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Sensors and Actuators B 127 (2007) 447–454

An ammonia gas sensor based on non-catalytically synthesized carbon

nanotubes on an anodic aluminum oxide template
Nguyen Duc Hoa, Nguyen Van Quy, Yousuk Cho, Dojin Kim ∗
School of Nano Science and Technology, Chungnam National University, Daejeon, Republic of Korea
Received 7 February 2007; received in revised form 27 April 2007; accepted 27 April 2007
Available online 3 May 2007

Abstract
In this study, an ammonia gas sensor structure for mass production is realized with an array of carbon nanotubes synthesized on an anodic
aluminum oxide (AAO) template. The device is expected to yield a uniform performance due to the regular and uniform nano channels in the
AAO. It is a vertical structure made with open-ended multi-wall carbon nanotubes through deposition on the inside wall of the AAO so that the gas
would diffuse into the nano channels for adsorption. The carbon nanotubes are in the form of flaked carbons having many defect sites. The results
show that the sensor has high sensitivity, fast response time of less than 1 min and good reproducible recovery behaviors in atmospheric pressure
at room temperature.
© 2007 Elsevier B.V. All rights reserved.

Keywords: Carbon nanotube; AAO; Ammonia gas sensor

1. Introduction difficult to control due to the self-assembling nature of the syn-

Gas sensors have attracted interest due to their varied appli-
cations [1–5]. Many of the traditional gas sensors were based
on the change in electrical conductance of the semiconducting
oxide materials, such as WO3 , TiO2 , SnO2 and ZnO [6–9]. The
oxide gas sensors, however, usually operate above room temper-
atures, rendering limited practical applications. Recently, with
the advent of carbon nanotubes (CNTs), they have attracted great
interest for use as gas sensors mainly due to their large surface
area, high electrical conductivity and chemical stability while
the surface reacts with gas molecules [10–14].
CNT-based sensors have been investigated for the detection
of gases of H2 , NO2 , CO2 , O2 and NH3 [15–20] as well as of
other chemicals like organic compounds [21,22]. Both single-
wall (SWNTs) and multi-wall carbon nanotubes (MWNTs) have
been used as the sensing probes. For device fabrication, either
CNTs were directly synthesized on substrates via chemical
vapor deposition (CVD), or the collected CNT powders were
pasted on substrates. In the former method of CNT application,
our experience showed that the uniformity of the CNTs was
∗ Corresponding author. Tel.: +82 42 821 6639; fax: +82 42 823 4224.
E-mail address: dojin@cnu.ac.kr (D. Kim).
thesis process. In particular, the control of the synthesis process
is usually not accurate enough to reproduce the length, density
and diameter of the CNTs from operation to operation. Also, the
poor adhesion of the CNTs on substrates is related with device
reliability. On the other hand, in the latter method, the perfor-
mance and sensitivity of the sensor device will greatly depend
on the amount of CNTs in the pastes. For a higher content of
CNTs in the paste, blending is a critical issue that is yet to be
resolved. Therefore, a precise control of the CNT amount in the
paste and the paste thickness are required for device uniformity.
In this context, the authors propose a new CNT sensor
structure. Its main features are: (i) the substrate called anodic
aluminum oxide (AAO) and (ii) the CNTs synthesized on the
surface of the nano pore wall. The AAO fabricated on a Si sub-
strate is mechanically stable and forms regular arrays of nano
pores of uniform diameter and length. The CNTs synthesized on
the surface of the nano pore wall conform to the geometry of the
nano pores in the AAO, and thus they also form regular arrays
of nanotubes of uniform diameter and length. In addition, since
the size control of the nano pores in AAO is very much repro-
ducible in the anodization process, the uniform CNT structure
can be reproducibly realized. Due to the large-area extensibility
of the AAO template, sensor devices can be mass-produced as
well. This integration capability of uniform structure is a key

0925-4005/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2007.04.041
448 N.D. Hoa et al. / Sensors and Actuators B 127 (2007) 447–454
factor in all the device fabrication procedures. Another charac-
teristic of the sensor is the vertical structure, which is contrary
to other parallel-to-the-surface structures in that it monitors the
gases diffused into the nano pores and adsorbed on the inside
wall of the CNTs. We tested the structure as an ammonia sensor
using the conductance change upon the gas adsorption.
2. Experiment
The schematic of the fabrication process of the sensor struc-
ture is illustrated in Fig. 1. It consists of fabrication of the AAO
template on a p-type Si(1 0 0) substrate (Fig. 1(a)), CNT synthe-
sis on the AAO by thermal CVD (Fig. 1(b)), formation of the
nano channel probe structure (Fig. 1(c)) and electrode formation
(Fig. 1(d)).
2.1. Anodic aluminum oxide template
The AAO template of nano pores was fabricated with Al
thin films deposited on Si wafers via the two-step anodization
process [23]. Aluminum thin films of ∼2 ␮m thickness were
deposited on p-Si(1 0 0) wafers using a RF-sputtering method.
The deposited Al films were annealed at 500 ◦ C in a nitrogen
atmosphere for 30 min to improve their adhesion to the Si sub-
strate. The first anodization process was carried out in a 0.3 M
oxalic acid solution maintained at 10 ◦ C. A constant voltage
of 45 V was applied between the cathode and the anode for
∼12 min. Since the morphology of the nano pores formed via
the first anodization was relatively poor, the AAO layer was
dip-etched away in a solution of 6 wt.% phosphoric acid and
1.8 wt.% chromic acid balanced in water. The Al surface after
the first anodization and the removal processes provided a sur-
face morphology suitable to seeding towards a more regular
array of nano pores. The second anodization was carried out for
25 min in the same manner as in the first anodization process.
The nano pores were then dip-etched in a 0.1 M phosphoric acid
Fig. 1. Schematics of sensor fabrication process. (a) Synthesis of AAO on p-type Si substrate, (b) synthesis of CNTs by thermal CVD, (c) removal of the top carbon
layer by oxygen plasma (for 1200 ◦ C synthesis) and (d) Ag electrode deposition.
for 35 min to completely remove the barrier layer at the bottom of
the nano pores. This process was necessary to guarantee the elec-
trical contact between the substrate and the CNTs, which will be
formed on the nano pore wall in the next step. Thus, the formed
AAO/Si substrate is schematically illustrated in Fig. 1(a). The
resultant nano pores in the AAO template are shown in Fig. 2(a).
2.2. CNT synthesis
CNTs were synthesized via a thermal chemical vapor depo-
sition (CVD) method. The CNTs on AAO templates can be
synthesized with or without metal catalysts. With the metallic
catalyst particles, the CNT synthesis usually occurs randomly
on a part of the particles, and it further grows out of the pores
[24,25]. This morphology has no advantages for using the reg-
ularity of the nano structure involved in the AAO template.
Therefore, we employed the synthesis without the catalysts. In
addition, we show in this study that flaked graphite sheets of
MWNTs are pyrolytically deposited on AAO, conforming to the
surface geometry of the nano pores [26]. Thus, a high synthesis
temperature could be expected to enhance the crystallinity of
the CNTs. We compared the gas sensing properties of the CNTs
synthesized at two different temperatures of 1200 and 900 ◦ C.
The AAO/Si template was placed in a horizontal quartz tube
furnace, and the tube furnace was evacuated to ∼10−3 Torr. The
furnace temperature was then raised to the synthesis tempera-
tures at a rate of 15 ◦ C/min for the CNT synthesis by allowing a
mixture of C2 H2 (90 sccm) and NH3 (10 sccm) gases to flow for
30 min. During the growth, the pressure in the furnace tube was
kept at ∼10−2 Torr. After the CNT growth, the tube was evacu-
ated again to ∼10−3 Torr and was kept there while the furnace
cooled down to room temperature.
The synthesis of CNTs on the AAO template is done by pyrol-
ysis of the carbon source, and the CNT growth rate on the top
of AAO is much faster than in the pores of AAO [26]. Thus,
the pore entrances are often blocked by an overgrown carbon
 N.D. Hoa et al. / Sensors and Actuators B 127 (2007) 447–454
Fig. 2. SEM images for (a) the AAO template (insert shows the top view), (b) the CNTs with blocked pores (1200 ◦ C synthesis), (c) the CNTs with open ends (900 ◦ C
synthesis) and (d) the sensor with Ag electrode deposition.
layer through the shadow effect, while the inside of the pores
are voided with CNT formation in the step, as shown in Fig. 2(b).
This is the case particularly at a high synthesis temperature of
1200 ◦ C. The top graphite layer then needs to be removed to
use the CNTs on the pore wall as the sensing probe. Oxygen
plasma etching was then used in order to remove the carbon
layer deposited on the top in order to obtain open tube CNTs in
the step, as shown in Fig. 1(c). This was done for 20 min with a
radio frequency power of 100 W at a pressure of ∼5 ×10−2 Torr.
However, the growth kinetics at 900 ◦ C was relatively slow, and
the pore entrances could be maintained open during the synthe-
sis; thus, the oxygen plasma etching process was not required.
In the following, we will see the effect of oxygen treatment on
the sensor performance.
The morphology of the synthesized CNTs was examined by
field-emission scanning electron microscopy (FE-SEM, Hitachi
S-4700), high-resolution transmission electron microscopy
(HRTEM), micro Raman spectroscopy using a wavelength
of 514.532 nm (Ar-ion laser) and X-ray photoelectron spec-
troscopy (XPS) methods.
2.3. Device fabrication and characterization
Thin films of Ag were then sputter deposited for the elec-
trode. In order to avoid the deposition into the pores, the sample
449
was tilted at about 30◦ from the normal incidence of the sputter
beam. The dc sputtering process was carried out at a pressure
of 5 × 10−3 Torr and a current of 40 mA for 2 min to achieve a
thickness of 40 nm (Fig. 1(d)).
The test chamber was first evacuated and then filled with N2 .
The initial state of the gas sensing test was established by a
steady state resistance of the sensor under a nitrogen flow. The
gas sensing properties were measured at atmospheric pressure
of the gases at room temperature by measuring the resistance
between the top Ag electrode and the bottom semiconductor.
The gases of nitrogen and ammonia were introduced into the
chamber at a rate of 500 sccm using mass flow controllers. The
concentrated ammonia was diluted by mixing with high purity
of N2 gas.
3. Results and discussion
3.1. Carbon nanotube property
The morphologies of the AAO template and the synthesized
CNTs investigated with FE-SEM are shown in Fig. 2. The AAO
nano pores of two-dimensional arrays with uniform size and dis-
tribution are illustrated in Fig. 2(a). The diameter and inter-pore
distance were about 65 and 105 nm, respectively. The pore length
450 N.D. Hoa et al. / Sensors and Actuators B 127 (2007) 447–454

was about 1.4 ␮m. It can be seen that the pores go through the
substrate. The morphology after the CNT synthesis at 1200 ◦ C is
shown in Fig. 2(b), where the entrances of the pores are blocked
with graphite layers due to the accelerated pyrolysis at a rel-
atively high synthesis temperature. The morphology at 900 ◦ C
did not show the blocking of the entrances, as shown in Fig. 2(c).
The surface with open entrances, after removing the top graphite
layers by oxygen plasma for 1200 ◦ C grown CNTs, was appar-
ently similar to that in Fig. 2(c). The partly cracked section
also revealed the CNTs synthesized on the inside of the pore
walls. The morphology after Ag electrode deposition is shown
in Fig. 2(d).
The crystallinity of the synthesized carbon nanotubes was
examined with TEM and Raman spectroscopy. Fig. 3(a) shows
a TEM image of the 1200 ◦ C grown CNTs taken after etching the
AAO template away. This again revealed the uniformity of the
synthesized CNTs in length and diameter. The average length
was 1.4 ␮m according to the length of the pores, but the diameter
of the CNTs, ∼70 nm, was a little greater than that of the pores.
The latter can be attributed to the shrinkage of the AAO body
during the high-temperature CNT synthesis. The as-synthesized
AAO template by anodization was mostly in amorphous form,
but it crystallized with high temperature annealing [27]. The high
synthesis temperature would certainly offer the annealing effect
for the crystallization and densification of the AAO, and accord-
ingly enlarge pore diameters. Fig. 3(b) shows an HRTEM image
of the MWNT wall grown at 1200 ◦ C. The stack of graphene
sheets was clearly observed for its thickness of ∼15 nm. The
crystallinity was better than that grown at 900 ◦ C, as shown in
Fig. 3(c). It is well known that the CNTs synthesized on AAO
without catalyst are formed by flakes of carbon sheet instead
of continuous sheets. One study noted at the higher tempera-
ture synthesis that: (i) the sizes of the flaked graphite plates
are greater and (ii) the interlayer spacing is ∼0.34 nm, which
agrees well with the spacing of the graphite of high crystallinity
[28]. Therefore, the present results are great improvements in
crystallinity with respect to the lower-temperature synthesis.
Raman spectroscopy investigation also revealed the high
crystalline quality of the synthesized MWNTs, as shown in
Fig. 4. In general, two main peaks were observed at 1288 and
1592 cm−1 . They are called D- and G-bands, respectively [29].
The D-band is known to be associated with defective, disordered
graphite or glassy carbon, while the G-band is related to the sp2
vibration in the graphite of a two-dimensional hexagonal lattice
[30]. The ratio of the peak intensities or IG /ID has often been
referred to as a measure of the crystallinity of the synthesized
carbon nanotubes [29]. The estimated ratio of ∼1.17 for 1200 ◦ C
CNTs was compatible with that of the MWNTs synthesized on
catalytic metals via a thermal CVD method [29]. The spectrum
can again be compared with that synthesized at a lower tem-
perature of 900 ◦ C [31], where the smaller IG /ID ratio (∼0.8)
suggests more defects in the CNTs. This comparison again con-
Fig. 3. (a) TEM image of the CNTs showing uniform distribution of length and
firms the higher crystallinity of the CNTs for higher synthesis diameters. HRTEM images of the CNT walls synthesized at (b) 1200 ◦ C and (c)
temperature. 900 ◦ C.
The XPS examination of the 1200 ◦ C CNTs is shown in
Fig. 5(a). It shows the presence of aluminum, oxygen and car-
bon. The analysis of the C 1s peak reveals it as an overlap of some
 N.D. Hoa et al. / Sensors and Actuators B 127 (2007) 447–454
Fig. 4. Raman spectra of the CNTs synthesized at (a) 1200 ◦ C and (b) 900 ◦ C.
peaks (Fig. 5(b)). The peak at 284.4 eV is attributed to sp2 car-
bon, and this C–C bonding peak indicates the high crystallinity
of the CNTs. The other broad peak at 288.5 eV is attributed to
carbons attached to oxygen (e.g., carboxyl and C–O groups)
[32]. The peak for metal-carbide (Al–C) at 282 eV was absent,
indicating the high thermal and chemical stabilities of the CNTs
at the employed high temperature of 1200 ◦ C. All the compar-
Fig. 5. (a) XPS spectrum of the CNTs synthesized at 1200 ◦ C and (b) the high
resolution of the core level peak for C 1s.
451
isons and measurements conclude that the employment of high
temperature in the CVD synthesis on AAO can really enhance
the crystallinity of the CNTs. However, we note that the gas sens-
ing properties were not positively related with the crystallinity
of the CNTs.
3.2. Sensor property
It is known that the conductivity of CNTs changes with the
adsorption of gas molecules, and such behavior allows us to use
CNTs as gas sensors. The current–voltage (I–V) characteristic of
the as-synthesized CNTs was measured by applying the voltage
between the top Ag electrode and the p-type Si substrate. The
typical I–V characteristic of the junction between the CNTs and
the Si substrate in nitrogen environment is illustrated in Fig. 6 for
the 1200 ◦ C grown CNTs. It reveals that the multi-wall metallic
flaked carbons form a rectifying junction at the contact with
p-type Si. The turn-on voltage was ∼0.5 V, which agreed well
with a report on MWNTs [33]. A similar rectifying I–V curve
was also obtained for the 900 ◦ C CNTs.
As shown in Fig. 6, the resistance change in an ammonia
gas environment was noticeable at forward biases (Va ). How-
ever, an interesting observation was that the resistance change
was positive for the 1200 ◦ C CNTs sensor, while it was neg-
ative for 900 ◦ C one, as clearly illustrated in Fig. 7(a), where
the response was measured upon the introduction of 6% ammo-
nia gas at Va = 5 V. A theoretical calculation showed that each
NH3 molecule donates 0.04 electrons to the nanotubes when
adsorbed on the surface of carbon nanotube [34]. Since ammo-
nia is an electron donor, a resistance decrease was expected
with ammonia adsorption on the CNTs. This is the case for the
900 ◦ C CNTs. However, the 1200 ◦ C CNT sensor behaves like
a p-type semiconductor, or resistance increases with ammonia
adsorption. Recall that the 1200 ◦ C CNTs underwent an oxygen
plasma etching process to remove the top carbon layer, while
the 900 ◦ C CNTs did not. This type of conversion was caused
by an oxygen adsorption as observed in other MWNTs [35] and
SWNTs [36]. This oxygen treatment effect was confirmed with
the 900 ◦ C CNTs sensor. It originally revealed a decrease in
Fig. 6. Current–voltage characteristics of the sensor with nitrogen () and
ammonia () flows for the CNTs synthesized at 1200 ◦ C.
452 N.D. Hoa et al. / Sensors and Actuators B 127 (2007) 447–454
Fig. 7. (a) Resistances change of the sensors by switching from N2 to NH3 (6%)
flow and (b) the sensor response of the sensors measured with varying the NH3
concentration.
resistance upon exposure to ammonia, but it rather revealed an
increase after exposure to oxygen plasma, as shown in Fig. 7(a).
Fig. 7(a) also compares the response to NH3 between the sen-
sors. When exponential function, exp(−t/τ) was used for fitting,
the response time τ was estimated to be ∼1.1, ∼0.3 and ∼0.5 min
for 900 ◦ C, 900 ◦ C oxygen treated and 1200 ◦ C sensors, respec-
tively. The fittings with one variable were quite excellent. In
particular, this response time is not worse than other high-quality
MWNT sensors [4,35,37]. The fast response time was more
remarkable considering the geometry of the device. Most of
the conventional sensor probes were freely exposed towards the
gas flow, and therefore, the sensing probes could quickly estab-
lish contact with the gases, and the response time depends on the
dynamics of the moving gases. On the contrary, our vertical nano
channel structure requires the diffusion of gas molecules deep
into the concave nano channels for adsorption. This will degrade
the response time as well as the sensitivity. The shorter response
time in the oxygen adsorbed CNT sensors suggests the positive
role of oxygen in the kinetics of NH3 molecules adsorption, but
the effect was negative with the sensitivity of the sensors.
The sensor response defined by S = 100% × (I − I0 )/I0 , where
I0 is the current measured under the flowing of N2 and I is that
under NH3 , was also examined by varying the ammonia concen-
tration. Fig. 7(b) shows the response values measured at Va = 5 V,
which are close to the condition for the maximum response of
the sensors. The comparison reveals that: (i) the lower-quality or
defective CNTs (900 ◦ C CNTs) have a larger response and (ii)
oxygen adsorption on CNT degrades the response. The obser-
vation suggests that the favorable gas adsorption sites are not
the perfect honeycomb lattices of the graphene sheet, but can
be the distorted lattices and/or the defective boundaries between
the flaked carbon sheet islands. One can observe that the 900 ◦ C
grown CNTs have more distorted wavy lattice in each flake and
more boundaries between the flakes, as shown by the TEM pic-
tures in Fig. 3. The favorable adsorption onto the defective sites
of the CNT surface was previously proposed [35]. However,
the smaller response of the CNTs having oxygenated defects
suggests that they are less interactive with NH3 than the balanc-
ing gas N2 . Ionescu et al. [35] theoretically and experimentally
showed that NH3 is not sensitive to the defects on CNTs created
by the oxygen plasma treatment, such as vacancies. Therefore,
the oxygenation degrades the response to ammonia, but the
crystallographic defects can enhance it in the CNT ammonia
sensors.
The switching behavior of the 900 ◦ C sensor was further
examined with varying NH3 concentrations in Fig. 8. The almost
complete return to the original resistance at each cycle was
remarkable. While this property is an extremely important ingre-
dient to be possessed by a sensor, such behavior may also suggest
the possible binding status of the molecules. The atomic bind-
ing sites on the CNT surface for ammonia and nitrogen kept
changing because they continuously flowed and washed out the
previously adsorbed molecules. Therefore, the exposure of a
binding site to a particular in-coming molecule was statistically
determined by the partial pressure of each molecule in the flow.
The response of the device measured at different NH3 concen-
trations, as summarized in Fig. 7(b), showed a linear increase
at a concentration higher than ∼1%. The linearity suggests that
the adsorption of ammonia is determined statistically and fur-
Fig. 8. Switching of the 900 ◦ C sensor measured at different NH3 concentra-
tions.
 N.D. Hoa et al. / Sensors and Actuators B 127 (2007) 447–454
ther that the binding energies of ammonia and nitrogen to the
defects are not much different in the investigated range. It also
showed a reasonably good recovery to the initial state, as shown
in Fig. 8. Although the recovery kinetics needs to be explored
more systematically, the observed recovery time not sensitive to
the gas concentration may be due to a forced desorption of the
gas molecules by the refreshing nitrogen flow. The minimum
detectable ammonia concentration was ∼0.1%, which was far
larger than the sensing accuracy of single-wall carbon nanotubes
at ppm level [38]. We tentatively thought that the multi-wall
nature degrades the sensitivity. One can see in Fig. 7(b) that the
adsorption sites on the CNT surface were not saturated up to
6% concentration. It requires further study on selectivity and
stability of the device for real application as a sensor.
As discussed so far, the major merits of the proposed structure
could be drawn from the regularity of the CNTs in terms of
diameter and distribution density as well as its build-up on the
Si wafer using microfabrication technology, rather than high
sensitivity. The regularity of the CNTs in diameter and length
was a great help in clearly defining the senor specification and
in realizing sensor-to-sensor uniformity. The fabrication on a Si
wafer also allowed further development for mass production.
4. Conclusions
A vertical transport type CNT-based ammonia gas sensor
structure and its fabrication process were developed. The struc-
ture features regular arrays of carbon nanotubes of uniform
diameter and length, but it also has high defect levels. It was
realized by using AAO and CNT synthesis without using metal-
lic catalysts. In spite of the geometrical handicap of a vertical
nano channel structure, the sensor revealed a very fast response
and good recovery behaviors due to the high defect density.
The CNTs with a higher defect density revealed better sensitiv-
ity. Nevertheless, the oxygen-related defects are not useful for
ammonia detection from the aspect of sensitivity although the
response time could still be improved by them.
Acknowledgments
This research was conducted with the financial support of the
Center for Nanostructure Materials Technology under the 21st
Century Frontier R&D Program of the Ministry of Science and
Technology, KOSEF Grant No. R01-2004-10104-0, and BK21
program, Korea.
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Biographies
Nguyen Duc Hoa received the degree of master of science in materials sci-
ence at Hanoi University of Technology (HUT), Vietnam in 2003. He is
now in PhD course in materials science and engineering, Chungnam Nat.
Univ., Korea. His research interests are nano-materials fabrication, character-
ization and application to electronic device, gas sensor and biosensor. Contact:
hoa273@yahoo.com.
Nguyen Van Quy received the degree of master of materials science and engi-
neering at Chungnam Nat. Univ., Korea in 2005. He is now in PhD Scholar
course in materials science and engineering, Chungnam Nat. Univ., Korea. His
current interests include fabrication, characterization of carbon nanotube and
its application to nano electronic devices of field emitter and sensor. Contact:
quynguyenh@yahoo.com.
Yousuk Cho received his PhD in materials science and engineering at Chungnam
Nat. Univ., Korea in 2007. He is now at a post doctor in nano materials and
application lab. at Chungnam Nat. Univ. His current interests are functionalizing
of CNTs and its application to field emitter, sensor and solar cell devices. Contact:
yousuk@cnu.ac.kr.
Dojin Kim received his PhD in materials science and engineering at University
of Southern California, USA in 1989. He is a professor of School of Nanotech-
nology and Department of Materials Science and Engineering at Chungnam
Nat. Univ., Korea. His current research interests are carbon nanotube synthesis
and applications to electronic devices of field emitters, solar cells, gas sensors,
etc. Also interested in III–V magnetic semiconductors growth and electrical
characterizations. Contact: dojin@cnu.ac.kr.