Sensors and Actuators B 146 (2010) 331336

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Sensors and Actuators B: Chemical

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Optical sensing of ammonia using ZnO nanostructure grown on a

side-polished optical-ber
A.Og. Dikovska a, , G.B. Atanasova b , N.N. Nedyalkov a , P.K. Stefanov b , P.A. Atanasov a ,
E.I. Karakoleva c , A.Ts. Andreev c
a
b
c

Institute of Electronics, Bulgarian Academy of Sciences, 72 Tsarigradsko Chaussee, Soa 1784, Bulgaria
Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bonchev str., bld. 11, 1113 Soa, Bulgaria
Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tsarigradsko Chaussee, 1784 Soa, Bulgaria

a r t i c l e

i n f o

Article history:
Received 7 December 2009
Received in revised form 3 February 2010
Accepted 4 February 2010
Available online 11 February 2010
Keywords:
Optical gas sensors
ZnO nanostructures
Distributed coupler
PLD

a b s t r a c t
In this work, thin ZnO lms were produced by pulsed laser deposition on a side-polished single-mode
ber in view of optical gas sensor applications. The experimental conditions used for preparation of the
samples were chosen so as to obtain smooth, porous and nanostructured lms. The inuence of the
lm structure on the sensitivity to ammonia was investigated. For all samples, a shift of the spectral
position of the resonance minimum to the longer wavelengths was observed under gas exposure at room
temperature. The nanostructured sensor element demonstrated a substantially higher sensitivity due to
its structure compared to the only smooth and porous samples.
2010 Elsevier B.V. All rights reserved.

1. Introduction
Gas sensors based on optical detection have focused signicant
attention due to the possibility to operate at room temperature, to
measure low gas concentrations with fast response time and to be
applicable even in explosive and/or electromagnetic environments.
The optical gas sensing by metal oxide thin lms utilize mainly the
properties of planar optical waveguides formed by these lms. The
optical detection is based on the refractive index changes of the thin
lms caused by the gas components of the reacting medium. The
measurements of the changes of the planar waveguide parameters
can be carried out using standard integrated optic measurement
techniques [1,2] or with an application of ber-optic distributed
couplers consisting of a side-polished ber coupled with the planar waveguide investigated [3]. At present, the main efforts are
focused on decreasing the minimum gas concentration necessary
for optical detection. One possibility for improving the gas sensitivity is to make use of the advantages offered by nanotechnologies,
in particular, the use of nanostructured planar waveguides. A high
surface-to-bulk ratio in metal oxide nanostructures allows very
sensitive transduction of the gas/surface interactions into a change
in the electrical, optical or other properties [4,5]. In addition,
the possibility to form a variety of morphologies and structures

Corresponding author. Tel.: +359 2 979 59 11; fax: +359 2 975 32 01.
E-mail address: dikovska@ie.bas.bg (A.Og. Dikovska).
0925-4005/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2010.02.018

offers many opportunities of tuning the gas sensing properties

[68].
Among the various sintering methods, pulsed laser deposition
(PLD) has been proven to be a simple and effective catalystfree method for preparation of nano-scale materials [912]. The
main advantage of PLD is its ability to create high energy species
which exhibit high reactivity and surface mobility when reaching the substrate. Several studies have been reported dealing with
ZnO nanostructures growth by PLD and exploring a wide range
of experimental parameters, such as choice of substrate, substrate temperature, background oxygen pressure, etc. [10,12,13].
For technological application, however, it is essential to develop
a methodology for nanostructure fabrication which can be easily
transferred and applied to real devices.
In the present study, we attempted to synthesize nanostructured ZnO planar waveguide by pulsed laser deposition; to fabricate
a simple and efcient sensor element consisting of a side-polished
single-mode ber and a nanostructured ZnO planar waveguide; and
to test the gas sensing performance of the sensor element under
ammonia gas exposure at room temperature.
2. Principle of sensor element operation
The distributed coupling between a side-polished single-mode
ber and a planar waveguide is an efcient method for constructing sensor elements utilizing the sensor properties of planar
optical waveguides. These sensors are an attractive addition to

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were deposited on the side-polished ber in an on-axis PLD conguration. The substrate temperature was kept at 300 C during
deposition. The second step consisted in deposition of ZnO on the
as-created nuclei in an off-axis PLD conguration. In the off-axis
deposition, the substrate repositioned away from the normal position in the PLD method at a distance of 1.5 cm. The laser uence
used was 3.5 J/cm2 . During the second step the substrate temperature and the oxygen pressure were kept constant at 300 C and 5 Pa,
respectively.
3.2. Characterization of the samples
The surface morphology of the as-deposited samples was characterized by atomic force microscopy (AFM). The morphology of
the nanostructured sample was analyzed using high-resolution
scanning electron microscopy (HR-SEM) Sirion-FEI. The surface
composition and chemical state of the ZnO waveguiding lms
were investigated by X-ray photoelectron spectroscopy (XPS). The
measurements were performed on a VG ESCALAB II electron spectrometer using MgK radiation with energy of 1253.6 eV. The
binding energies (BE) were determined with an accuracy of 0.1 eV
utilizing the C 1s line at 285.0 eV (from an adventitious carbon) as
a reference.
Fig. 1. (a) A schematic view and (b) cross-section of the side-polished ber sensor
element.

the standard integrated optic elementsprism and grating couplers, because of their inherent in-line ber-optic construction.
A schematic view of the sensor element is presented in Fig. 1a.
A single-mode ber is glued into a fused silica rectangular block
inside a convex groove. The optical cladding of the ber is mechanically ground and polished to about 1 m of minimal residual
cladding thickness to the ber core. The planar waveguide is
grown on the at polished ber surface so that a distributed
evanescent wave coupling between the ber and the planar waveguide is implemented. The mechanism of interaction between a
side-polished single-mode ber evanescently coupled to a planar
waveguide has been already well described [14,15]. Light coupling
takes place under the condition of waveguide resonance between
the ber mode and the corresponding planar waveguide mode,
leading to the appearance of a channel-dropping lter in the spectral transmittance of the ber [16,17]. The spectral position of the
dropping lter is strongly sensitive to the parameters of the planar
waveguide (thickness, refractive index of the lm, refractive index
of the superstrate) forming in this way the basis for sensor applications. Sensor elements consisting of a side-polished ber coupled
to a planar waveguide have been used for registration of different
physical and chemical parameters [1822].
3. Experimental
3.1. ZnO planar waveguide deposition
Thin ZnO lms were grown by PLD on the side-polished ber.
A XeCl excimer laser ( = 308 nm,  = 30 ns full width at half maximum (FWHM), and rep rate of 2 Hz) at a uence of 2 J/cm2 was used
for ablation of the ZnO ceramic target. The target to substrate distance was xed at 40 mm in a standard on-axis conguration. The
lms were grown at substrate temperatures of 300 C. All experiments were performed in oxygen atmosphere. Smooth lms were
prepared at oxygen pressure of 5 Pa and porous lms at 20 Pa.
The nanostructured ZnO waveguides were fabricated via a two
step process. As the rst step, a ZnO lm was prepared at oxygen pressure of 20 Pa in order to form growth nuclei. These nuclei

3.3. Fabrication of the side-polished ber

An isotropic single-mode ber (SM800-5.6-125; Fibercore) was
used. The cross-section of the side-polished ber is presented in
Fig. 1b. The ber was glued into a fused silica block with dimensions
of 3 mm 6 mm 15 mm inside a convex groove. The radius of curvature at the groove bottom was 125 mm. Such a small radius was
chosen in order to obtain a short interaction length between the
optical-ber and the planar waveguide (approximately 1 mm). A
high temperature optical epoxy (Epo-Tek 354) was used for embedding the ber into the silica block.
The optical set-up for in situ control of the lm thickness during
the deposition process was already reported in [3]. The set-up for
in situ control allowed us to convert the increase of the oxide lm
thickness during the deposition process into a time-dependence
of the output ber intensity. The deposition of the oxide lm was
stopped at the second minimum which corresponds to the interaction with the TM0 mode of the planar waveguide. The interaction
with the TM0 mode was chosen for two reasons: (i) to reduce the
time of lm deposition and (ii) this interaction is more sensitive
in comparison with the TE1 mode previously used in similar measurements [23].
The measurements of the spectral transmittance of the ber
samples were carried out using a halogen lamp as a light source
and a monochromator. The light from the monochromator output
was polarized by a Glan prism and then focused into the ber by
a microscope objective. The output signal from the ber was measured by a lock-in-amplier (SR 510, Stanford Research Systems).
The spectral shapes of the receiving channel-dropping lters are
presented in Fig. 2. The FWHM of the channel-dropping lters was
evaluated to be approximately 25, 30 and 40 nm for smooth, porous
and nanostructured lms, respectively.
The optical set-up for measuring the sensitivity to gaseous
ammonia is presented in Fig. 3. The light source was a broadband superluminescent light emitting diode (SLD). The light from
the SLD passed through a ber polarizer and a ber polarization
controller for accurate polarization adjustment of the channeldropping lter. The output ber was connected to the entrance of
a 0.2 m monochromator (Photon Technology International, Model
101, grating 600 l/mm, 1000 nm blazed). The ber core served as
an entrance slit, the exit slit was adjusted to ensure 1 nm spectral resolution. The intensity of the passing light was measured by

A.Og. Dikovska et al. / Sensors and Actuators B 146 (2010) 331336

Fig. 2. Spectral dependence of the output signal from the sensor element with
deposited: (a) smooth, (b) porous and (c) nanostructured ZnO lm and interaction
with the planar waveguide TM0 mode.

a large area silicon photodiode (PD) (Siemens BPW 34) mounted

on the monochromator exit. The photodiode signal was registered
by a lock-in amplier. The monochromator grating was turned so
that the intensity in the middle of the long wavelength slope of
the channel-dropping lter could be measured. The measurements
were carried out in a home-made vacuum chamber equipped with
needle valves. The ammonia vapors were produced by evaporation
of 0.2 ml water solution of 2.5, 5, 10 and 25% NH3 in a container with
volume of 0.01 m3 . Ammonia concentrations of approximately 500,
1000, 2000 and 5 000 ppm were thus obtained. The vacuum chamber allows the reactive gas from the gas container to ll the test
chamber, keeping the pressure at atmospheric value. All experiments were carried out at room temperature. The gas sensor tests
were performed several times in order to check the reproducibility
of the response.
4. Results and discussion
4.1. Surface morphology of the sensor element
Our previous investigations showed that ZnO lms prepared at
5 Pa oxygen pressure have smooth surface with root mean square
(RMS) value of a few nanometers [24]. This is why in the present
work these lms are referred to as smooth lms.
As it is well known, raising the oxygen pressure enhances the
porosity of the surface and increases the RMS value [25]. The
lms prepared at a higher oxygen pressure, 20 Pa, exhibit a rough
surface with a high peak-to-valley ratio [24]. The lms prepared

333

Fig. 4. AFM image of the porous ZnO planar waveguide taken from an area
800 nm 800 nm.

under these experimental conditions in our work are referred to as

porous lms. An AFM image of a porous ZnO lm is presented in
Fig. 4.
The surface morphology is a very important parameter for formation of nanostructures. The rough surface plays the role of nuclei
for nanostructured lms growth [26]. Therefore, our rst step of
nanostructure preparation was formation of a thin ZnO lm with a
clearly expressed rough surface. A lm with thickness lower than
30 nm was deposited at the same experimental conditions as the
porous lm in order to create the growth nuclei (see Fig. 4). In the
second step, ZnO was deposited on the as-created nuclei. The ZnO
growth follows the nuclei during the off-axis deposition and then a
nanostructured lm is formed. Fig. 5 shows the HR-SEM image of a
nanostrucured ZnO lm. The top view of the sample shows uniform
and densely packed nanostructures with average diameter in the
range of 4070 nm.
The chemical composition of the surface is of essential importance for gas sensor elements performance. Thus, the surface
composition of the samples was investigated by XPS. The XPS spectra of porous and nanostructured ZnO are presented in Fig. 6. For
both samples, the Zn 2p3/2 peak is characterized by a binding energy
of 1021.5 eV, which is typical for zinc in ZnO (see Fig. 6a). A mod Zn = BE Zn 2p + KE Zn LMM) was used to
ied Auger parameter (
investigate the changes in the chemical environment of the Zn
and O ions in the samples. The modied Auger parameter shows
similar values (2010.6 and 2010.7 eV) for both samples which indicates that the chemical surrounding of Zn2+ ions is practically

Fig. 3. Optical set-up for measurement of the NH3 inuence.

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A.Og. Dikovska et al. / Sensors and Actuators B 146 (2010) 331336

Fig. 5. 45 HR-SEM view of the nanostructured ZnO lm.

identical. Similar results were obtained for the smooth waveguide

lm.
The O 1s peaks of both samples are wide and asymmetric, as
it is clearly seen in Fig. 6b. The O 1s peak was deconvoluted by a
LorentzianGaussian curve tting into two components at 530.1
and 531.8 eV, respectively [27]. They are attributed to O2 ions in
the ZnO lattice and to oxygen bound in OH groups, respectively.
A signicant difference was found in the values of the OOH /O2
intensity ratio for the nanostructured sample (0.89), and for the
porous one (0.41). This can be attributed to the higher specic surface area of nanostructured ZnO as compared to the porous sample
resulting in the adsorption of a larger amount of OH on its surface.
4.2. Ammonia gas sensing results
For all the three samples, a shift of the spectral position of the
resonance minima to the longer wavelengths was observed after

Fig. 7. Typical response of the nanostructured ZnO sensor element to various ammonia gas concentrations: (a) 500 ppm, (b) 1000 ppm, (c) 2000 ppm and (d) 5000 ppm.

exposure to ammonia vapors. Fig. 7 presents the changes in the

intensity of the ber output power as a result of ammonia exposure
for the sample with a nanostructured waveguide lm. A relatively
fast response was observed in the range of 2030 s for the higher
gas concentration. The time for gas reaction slightly increased as the
concentration was decreased (500 ppm). The time of the full signal
restoration after opening the test chamber to the atmospheric air
was measured to be about 20 min for the samples with smooth and
porous lms and about 3035 min for the sample with a nanostructured lm. For the latter, sample uctuations in the intensity
during the restoration process were typical. We relate this observation with the fact that no air ow was applied around the samples so
that back absorption of ammonia molecules was possible. Because
of the different slopes of the samples curves, a transformation

Fig. 6. XPS of the: (a) Zn 2p and (b) O 1s core level on the surface of the: (1) porous and (2) nanostructured ZnO planar waveguides.

A.Og. Dikovska et al. / Sensors and Actuators B 146 (2010) 331336

335

were studied experimentally under exposure to ammonia. The

nanostructured waveguide demonstrated a substantially higher
sensitivity, which allows us to predict a low concentration limit
of 50 ppm for NH3 in air.
Acknowledgment
This work was supported in part by the Bulgarian Ministry of
Education and Science under Contract DO 02-293/08.

References

Fig. 8. Wavelength shifts of the smooth, porous and nanostructured ZnO sensor
elements in dependence of the ammonia concentration.

of the intensity changes to the corresponding wavelength shifts

was performed to enable a comparison of the samples sensitivities.
The results are presented in Fig. 8. The nanostructured waveguide demonstrated substantially higher sensitivity, conrming the
assumptions that the physical absorption is the main gas sensing
mechanism. Using the data in Fig. 8, a calculation of the refractive
index changes of the waveguiding lms was performed. For example, for the highest concentration (5000 ppm) these changes are
0.81 103 , 2.14 103 and 6.35 103 for the smooth, porous and
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mechanism. The nanostructured thin lm provides a larger gas
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The optical set-up used permits us to register intensity changes
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With such resolution, the sensitivity reported here would yield a
low concentration limit of approximately 50 ppm for NH3 in air.
5. Conclusions
A simple and effective sensor element was fabricated consisting of a side-polished single-mode ber and a PLD ZnO planar
waveguide. The sensor element operation principle is based on a
distributed coupling between the ber mode and the corresponding mode of the metal oxide planar waveguide. The change of the
spectral behavior of the as-obtained channel-dropping lter under
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Biographies
Anna Og. Dikovska graduated in 1996 from the Faculty of Physics of St. Kliment
Ohridski University of Soa with M.S. degree in Engineering Physics, and received
in 1997 a Ph.D. degree in Physics of Wave Processes at the Institute of Electronics, Bulgarian Academy of Sciences. Her eld of research is pulsed laser deposition
of oxide materials for optical applications. She is currently involved in the development of nanostructured thin lms. She has authored more than 25 papers and
communications.

Plamen K. Stefanov is a Senior Research Associate and Head of the Laboratory of

Electron Spectroscopy at the Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences. His research interests include gas sensors and thin lm
catalysts for environmental applications.
Petar A. Atanasov is a Corresponding Member of the Bulgarian Academy of Sciences,
Full Professor and Head of the Gas Lasers and Laser Technologies Laboratory at the
Institute of Electronics, Bulgarian Academy of Sciences, Soa, Bulgaria. He graduated
in Physics from the Faculty of Physics of the University of Soa in 1967, and received
Ph.D. degree in 1977 and Dr. Sc degree in 1990 at the Institute of Electronics. He
was Visiting Professor several times at Keio University, Chiba University, Japan, and
Instituto de Optica, CSIC, Madrid. His scientic and application activities are in the
eld of micro- and nano-photonics, optoelectronics. He is author or co-author of
more than 280 contributions.

Genoveva B. Atanasova graduated in 1996 from the Faculty of Physics, St. Kliment
Ohridski University of Soa with M.S. degree in Engineer Physics, got qualication
Quantum Electronics and Lasers Techniques and Measurement Electronics. She
has been Research Scientist in the Laboratory of Electron Spectroscopy, Institute of
General and Inorganic Chemistry, Bulgarian Academy of Sciences, since 2000.

Elka I. Karakoleva received in 1978 the B.S. degree from the Faculty of Physics
of the University of Soa. In 1979 she joined the Department of Nuclear Reactor
Physics at the Institute of Nuclear Physics and Nuclear Energy of the Bulgarian
Academy of Sciences, Soa. Since 1990 she has been working as a Research Associate
at the Department of Optics and Spectroscopy, Institute of Solid State Physics of the
Bulgarian Academy of Sciences, Soa. Her current interests are in the eld of the
development of ber-optics elements and the optical waveguide modeling.

Nikolay N. Nedyalkov received in 1998 M.S. degree in Quantum Electronics at the

Faculty of Physics of St. Kliment Ohridski University of Soa. He obtained Ph.D.
degree in Physics of Wave Processes in 2005 in the Institute of Electronics, Bulgarian Academy of Sciences. His research topics include lasermatter interaction,
plasmonics, optical properties of metal nanoparticles, ultrashort laser nanostructuring. N. Nedyalkov holds a permanent position as a Senior Research Associate at
the Institute of Electronics, Bulgarian Academy of Sciences.

Andrey Ts. Andreev graduated in 1975 from the Faculty of Physics of St. Kliment
Ohridski University of Soa. He received his Ph.D. degree in the Lebedev Institute of
Physics, Russian Academy of Sciences, Moscow, in 1981, in the eld of optical-ber
loss measurements. Since 1981 he has been working as a Research Associate and
Senior Research Associate (1994) in the Department of Optics and Spectroscopy
at the Institute of Solid State Physics, Bulgarian Academy of Sciences. His current
interests are in the eld of ber-optics components and sensors.