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Paper-Based ZnO Oxygen Sensor

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DOI: 10.1109/JSEN.2014.2361780

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This article has been accepted for publication in a future issue of this journal, but has not been fully edited. Content may change prior to final publication. Citation information: DOI
10.1109/JSEN.2014.2361780, IEEE Sensors Journal
Sensors-10604-2014 Paper-based ZnO Oxygen Sensor
Paper-basedZnOOxygen Sensor
Alejandro J. Gimenez1, Gabriel Luna-Bárcenas1,*, Isaac C. Sanchez2, and J. Martin Yáñez-Limón1
 and the kinetics of the device [8, 9].
Abstract—In this work we report the development of an
oxygen sensor using a simple device made from a film of ZnO
crystals dispersed over a paper surface. Due to the high porosity
of this kind of device made from paper and ZnO, a large
photoconductive effect is observed as result of the fast absorption
and desorption of oxygen from the ZnO surface. To detect
oxygen we propose to use ultraviolet (UV) illumination over the
photoconductive surface of the sensor, the applied UV light
produces oxygen desorption causing current variations through
the sensor that are proportional to the oxygen presence nearby
the sensor surface. The sensor developed in this work is
attractive because it is remarkably easy to fabricate, employs
only very low cost materials for its construction and shows a
better sensitivity at low concentration of oxygen at partial
vacuum environments.
Index Terms—Gas sensors, paper substrate, UV assisted
sensor, ZnO nanoparticles.
I. INTRODUCTION
Oxygen sensors are important for many purposes, for
example; monitoring air quality for breathing and measuring
air-fuel mix concentration for internal combustion engines,
among many other industrial and scientific applications.
Actually there are several different kinds of oxygen sensors
depending on the specific application, some sensors use
electrochemical cells to obtain a potentiometric or
amperometric signal dependence on the oxygen content[1, 2],
also semiconductive metal oxide sensors are commonly used
to measure O2[3-6]. Metal oxide sensors typically use heated
semiconductive films that change resistivity when exposed to
different oxygen concentrations. The heating is required to
maintain the adsorption-desorption kinetics, thus avoiding
sensor saturation and improving the measurement speed [7].
More recently, UV-assisted semiconductive sensors have been
proposed to use UV illumination to generate electrons at the
semiconductor’s conduction band to enhance the sensitivity
We acknowledge support from Conacyt. We acknowledge characterization
support from Laboratorio de Investigación y Desarrollo Tecnológico de
Recubrimientos Avanzados (LIDTRA). Complementary funding for the
establishment of research and technological development laboratories 2009,
CONACYT (123630).
1
CINVESTAV Querétaro, Libramiento Norponiente no. 2000, Querétaro,
QRO 76230 México.
2
Department of Chemical Engineering, The University of Texas at Austin,
Austin, TX 78712
*Corresponding author (e-mail: gluna@qro.cinvestav.mx)
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1
In the approach proposed in this study, we use a film of
ZnO crystals dispersed over paper as the active part of our
sensor, in previous work we report that ZnO crystals
embedded in paper and cellulose matrices present a large
photoconductive response to UV [10-12]. UV assisted ZnO
oxygen sensors; work on the basis that UV light produces
oxygen desorption, this oxygen desorption is necessary to
induce a desorption-adsorption kinetics which yields a
resultant resistance related to the oxygen presence[8, 9].
Experiments performed by Q. Li et al., and Z. Fan et al.,[13-
15] demonstrate that the large photoconductivity of ZnOnano
particles is due to the process of adsorption and desorption of
atmospheric oxygen. In the previous photoelectrical
experiments performed, it is observed that ZnO devices
normally may take several minutes to reach an desorption-
adsorption equilibrium[10, 16]. This time might be too long
for some sensing applications, for that reason we propose a
method using pulsating UV from a LED source, the LED
pulses produce separated desorption and adsorption signals
that yield faster information making not necessary to wait for
an adsorption-desorption equilibrium of a fixed UV
illumination scheme.
As a substrate for our sensor we use plain bond paper
without any modification, recent studies point out that porosity
and good mechanical and chemical properties of cellulose
make paper a good candidate for many technological
applications such as sensors and actuators [17-21]. A
representation of a paper-based ZnO device is shown in figure
1. In this image we propose the possible mechanism for
oxygen sensing over paper-based surfaces. We propose that
high porosity of cellulose fibers from paper allows gases to
flow easily in and out the sensor improving both the
photoconductivity and sensitivity to oxygen in this kind of
device.
It is worth to notice that as the proposed sensor
device is based on paper this allows the flexibility of the
whole sensor; recently a large effort is performed to develop
flexible electronic devices in order get benefits like ease of
assembly and the implementation of flexible gadgets, such as
folding cell phones[22].
This article has been accepted for publication in a future issue of this journal, but has not been fully edited. Content may change prior to final publication. Citation information: DOI
10.1109/JSEN.2014.2361780, IEEE Sensors Journal
Sensors-10604-2014 Paper-based ZnO Oxygen Sensor
Figure 1.Representation of paper-based O2sensor.ZnO crystals (grey
hexagons) are embedded on a cellulose matrix (yellow rods), electric flow
(green line) percolates through the ZnO crystals as the current varies
depending on the O2concentration and UV stimulus.
II. EXPERIMENTAL
To fabricate the sensing device we use a method described
in previous work[10]. Briefly, this sensor is made by drawing
interdigitated electrodes over paper with a graphite pencil in
the “pencil-on-paper” approach already used by many research
groups [23-26]. Over the interdigitated pencil
electrodes(inside a paper surface of 1cm2),one drop (30µL) of
an aqueous suspension of ZnO crystals (Sigma Aldrich
<100nm) is deposited and dried over a hot plate for 5 minutes
at 120oC. The sensor microscopic structure and chemical
composition mapping of the sensor surface is studied using
aJeolJXA-8530F HyperProbe Electron Probe Micro Analyzer
(EPMA).
The device obtained is fixed to a printed circuit board
including the excitation UV (365nm) LED and a simple very
low cost amplifier circuit (schematic in figure 2(a)) that helps
to avoid electrical noise due to the high impedance of the
device, the proposed amplifier induces an small level of
undesired distortion, however the distortion can be corrected
when the sensor is calibrated; the printed circuit board is
shown in Figure 2(b). The Paper-ZnO sensor is polarized
using 11 VDC and the current flowing through the sensor is
amplified 600 times through a lower impedance resistor to
obtain an easier to read output from the sensor. UV
illumination from a 365 nm LED is implemented over the
same printed circuit. Experiments were performed applying
luminous intensities of: 7, 5, 3.5, 2.2 and 1.1 mW. We studied
the sensitivity to O2, both applying a fixed UV intensity and
using 50 second ON-OFF pulses (10mHz). Using pulses may
help to understand better the O2adsorption when the device is
not illuminated by UV.
(a)
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2
(b)
Figure 2.(a) Schematic for the amplifier circuit used to enhance the signal, (b)
Actual printed circuit board including sensor, UV LED lamp and amplifier
circuit to make current measurements on different oxygen concentrations and
UV light intensities.
The sensor is tested in an air-pressure controlled container
applying different pressures from 1 to 0.1 Bar to test the
readings at different oxygen concentrations. Since oxygen is
23% wt. of air [27], this is equivalent to 276 g/m3of oxygen.
Thus, by changing sensor air pressure, we adjusted the oxygen
exposition to the sensor from 276 to 27.6 g/m3. Silica gel was
used as desiccant to keep a low humidity environment inside
the measurement chamber. Experiments were performed to
measure the effect of oxygen on the electric current flow
through the sensor at different O2concentrations and UV light
intensities to study the use of paper-based ZnO devices as
oxygen sensors. It was used a relative humidity logger
(Extech RHT10) to measure the effect of moisture on the
electrical current through a sensor device, this measurement
was performed without UV excitation at atmospheric
conditions.
III. RESULTS AND DISCUSSION
From the SEM characterization, we observed the
microscopic structure of the sensor used in this study. In
Figure 3(a, b, c) we observed the morphology of the fabricated
sensor. In these images, it can be noticed that the cellulose
fibers are coated by a film of ZnO particles. A good affinity
apparently exists between cellulose and ZnO that causes ZnO
particles to be homogeneously spread, forming a film that
allows photocurrent to flow through the device. ZnO crystals
size can be estimated from Figure 3(c) to be about a few
hundred nanometers.
This article has been accepted for publication in a future issue of this journal, but has not been fully edited. Content may change prior to final publication. Citation information: DOI
10.1109/JSEN.2014.2361780, IEEE Sensors Journal
Sensors-10604-2014 Paper-based ZnO Oxygen Sensor
Figure 3. Microscopic structure of ZnO crystals distributed over paper
surface. (a) X100, (b) X2,000 and (c) X15,000.
A chemical composition EDS HPMA mapping of the sensor
surface has been performed to determinate the presence of
Zinc from ZnO and Carbon from Cellulose, to be able to
differentiate between these two materials composing the
sensor. In figure 4(a) the mapped surface is shown. In figure
4(b) the composition of the surface is shown. The Zn atoms
from ZnO are shown in green and the C atoms from paper
cellulose are shown in red. Composition mapping shows that
cracks exist over the surface, affecting the electrical continuity
of the ZnO film. However from our electrical measurements,
we infer that these ZnO structures percolate to achieve
currents of several hundreds of nano Amperes when the device
is illuminated by UV light.
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Figure 4.EDS composition mapping for Paper-ZnO oxygen sensor substrate.
(a) surface mapped, (b) chemical composition mapping, Zn atoms from ZnO
in green and C atoms from cellulose in red.
In Figure 5 the photoconductivity rise on the ZnOpaper-
based sensor when exposed to UV radiation of different
intensities at atmospheric pressure can be observed. From
these measurements the large photoconductivity effect present
in these kinds of devices as already reported[10] can be
observed. The current on the sensor increases from around 5
nA to nearly 200 nA when 7 mW of UV light is applied. In
this experiment it is worthwhile noticing the non-linearity of
the current vs. light intensity. This non-linearity denotes that
some saturation effect may take place at high luminous
intensities probably due to the limit on the oxygen that can be
effectively adsorbed and desorbed over the ZnO surface.
200 UV Stimulus ON
7 mW
5 mW
Current (nA)
150
3.5mW
100 2.2mW
1.1mW
50
0 mW
0
0 10 20 30 40 50
Time (S)
Figure 5. Photoconductivity of paper-ZnO device exposed to different
intensities of UV light.
The sensor device is tested under different O2
concentrations and non-pulsed UV light intensities; the plot of
the currents obtained during this experiment can be seen on
Figure 6. In this plot it can be inferred that, at relatively high
concentration of O2(between 200-300 g/m3),there is a poor
resolution to differentiate the O2 level. However, as the
oxygen concentration nearby the sensor decreases, there is an
exponential increment in the sensor current which could be
used to measure the oxygen concentration detected by the
sensor. From the same series of measurements, it was
observed that the higher the UV power of the stimulus applied,
the larger the photocurrent is and, therefore, a better resolution
could be read from the sensor. These measurements were
taken exposing the sensor to the corresponding stimulus and
waiting until the reading stabilized. For the case of low
This article has been accepted for publication in a future issue of this journal, but has not been fully edited. Content may change prior to final publication. Citation information: DOI
10.1109/JSEN.2014.2361780, IEEE Sensors Journal
Sensors-10604-2014 Paper-based ZnO Oxygen Sensor 4

oxygen concentration (27.6 g/m3O2), the current takes up to 30 increases as the oxygen concentration clearly decreases.
minutes to stabilize.
The enhanced sensing speed using pulsed UV, might be
700 explained by the porous nature of the paper matrix in which
the ZnO crystals are embedded, this porous structure allows a
600
more quickly oxygen adsorption and desorption process, this
500
Current (nA)

can be traduced to a faster response of the sensor.

400
300
7 mW 500
200 27 g/m3
3.5 mW
100 1.1 mW 400

Current (nA)
0 0 mW
300
0 100 200 300 138 g/m3
3
Oxygen Concentration (gr/m3) 200 276 g/m

Figure 6. Current vs. Oxygen concentration for different intensities of UV 100

light applied.
The sensor developed was submitted to pulsed stimulus to
study the O2 absorption and desorption kinetics of the process.
This way of sensing oxygen could also lead to a faster way to
measure oxygen concentrations. In figure 7, Current vs. Time
is plotted when a 7 mW-10 mHz pulses are applied over the
sensor surface at different O2 concentrations. From this plot
we see that in a period of 1000 seconds the current from a
non-pulsed UV stimulus is not yet stabilized. On the other
hand, the current pulses resulting from pulsed UV stimulation
have more stable amplitude than the first pulse. The unstable
part of the signal is found at the DC level of the signal.
However, for practical use in a sensor, the DC part can be
filtered easily by analog or digital electronic means.
Therefore, by implementing a pulsed stimulus, the sensor
reading could be stabilized much faster in comparison with a
fixed UV stimulus.
600
500
400
Current (nA)
0
0 200 400 600 800 1000
Time (S)
Figure 8. Current signals from pulsed UV stimulated oxygen sensors at
different concentrations of O2.
All experiments performed in this work were done under
low humidity conditions (<40% R.H.), however to verify the
effect of the humidity changes we performed an experiment to
measure the current through an sensor device at different
relative humidity conditions, figure 9 shows a plot of the
current induced by humidity in a ZnO-paper oxygen sensor
(without UV stimulus), in this plot it can be noticed that the
current induced below 40% R.H. is about a few nA which is
negligible compared to the order of magnitude of the obtained
measurements when the sensor is excited with UV. However
this plot also shows that above 40% R.H. the moisture current
increases rapidly, therefore attention should be taken to keep a
low R.H. level.

100
300
200
I (nA)

100 10
0
0 200 400 600 800 1000
Time (S) 1
Figure 7. Current rise when a 0.1 Bar (27 g/m3O2) vacuum is applied. The 39 42 45 48 51 54
current for a non-pulsed UV stimulus takes a long time to stabilize (black R.H. (%)
line). Amplitude pulses for pulsed UV stimulus (red line) stabilize much
Figure 9. Current vs. relative humidity measured on a ZnO-Paper O2 sensor
faster in comparison to non-pulsed current.
(Without UV excitation).

The sensor has been tested using pulsed stimulus at A continuous current response experiment was been done
different O2concentrations. The current signals obtained from submitting the sensor to: (a) 1 atm. (b) pumping air down to
this comparison are shown in Figure 8. In these measurements, 0.1 atm. and (c) venting up to 0.5 atm. using both atmospheric
the amplitude obtained at different oxygen concentrations air and argon gas. The results of these experiments are shown

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This article has been accepted for publication in a future issue of this journal, but has not been fully edited. Content may change prior to final publication. Citation information: DOI
10.1109/JSEN.2014.2361780, IEEE Sensors Journal
Sensors-10604-2014 Paper-based ZnO Oxygen Sensor
in figure 10, from these results it can be noticed that Argon in
spite of being an inert gas has a detrimental effect on the
photoconductivity, however the effect of air venting at the
same pressure is much greater, from this result we can infer
that both oxygen partial pressure and absolute pressure affect
the paper-based sensor device, the absolute pressure effect
should be compensated or should be kept stable in order to
obtain a practical sensor from this type of devices.
Figure 10. Continuous current response of a sensor under different pressure
conditions, it is shown the effect of venting the sensor using atmospheric air
and Argon gas.
IV. CONCLUSIONS
In this study we demonstrated that oxygen sensor devices
could be made easily using common materials and a very
simple fabrication method. The sensor developed has been
exposed to UV pulsed and non-pulsed stimuli. From the
measurements made, it is observed that this kind of sensor
presents a much higher sensitivity at low concentrations of O2.
At a concentration level near to the atmospheric oxygen
concentration, the signal current variation measured is not
very significant and it might be lost due to the noise caused by
thermal fluctuations and humidity changes from the
environment. However, the noise problem could probably be
solved by compensating the signal implementing a proper
measurement of temperature and humidity, moisture
interference in the proposed sensors could also be avoided by
the use of desiccants. It is important to emphasize that in this
work we are proposing a novel method to develop gas and
chemical sensors using paper as substrate, the use of paper as
substrate brings both advantages and disadvantages, however
from our experiments it can be inferred that most technical
problems can be solved or compensated in order to obtain a
practical sensor. As a compensating technique for example:
temperature response on this kind of device follows a well-
known Arrhenius behavior[28]; therefore Arrhenius equation
could be used to compensate the O2 measurements by using a
thermometer to read sensor temperature.
Also relevant, we observed that applying UV pulses instead
of a non-pulsed stimulus helps to obtain a much faster
measurement by measuring the amplitude of the current pulses
readout of the paper sensor device. The way in which we
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5
implemented our experiments opens the possibility of using
the devices developed in this work as vacuum sensors for
oxygen containing environments. The results obtained in this
work corroborate that using paper as a substrate matrix for
semiconductiveZnO crystals enhances the capacity of this
material to absorb and desorb oxygen which can be an
advantage for the fabrication of oxygen sensors and probably
for other types of chemical sensors.
ACKNOWLEDGEMENTS
We thank Ken Pomper from Peace Corps for proof reading
the manuscript, Jose EleazarUrbina Alvarez for his assistance
to use the Electron Probe Micro Analyzer, Reina Aracely
Mauricio Sanchez and Rivelino Flores Fariasfor technical
assistance.
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