verified further that the experimental fea-
beam passes through a sensor fiber, with the fiber unclad to dif- tures of interest in this paper remain the same if we expose the
ferent extents, immersed in the fluid of interest. The beam falls fiber to sulphuric acid for 30 h instead of 50 h; the measured fiber
on two separate matched photo-detectors (Hamamatsu) whose diameter is the same within error in both cases. Uncladding to dif-
output currents are converted into proportional voltages. The pho- ferent lengths is achieved using glass tumblers of different lengths
todiode is appropriately biased to minimize noise. The two voltages in which the fiber is exposed to Sulphuric acid. The unclad length of
are then fed into two separate Stanford Research System (SR 830) the fiber is measured by weighing it in a microbalance and using the
Lock-in-Amplifiers. The ratio of their outputs is calculated in a per- manufacturer specified core and cladding density. Unclad length so
sonal computer that is interfaced to the Lock-in-Amplifiers in a determined is within 1 mm of the tumbler length. Schematic dia-
Labview environment. The system is verified to be linear within gram of an optical fiber whose sensing region is stripped of cladding
a certain range of light intensity in which we perform experiments. is given in Fig. 2.
A typical measurement lasts for about 15 min. Total number of data
points over which averaging is done is 20/min. The standard error
of mean, too small to be visible on any of the figures we show and 2.4. Solution preparation
is fractions of a percent in all cases.
In this experiment 15 different liquid media with known RI
2.2. Fiber specification have been used: distilled water, 5%, 12%, 18% and 24% sucrose solu-
tion, 44%, 60%, 76%, 80%, 84%, 88%, 96% (mass of solute divided by
The plastic clad silica fiber (JTLFH) was procured from M/s Poly- mass of solution, expressed as percent) 100% glycerol solution, pure
micro Technologies, USA; Fiber diameter: 430,830, core diameter: dimethyl sulfoxide and pure nitrobenzene. Fewer liquids from this
400, 800 ␮m, maximum error for both diameters: +5, −10 ␮m for list have been used in experiments on 800 ␮m core diameter fiber.
400 ␮m fiber and ±10 ␮m for 800 ␮m fiber. Numerical Aperture RI of aqueous glycerol solutions of intermediate concentration used
(NA): 0.37 ± 0.02. Refractive index of fiber core at 630 nm is 1.457. for finer scanning on RI axis around the maxima we observe was
Refractive index of cladding calculated using core RI and N.A. is calculated by linear interpolation. RI of these liquids is obtained
∼1.40. from CRC Handbook of Chemical and Engineering Data [32]. The RI
data are reported at  = 589 nm.

2.3. Fiber uncladding

Optical fiber is unclad in the sensing region to make it an effec-


tive refractive index sensor. The plastic buffer jacket covering the
fiber is removed by a razor. The plastic clad silica fiber was unclad
by immersing it in 98% concentrated sulfuric acid for ∼50 h so that
no cladding is left behind on the fiber length exposed to sulphuric
acid. The degree of uncladding is monitored by measurement of
its thickness in an optical microscope with digital read-out facil-
ity. An image processing algorithm is used for edge detection. The
thickness is then measured by counting the number of pixels along
the diameter. The counting error is two pixels, one at each end,
resulting in an error of 1.5 ␮m in a 400 ␮m fiber and 3 ␮m in an
800 ␮m fiber. The inhomogeneity of fiber etching along the fiber
length introduces a further imprecision of ∼1% in the mean value
of the diameter. The larger error by a factor of 2 in an 800 ␮m fiber
Fig. 2. Schematic diagram of an optical fiber sensor of refractive index whose
arises from the fact that magnification of 20 used in smaller diam- sensing region is stripped of cladding. Light propagates in X-direction. Cladding is
eter fibers takes the magnified image out of the range of the PC. As stripped in Z-direction.
A. Mukherjee et al. / Sensors and Actuators B 145 (2010) 265–271 267

at higher (6.0 and 8.0 cm) unclad lengths. Fig. 3(b) shows data at
8.0 cm unclad length. In Fig. 4 we show R as a function of liquid
RI for both core diameters in the range where these local maxima
are observed at smaller unclad lengths. The maximum in each case
has been reproduced several times. The maximum is sharper for
an unclad length of 1.5 cm as compared to that of 3.0 and 4.5 cm
for both fiber core diameters. In each of these three maxima for
400 ␮m fiber core, the height of the falling edge of the intensity
ratio profile is 0.11, while those of the rising edge is 0.11 in 1.5 cm
unclad length and ∼0.029 (these numbers are in arbitrary units) in
the other two.
Experimental data on intensity ratio for a given fiber diame-
ter and a given unclad length are verified to be free from possible
differences in fiber alignment that may result from change in test
liquid. The fiber is held rigidly on both ends by stable mechanical
support. The intensity ratio for a given core diameter and different
unclad lengths are made free from possible alignment differences
by adjusting them to same intensity ratio in air. If the core diame-
ter is different then perfectly equivalent alignment in air will also
not give same intensity ratio. The relative locations of the plots for
400 and 800 ␮m core diameter fibers in Fig. 3(a) and (b), therefore
do not have any physical significance and are adjusted merely for
clarity of the figures.
In addition to the presence of the above-mentioned maxima, the
plots for 400 ␮m core diameter fiber (Figs. 3 and 4) show a mini-
mum at a liquid RI equal to core RI and a switchover from negative
to positive slope as the liquid RI exceeds RI of the fiber core. This
feature has been reported by Cusano et al. [15] who use a fully
clad single mode fiber to monitor RI of polymer-based composites
deposited on the fiber. They make measurements with liquid sam-
ples for purposes of calibration. The quantity that monitors the RI of
the liquid is the intensity of reflected light at the liquid–fiber inter-
face. They observe, just as we do, a negative slope in the range of
liquid RI below the fiber RI (∼1.37–1.48) and a positive slope when
RI of test liquid exceeds that of fiber. An earlier report from our
group [23] that used the experimental arrangement described in
this paper, also noted this switchover. That report was less detailed
and the fibers and the process of uncladding were not as well char-
Fig. 3. Plot of intensity ratio (R) as a function of liquid refractive index (RI, n) with acterized.
fibers of two different core diameters (400 and 800 ␮m core radius) of two different
unclad lengths ((a) 1.5 cm and (b) 8.0 cm). Feature to note is the presence of maxima
3.3. Sensitivity maximum at intermediate unclad length
in (a) and its absence in (b).

Fig. 5(a)–(e) shows RI sensitivity (ratio of R and n (n is RI)) as


3. Results and discussions a function of unclad length using a fiber with core diameter 400 ␮m
for five different liquid pairs chosen from different regions of liquid
3.1. Sensor response to RI change refractive indices that we study: Fig. 5(a): liquid pair RI < cladding
RI; Fig. 5(b): liquid pair RI > cladding RI, but considerably smaller
Let Isig denote the output intensity from the unclad fiber than core RI; Fig. 5(c): liquid pair RI ∼ core RI, where the local max-
immersed in the liquid under test and let Iref be the intensity of imum is observed at shorter unclad length, this figure displays data
the reference beam. The experimental indicator of the value of the in the rising edge of the maximum; Fig. 5(d): liquid pair RI ∼ core
RI of the liquid under test is the ratio R = Isig /Iref . RI, this figure is in the falling edge of the maximum; Fig. 5(e): liquid
pair RI > core RI, beyond the minimum in the plot of intensity ratio
3.2. Local maxima and minima in sensor response as a function of liquid RI. The feature of interest in these figures
is (i) presence of a maximum at an intermediate unclad length of
Fig. 3 shows typical experimental data of R as a function of 4.5 cm (Fig. 5(a) and (b)); (ii) disappearance of the maximum in the
liquid RI for two specified unclad length of the sensor fiber with plot with the liquid pair in the rising edge of the local maximum
core diameter 400 and 800 ␮m. The cladding of these fibers was (Fig. 5(c)); (iii) reappearance of a maximum at a higher liquid RI
fully removed by treatment with concentrated sulphuric acid. A (Fig. 5(d) and (e)), where the maximum is less prominent in both
monotonic negative slope, which increases as the liquid RI exceeds figures and its location is shifted to an unclad length of 3.0 cm in
cladding RI (Section 3.4) is observed over a large range of liquid Fig. 5(e). The disappearance of the maximum at an intermediate
RI below core RI in these plots irrespective of unclad length. These unclad length in Fig. 5(c) results from the presence of the local
features have been reported earlier [15,23]. However, a remarkable maximum which is most prominent at the shortest unclad length
new feature is the presence of a local maximum at a liquid RI equal of 1.5 cm.
to core RI (1.457) within error, for smaller unclad lengths (1.5, 3.0 An examination of the numerical values of R/n given on
and 4.5 cm). This feature is present for both core diameters. Fig. 3(a) the y-axis in each of Fig. 5(a)–(e), further shows that RI sensitivity
shows data at 1.5 cm unclad length. This local maximum disappears increases at each of the five unclad lengths in going from Fig. 5(a)
268 A. Mukherjee et al. / Sensors and Actuators B 145 (2010) 265–271

Fig. 4. Plot of intensity ratio (R) with fibers of different unclad lengths (core diameters of the two fibers are 400 and 800 ␮m) as a function of liquid refractive index in the
region where the maxima of interest are observed at smaller unclad length. The value of the unclad length is indicated on each figure. x-Axis of each figure indicates liquid
refractive index. y-Axis indicates intensity ratio in arbitrary units (see text).

and (b) (range on y-axis: 0–0.6 and 3.65–3.85, respectively), further by the effect of frustrated total internal reflection, as discussed
increases in Fig. 5(c) and (d) (range on y-axis: −6 to 10 and 14–20, below. A non-monotonic dependence of transmitted light inten-
respectively) where we are on the two edges of the local maximum sity on liquid RI is then superimposed on the monotonic profile. As
observed for smaller unclad lengths, and then in Fig. 5(e) as we liquid RI exceeds core RI, total internal reflection does not take place
go past the point where nliquid ∼ ncore the sensitivity becomes very and evanescent wave no longer participates in the sensing mech-
small (range on y-axis:1.6–2.0). The absolute values of R are depen- anism. A minimum in transmitted light intensity at nliquid = ncore is
dent on the alignment of the fiber, but, as already stated, we have observed because, then light rays do not sense any optical inhomo-
taken care in correcting for different alignments by adjusting the geneity at the core–liquid interface.
alignment to equalize the intensity ratio to the same value in air. The evanescent waves within the cladding layer associated with
The values of R/n in Fig. 5(a)–(e) are then on equal footing. the guided modes experience two discontinuities: both along the
We have performed experiments, corresponding to those direction of propagation, one at the beginning and the other at
reported above, in our laboratory on fiber sensors whose cladding the end of the unclad region. The evanescent wave entering the
have not been fully removed, but have been unclad to differ- unclad region encounter conditions akin to that in the well known
ent thickness values. The results show a systematic dependence frustrated total internal reflection (FTIR) [33], i.e., propagating
of experimental results on cladding thickness for a given unclad modes in the larger core region (with RI = ncore ) are evanescent
length. The maximum sensitivity at an intermediate unclad length within the thin barrier region (cladding layer with RI = ncladding )
is also observed. These results will be reported in a separate com- followed by an extended region with higher RI (=nliquid ∼ ncore )
munication. where they become propagating modes again. The guided modes
of the fiber tunnel through the barrier and become propagating
3.4. Interpretation of results modes within the liquid-filled unclad region. These new prop-
agating modes re-enter the guiding core region by the reverse
Energy loss from light propagating in a partially cladding- process at the second interface of the unclad region, leading to the
stripped fiber with shorter unclad lengths in the range of unclad enhanced transmission intensity through the fiber. As the unclad
lengths we study show, in the local maxima we observe with region is made longer, fewer propagating modes are able to cou-
nliquid ∼ ncore for shorter unclad lengths, a non-monotonic depen- ple back into the fiber at the second interface. We note that only
dence on liquid RI. The dependence is monotonic at larger unclad around nliquid = ncore the direction of propagation vectors within
lengths, where the local maxima disappear. This is an interesting the core and of the new propagating modes are collinear (as is
experimental result. We are not aware of a similar report in the well known in FTIR geometry) leading to efficient coupling back
literature. into the fiber [33a ]. Hence, light couples back into the fiber most
A monotonic dependence on liquid RI (<core RI) with a more efficiently in the regime where nliquid ∼ ncore . The peak in the plot
rapid rate of energy loss as liquid RI exceeds cladding RI is a result of I/I0 as function of RI that we observe (Figs. 3 and 4) is the
of an increase in the extent of evanescent field in the liquid under result. FTIR has recently been used in the design of a fiber-optic
test. As liquid RI approaches core RI, this increase is accompanied RI sensor. The sensor principle is based on FTIR effect caused by
A. Mukherjee et al. / Sensors and Actuators B 145 (2010) 265–271 269

Fig. 5. Plot of sensitivity of intensity ratio to liquid refractive index change as a function of unclad length of 400 ␮m core diameter fiber for five different liquid pairs with
refractive indices in different RI regions. The liquid pair and their refractive indices are indicated on each figure ((a)–(e)).

refractive index change of a medium surrounding an optical fiber (b), (d), and (e)) owes its origin to the presence of local maxima we
tip [34]. interpret above in terms of FTIR. In Fig. 5(c) R/n (i) is positive at
The deviation of the plot of RI sensitivity as a function of unclad lower unclad lengths for the liquid pair studied (ii) has the largest
length for the liquid pair in the rising part of the local maximum positive value in the shortest unclad fiber length which has the most
(Fig. 5(c)) from the pattern with a maximum at an intermediate prominent maximum (Fig. 4(a) and (f)) and (iii) becomes negative
unclad length we observe for other liquid pairs studied (Fig. 5(a), at larger unclad lengths (Fig. 4(d), (e), (i), and (j)). In the other four
270 A. Mukherjee et al. / Sensors and Actuators B 145 (2010) 265–271

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Biographies Iowa State University, USA; Nanyang Technological University, Singapore. He is a


Professor in EE Department in IIT, Kanpur. Currently he is a Professor in Depart-
ment of ECE, Oklahama University, Tulsa, USA; senior member of IEEE, area: Optical
Arunava Mukherjee obtained his Master’s in Physics from IIT Kanpur (2007) and is Information Processing, Optical Communications, Photonic Sensors, Instrumenta-
now a Graduate Student in Physics at the Tata Institute of Fundamental Research, tion.
Mumbai, India.
Joseph John obtained his B.Sc. in Engineering from College of Engineering
Debanjan Munsi obtained his Master’s in Physics from IIT Kanpur (2008) and is Thiruvanantapuram, University of Kerala. He obtained his M.Tech. in Electrical Engi-
now a Graduate Student in Physics at the Tata Institute of Fundamental Research, neering from IIT Kanpur, Ph.D. degree in Electrical Engineering from Birmingham
Mumbai, India. University, UK. He was a Scholar of the Commonwealth fund. He is currently a
Professor in Electrical Engineering Department, IIT Kanpur; area: Photonics, Instru-
Vishal Saxena obtained B.Tech. (1969) and M.Tech. (1985) degrees in Electrical mentation.
Engineering from IIT Kanpur. He is currently Principal Research Engineer in the
Department of Electrical Engineering, IIT Kanpur; area: Instrumentation. Harshawardhan Wanare obtained his B.Sc. and M.Sc. (Physics) from Sri Sathya Sai
Institute of Higher Learning, Ananthapur, India. He received his Ph.D. in Physics
Ramaswarup Rajput is a member of technical staff in IIT Kanpur. from the University of Hyderabad, India. He worked as a Post-Doctoral Fellow at the
Washington State University, Pullman, USA and the Illinois State University, Normal,
Paramhans Tiwari is a member of technical staff in IIT Kanpur.
USA. He is an Associate Professor in the Department of Physics, Indian Institute of
Vandana Singh has obtained Ph.D. degree in Physics from G.B.P. University of Agri- Technology, Kanpur. Area of Research Interest: Quantum optics, Metamaterials and
culture and Technology, Pantnagar, India. She is Senior Project Scientist from Samtel Imaging in random media.
Center for Display Technology, IIT Kanpur; area: Organic Flexible Printable Electron-
Pinaki Gupta-Bhaya did his Natural Sciences Tripos leading to B.A. (Honors) in Cam-
ics.
bridge University, England (1967). He obtained his M.A. Degree from Cambridge,
Anjan Kumar Ghosh has obtained B.Tech. degree in EE from IIT, Khargpur and MS in Ph.D. in Chemistry from Columbia University, New York (1971), was a Post-Doctoral
EE from SUNY, StonyBrook, USA. He has obtained Ph.D. degree in EE from Carnegie Fellow at the Max Planck Institute für Biophysikalische Chemie, Göttingen, Germany.
Mellon University, USA. He is a member in Technical Staff, Bell Labs, Taught at He is currently a Professor of Chemistry at IIT Kanpur.

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