Preliminary Analysis on Cellulose-based Gas Sensor by Means of
Aerosol Jet Printing and Photonic Sintering
Edoardo Cantù
1
, Matteo Soprani
1,2
, Andrea Ponzoni
1,2
, Emilio Sardini
1
and Mauro Serpelloni
1
1
Department of Information Engineering, University of Brescia, Via Branze, Brescia, Italy
2
National Institute of Optics, National Research Council, Brescia, Italy
Keywords: 3-D Printing, Aerosol Jet Printing, Photonic Sintering, Ammines Sensing, Cellulose-based Sensor.
Abstract: In this paper, we present a preliminary analysis on the possibility to realize low-cost and eco-friendly
cellulose-based gas sensors by means of Aerosol Jet Printing (AJP) and flash lamp annealing (FLA). To the
authors knowledge, it is the first time that these two techniques are combined in the realization of such a
device. The intrinsic hygroscopic properties are the key element of this device: cellulose contains substantial
amount of moisture, adsorbed from the environment, enabling the use of wet chemical methods for sensing
without manually adding water to the substrate. The sensors were tested in terms of electrical resistance. The
penetration of the carbon ink in the cellulose network was stated thanks to cross-sections captured at the
microscope. Once placed in a damp environment, all the sensors showed a comparable behavior settling at an
asymptotic value of 3.68 (relative standard deviation of 8%). In presence of different concentration of
NH4OH, the sensors showed a resistance proportional to the amount of analyte present in the working volume,
showing 25.6% increase compared to the 0.5 M concentration, while 34.1% compared to the 1M.
1 INTRODUCTION
Printed electronics represents an attractive and
innovative field of application of Additive
Manufacturing (AM) with flexible electronic devices,
paper electronics and wearable devices that are
becoming widespread coming with the need for
advanced printing processes, reducing the number of
processing steps, material waste and production cost
(Gandhiraman et al., 2014).
3D printing is considered a valid candidate for the
new generation of biosensors (Ragones et al., 2015;
Yang et al., 2016), and Aerosol Jet Printing (AJP) is
belonging to this technological family. AJP is a
direct-write printing technique which deposits a
continuous aerosol beam of liquid droplets,
generating specific surface features without
masks(Hoey et al., 2012; Lee, An and Chua, 2017).
The liquid inks typically have a viscosity between 1
and 1000 cP, in case of pneumatic atomization, and 1
to 5 cP, in case of ultrasonic atomization (Tan, Tran
and Chua, 2016). Once the mist is generated, it passes
through the virtual impactor to regulate droplets
dimensions and then it is focused on the substrate
thanks to a coaxial sheath gas flow(Binder, Glatthaar
and Rädlein, 2014; Wadhwa, 2015; Optomec, 2017).
This 3D printing technique is adopted in different
fields: high-efficiency solar and fuel cells, thin-film
transistors, resistors, antennae, MEMS,
photodetectors, thermistors, etc. But it is also used in
applications for the biological field like high-density
assays for drug discovery, lab-on-chip devices,
protein and glucose sensing (OPTOMEC, no date;
Coupland et al., 2010; Yang et al., 2016; Wang et al.,
2017; Bolse et al., 2017; Liu et al., 2017; Agarwala
et al., 2018; Baldwin et al., 2018; Cantù et al., 2018;
Gupta et al., 2018; Khorramdel, Torkkeli and
Mäntysalo, 2018; Di Novo et al., 2019).
In the printed electronics field, the sintering step
is mandatory to ensure a proper conductivity in the
printed layer, which is usually performed by means of
hoven for high temperature processes. One of the
emerging topics in printed electronics is the usage of
paper due to its unique capabilities (high Young’s
modulus, biodegradability, biocompatibility,
renewability, low-cost, lightweight) (Kim et al.,
2014). This material needs great attention in sintering
printed inks due to low melting/ignition point.
Therefore, only low-temperature processes are
allowed, which do not ensure high conductivities.
Photonic sintering, also known as flash lamp
annealing (FLA) or intense pulsed light (IPL), is a
200
Cantù, E., Soprani, M., Ponzoni, A., Sardini, E. and Serpelloni, M.
Preliminary Analysis on Cellulose-based Gas Sensor by Means of Aerosol Jet Printing and Photonic Sintering.
DOI: 10.5220/0009095702000206
In Proceedings of the 13th International Joint Conference on Biomedical Engineering Systems and Technologies (BIOSTEC 2020) - Volume 1: BIODEVICES, pages 200-206
ISBN: 978-989-758-398-8; ISSN: 2184-4305
Copyright
c
2022 by SCITEPRESS Science and Technology Publications, Lda. All rights reserved
technology, developed by Novacentrix, in which the
heating process is accomplished thanks to a couple of
xenon flash lamps and mirrors which radiate energy
toward the sample that must be sintered, following
phenomenon of melting/sintering point depression in
nanoparticles described by the Gibbs-Thomson
equation.
The advantages are remarkable: this is a fast
sintering technique (heat treatment in the
milliseconds scale), it produces minimal damage to
low temperature substrates and avoids unwanted
processes (diffusion). Possible applications range
from thin-film transistors, solar cells, RFID
components to wearable devices, using conductive,
bioresorbable or ceramic inks (silicon, silver, zinc) on
different kind of substrates (wood, cardboard,
textiles, glass, kapton (West et al., no date; Akbari et
al., 2017; Mahajan et al., 2017; Mudgal et al., 2017;
Rizwan et al., 2017; Bobinger et al., 2018; Cronin et
al., 2018; Danaei et al., 2018; Li et al., 2018; Schube
et al., 2018).
In light of this, the present work aims to propose
the combined use of AJP and FLA, to realize a
c
ellulose gas sensor, designed for food industry. Food
waste is one of the hardest challenges for humanity as
it impacts on society not only in food terms (direct
food loss and waste), but also in environmental terms
(exploitation of water and land, disposal, emissions)
(Springmann et al., 2018) For example, the use by-
date is an estimation of the date on which a perishable
product may no longer be edible, and this number
cannot clearly state the condition of the food (Labuza
and Taoukis, 1990).
Ammonia and its compounds can be considered
toxic, capable of generating damages and unwanted
pathologies to human body if ingested (nausea,
migraine, vomiting, allergies) (Douny et al., 2019;
Filipe-Ribeiro et al., 2019). The research is working
on wireless and automated systems capable to
continuously give a feedback of the sample (Bellitti
et al., 2017; Tonello et al., 2017). The possibility to
include a sensor inside the packaging appears to be a
solution which can monitor the current state of the
food defining its freshness (Yam, 2012; Liu et al.,
2015).
Paper-based sensor with carbon electrodes
exploits the intrinsic hygroscopic characteristics of
cellulose paper. Cellulose fibers contain a certain
amount of moisture, even if paper looks dry. This
aspect is mandatory in evaluating the presence of
water-soluble gases. In presence of a water-soluble
gas (due to food degradation), electrical impedance or
conductance of paper can be probed thanks to carbon
electrodes realized on the surface of the paper sheet.
The feasibility of these sensors has been recently
reported in literature using a low-cost cutter plotter
for preparation (Barandun et al., 2019). Our goal is to
develop this class of devices by combining the AJP
and FLA methods, investigating the improvement we
can achieve thanks to the more sophisticated
preparation technique. Chapter two will present
methods followed during tests, while chapter three
shows the results obtained during validation and
characterization tests. Chapter four will summarize
the preliminary results achieved, with future
perspective of this application.
2 SENSOR FABRICATION
2.1 Sensor Design
Optomec’s Aerosol Jet Printing AJ300 system was
employed in the fabrication of the proposed gas
sensor: this 3D printing machine is designed to
interface with AutoCAD drawings. Specific attention
was put in the definition of printing parameters,
considering inks viscosity, in order to achieve a
homogeneous filling of the interdigitated geometry,
also thanks to the use of a crossed pattern. The sensors
were designed thanks to AutoCAD software
(Autodesk), a devoted Optomec’s gadget for
AutoCAD ensured a proper ink filling of closed
shapes. The lines were designed as polylines to
improve the timing and the homogeneity of printed
lines.
Surface area of the interdigitated electrodes and
spacing in between, are the two main factors that must
be considered during the design phase, thus
determining the overall impedance of the sensors,
which have a critical effect on its sensitivity. More
specifically, a total sensing area of 150 mm
2
and a
spacing of about 1.5 mm were selected (fig. 1).
Figure 1: AutoCAD layout of the sensor.
Preliminary Analysis on Cellulose-based Gas Sensor by Means of Aerosol Jet Printing and Photonic Sintering
201
2.2 Materials and Methods
Whatman
TM
chromatography 1 cellulose paper is the
selected substrate on which we printed our sensors,
due to the capability of this kind of paper to capillary
handling liquid samples. The second reason we
employed this material is the high degree of purity
respect to other commercial grades which include
chemical additives that could influence the
functioning principle of the proposed sensors. Thanks
to its highly hygroscopic properties, cellulose fibers
within paper contain a substantial amount of
moisture, even if it looks dry (at a relative humidity
of 50%, paper contains ~5% water by weight).
Additional ions coming from the dissociation of
water-soluble gases on the surface of paper increases
its ionic conductance.
Carbon ink (EXP 2652-28) was purchased by
Creative Materials Inc., characterized by a starting
viscosity of 15-20 mPa∙s. The ink was properly
atomized together with its own thinner to obtain a
better printability and adhesion to the substrate.
Carbon ink specific process parameters are reported
in Table 1, while figure 2 presents a prototype and our
AJ300 during printing.
Table 1: Printing process parameters for C ink.
Process Parameters
Sheath
g
as flow
(
SCCM
)
110
Atomizer flow
(
SCCM
)
770
Exhaust flow (SCCM) 750
Process speed (mms-1) 4
Plate temperature (°C) 70
Figure 2: AJ printer printing a first concept (left); a printed
sensor in its final layout (right).
With the aim to define the sintering parameters
for our carbon sensors, a sample geometry was
considered in order to define FLA sintering
parameters. These samples were tested in terms of
electrical resistance, evaluated thorough the digital
bench-top multimeter Hewlett-Packard 34401a,
applying testing probes to the extremities of each
path, in standardized and repeatable points, thus
measuring the resistance offered by all its length.
An optical microscope by Orma Scientific
NB50T (trinocular zoom 0.8x–5x–LED), with its
devoted software and HDMI MDH5 camera model,
was used to acquire the images and to evaluate the
features of the printed elements (Orma Scientific,
Sesto San Giovanni, Milan, Italy).
After the definition of the abovementioned
parameters, four sensors were put in four different
vials to examine their capability to absorb ions
present in a humidified atmosphere and their response
was simultaneously studied in terms of resistance. 5
ml was the selected working volume and distilled
water was employed for the stabilization step (used to
reach a relative humidity of 100 % inside the vial to
let sensors work properly in presence of water-soluble
gases), aiming to state the repeatability of this kind of
measurement principle with these AJ printed sensors.
After this step, a qualitative study was performed by
means of distilled water/NH
4
OH solutions in two
different concentrations, 1 M and 0.5 M, which will
develop a gas-phase of ammonia in a humidity
saturated air background. Additional tests have also
been carried out with ethanol in an ambient air
background to test the working mechanism of this
class of devices. Four digital bench-top multimeter
Hewlett-Packard 34401a were connected thanks to a
GPIB-USB cable to a personal computer and the
behaviour of the sensors monitored thanks to a
program written in LabVIEW.
3 PRELIMINARY RESULTS
Once printed, carbon samples must be sintered in
order to ensure the realization of a unique conductive
track. Impulse duration was studied keeping it fixed,
initially at 1000 μs, increasing the lamp voltage from
200 up to 300 V. The same approach was replicated
for other three pulse time-lengths, specifically 1250,
1500 and 1750 μs. At the end of this step the best
sintering parameters which gave the lowest resistance
were selected. As evidenced in figure 3, 1000 μs
seems to be a too short impulse duration, being not
able to completely penetrate the whole thickness of
our chromatographic paper (paper thickness is about
180 μm). 1250 and 1500 μs showed a similar
behavior, with the second one presenting a lower
resistance.1750 μs and 250 V are the best sintering
parameters, as they allow to reach a final resistance
of 2.8 kΩ (relative standard deviation of 7%). So, the
BIODEVICES 2020 - 13th International Conference on Biomedical Electronics and Devices
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complete pool of production parameters for our
sensors are the ones reported in table 1, with six
consecutive depositions, sintered at 250 V, 1750 μs.
Figure 4 displays a magnification of an
interdigitated printed element, suggesting the need of
a proper wavelength to fully penetrate the cellulose
sheet to sinter carbon ink. The effectiveness of the
deposition process was initially tested evaluating the
resistance of individual dry electrodes resistance,
after both printing and sintering steps. It was found a
mean value of 8.45 kΩ (relative standard deviation of
23%) after printing, while 7.44 kΩ (relative standard
deviation of 21%) after sintering. It is interesting to
compare these values with those reported in literature
for a preparation method based on an ultra-low cost
cutter plotter printer. In this case the average
resistance is of an individual electrode is 6.40 with
a relative standard deviation of 43% (Barandun et al.,
2019). The presented results demonstrate a difference
in standard deviation of 22% so the combine use of
AJP and FLA have improved the sensors realization
procedure.
Figure 3: Resistance measurements as funciton of voltage
at different impulse duration, for C samples.
Figure 4: Magnification of an interdigitated element
(bottom).
To validate and demonstrate the functioning of
our paper-based sensors, they were tested in a damp
environment. Four sensors were simultaneously put
in four different vials in presence of a working
volume of 5 ml of distilled water. Figure 5 shows the
behaviour of the sensors reaching the stabilization at
an asymptotic value of
3.68 MΩ
(relative standard
deviation of 8%). The condition step was 30 hours
long in order to clearly evidence the stabilization of
the sensors reaching a relative humidity inside the
vial of 100 %. Since sensors resistance appeared to be
stable before reaching the thirtieth hour, in future
works the precondition duration will be performed
taking into account only the strictly necessary time.
Figure 5: Resistance values during stabilization of four
sensors in distilled water.
After this, a simple qualitative study was
performed aiming to state the capability of the sensor
to recognize different concentrations of the same
analyte in a humidity saturated background, which
optimize the sensing mechanism of this kind of
devices (Barandun et al., 2019). Once run a
precondition phase in presence of 5 ml of water, one
sensor was exposed to the vapours generated by a 1M
solution of NH
4
OH in water, one sensor with a 0.5M
solution of NH
4
OH and one with a new vial with
distilled water (blank sample). To further test the
effect of the working environment, an additional
experiment has been carried with a fourth sensor
exposed to vapors generated from an ethanol solution.
This allows to test the effects of extreme working
conditions (saturated ethanol, vapors).
Figure 6 evidences these experiments.
The data regarding NH
4
OH vials are reported as
ΔG/G
0
in percentage in table 2. ΔG values are
calculated as the difference between the maximum
and minimum resistance values when the analyte is
recognized after vial change, while G
0
is the
minimum resistance value in the same time interval.
The sensors show a 25.6% increase compared to the
0.5 M concentration, while 34.1% compared to the
1M. Thus, with an 8.5% difference between the
highest and the lowest concentration.
The exposure to saturated ethanol vapours in the
ambient air background cause a sudden and large
increase of the sensor resistance. This extreme
behaviour is likely to arise from the large ethanol
concentration (saturated vapours), which modifies the
condition of the cellulose fibres making them
Preliminary Analysis on Cellulose-based Gas Sensor by Means of Aerosol Jet Printing and Photonic Sintering
203
anhydrous, hence much less suitable for ionic
conduction. The result further supports the working
mechanism proposed in literature, based on the
intrinsic ionic conductivity of the water layer
covering cellulose in ambient conditions. To better
clarify this point, we have planned additional tests
with lower ethanol concentrations.
Table 2: ΔG comparison between 0.5M and 1M solutions.
Concentration (M) ΔG/G
0
(%)
0.5 25.6
1 34.1
Figure 6: Behaviour of the sensors in presence of different
analytes (water, ethanol, NH
4
OH 1 M and 0.5 M).
4 CONCLUSIONS
We present a new kind of disposable gas sensor,
produced thanks to Aerosol Jet Printing and Flash
Lamp Annealing on a cellulose-based material. The
production method presents good reproducibility
despite a porous substrate such as chromatographic
paper. In this first research step, we want to verify the
functioning of the sensors, considering a first design
which is not optimized for our future perspectives.
The following steps will regard the complete
optimization of the production procedure, thus
redefining the optimal sintering parameters for the
new the design of the sensors. Once tested in presence
of a damp environment, our device behaved in the
same way, showing an asymptotic value of
3.68
,
regardless of the specific starting conducting value.
The sensors were also qualitative tested, showing a
signal proportional to the amount of NH
4
OH present
in the sample volume. Future developments will
regard the investigation of the limit of detection of
these cellulose-based sensors and their selectivity. In
particular, tests are planned to check the effects of
ethanol vapours, which are likely to alter the hydrous
status of the cellulose fibres, especially at high
concentrations. More in general, considering the
prospective to tune the sensing properties of this class
of devices to a given gas-target, this possibility should
be strictly checked against its working principle,
whose simplicity represents at the same time the
strength and the weakness of these devices. Indeed, if
gases containing ammine groups can be easily sensed
by this simple and extremely cost-effective device,
any alteration of the hydrous status if the paper may
deeply alter its sensing capability. Any
functionalization of the paper aimed to tune its
sensitivity to a given gas-compound, should be
carried out in careful consideration of this aspect.
ACKNOWLEDGEMENTS
The authors declared no conflict of interest.
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