Korotcenkov2014 PDF

Accepted Manuscript
Title: Engineering approaches to improvement of

conductometric gas sensor parameters. Part 2: decrease of
dissipated (consumable) power and Improvement stability and
reliability
Author: G. Korotcenkov B.K. Cho
PII: S0925-4005(14)00345-1
DOI: http://dx.doi.org/doi:10.1016/j.snb.2014.03.069
Reference: SNB 16720
To appear in: Sensors and Actuators B
Received date: 18-9-2013
Revised date: 12-2-2014
Accepted date: 19-3-2014
Please cite this article as: G. Korotcenkov, B.K. Cho, Engineering approaches to
improvement of conductometric gas sensor parameters. Part 2: decrease of dissipated
(consumable) power and Improvement stability and reliability, Sensors and Actuators
B: Chemical (2014), http://dx.doi.org/10.1016/j.snb.2014.03.069
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ENGINEERING APPROACHES TO IMPROVEMENT OF

CONDUCTOMETRIC GAS SENSOR PARAMETERS.
PART 2:
DECREASE OF DISSIPATED (CONSUMABLE) POWER
AND IMPROVEMENT STABILITY AND RELIABILITY

G. Korotcenkov
1
, B.K. Cho
1,2

1
Department of Material Science and Engineering, Gwangju Institute of Science and Technology,
Gwangju, 500-712, Korea
3
Department of Nano Biomaterials and Electronics, Gwangju Institute of Science and Technology,

Corresponding authors:

G. Korotcenkov
Tel.: +82-62-715-2354;
Fax: +82-62-715-2304;
E-mail: ghkoro@yahoo.com (G. Korotcenkov).

B.K. Cho
Tel.: +82-62-715-2318;
Fax: +82-62-715-2304;
E-mail: chobk@gist.ac.kr (B.K. Cho).

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ENGINEERING APPROACHES TO IMPROVEMENT OF

CONDUCTOMETRIC GAS SENSOR PARAMETERS.
PART 2:
DECREASE OF DISSIPATED (CONSUMABLE) POWER
AND IMPROVEMENT STABILITY AND RELIABILITY

G. Korotcenkov
1
, B.K. Cho
1,2

1
Department of Material Science and Engineering, Gwangju Institute of Science and Technology,
3
Department of Nano Biomaterials and Electronics, Gwangju Institute of Science and Technology,
Abstract

Engineering approaches designed to improve parameters of conductometric gas sensors are being
considered in this survey. In particular, in this paper we have analyzed engineering approaches used
both for improvement of sensor stability and reliability, and for decrease of power dissipated by
conductometric gas sensors. Analysis has shown that those engineering approaches can eliminate
some genetic disadvantages of conductometric gas sensors, provide a significant improvement of
their exploitation parameters, and expand their application in various fields.

Keywords: Gas sensors; parameters; dissipated power; stability; improvement; engineering
approaches;

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1. Introduction

At present it was published a great number of published review papers devoted to summarizing
results of research focused on optimizing parameters of metal oxides aimed for use in
conductometric gas sensors [1-22]. It was established that essential improvement of conductometric
gas sensor parameters can be achieved using approaches such as (1) searching new materials with
unusual properties [15,20,23-27], (2) optimization of technological routes of gas sensor fabrication
[21,28] (3) design of new technologies of gas sensing materials synthesis and deposition [29-37],
(4) controlling the thickness of the films, the size and the shape of the grains [38-43], (5) using 1D,
hierarchical and hollow metal oxide nanostructures [22,44-46], (6) controlling the porosity of gas
sensing matrix [40,47-50], (7) optimization of the phase composition of the gas sensing layer
[28,39,51-53], (8) design of new methods of surface and postdeposition treatments [36,54-56], and
(9) an increase in the catalytic activity of gas sensing material through introduction of catalytically
active additives, using bulk doping and surface modification [39,51,57-59]. However, despite a
considerable efforts to improve the technology of synthesis, deposition and functionalizing metal
oxide materials, it should be recognized that some problems peculiar to conductometric gas sensors,
such as insufficient response to some specific gases, low selectivity, instability, temporal drift, and
high sensitivity of parameters to the air humidity, are not resolved yet [36,57,59-60].
Studies, conducted during last decades, have shown that existing problems can be partially
resolved through engineering approaches which are not related to the changes in the properties of
gas-sensitive matrix. However, we have to note that so far there are no published reviews,
generalizing results of studies in this area. In present survey, consisting of two parts, we have tried
to overlap this gap. The first part, published recently [61], covers the analysis of engineering
approaches used for improvement of sensor sensitivity and selectivity. In the second part we discuss
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the effectiveness of engineering approaches proposed for the reduction of power consumption and
for improvement of stability and reliability of conductometric gas sensors. The nature of this
instability has been discussed in the reviews [36,60].
One should note that other types of gas sensors can also have problems in terms of
sensitivity, selectivity and stability [20,21]. Therefore, we believe that topics covered by this review
might be of interest for researchers working in the field of another solid state gas sensor design as
well.

2. ENGINEERING APPROACHES TO IMPROVEMENT STABILITY AND
RELIABILITY

Stability is a key quality indicator in the development of gas sensors for real markets. It is known
that devices designed for the sensor market should exhibit a stable and reproducible signal for a
period of at least 23 years (typically 17 00026 000 h of operation). But still, the temporal drift of
operating characteristics of conductometric gas sensors based on metal oxides (MOX), along with
the low selectivity of sensor responses, are considered to be major disadvantages of these devices
[24,62-68]. For example, Fig. 1 shows results of 3 year study of conductivity drift of 6 different
TGS sensors, fabricated by Figaro.
***Figure 1*** near here [63]

It is clear that the sensor aging and environmental disturbances produce changes in sensor
responses that make initial statistical models for gas or odor recognition unacceptable for use after a
relatively short period of time. This means that analytical devices based on such sensors will have
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poor repeatability, since sensors during aging produce different responses for the same odor. That is
particularly troublesome for electronic noses [61]. Besides, such drift substantially limits the ability
to measure the absolute value of target gas concentrations. For example, in the alarm system set for
a specified level of a poisonous contaminant, the drift terms may lead to a false alarm or a failure to
announce a dangerous contamination level. Frequent recalibrations are needed to preserve system
accuracy [65,66]. However, when recalibrations involve numerous samples they become expensive
and laborious.
Gas sensor drift consists of a random temporal variation of the sensor response when it is
exposed to the same analytes under identical conditions. An analysis of current literature allowed us
to conclude that instability in the performance of the MOX conductometric sensor (temporal drift) is
conditioned by a number of reasons listed below [24,41,60,69-77]:
Structural transformation, including grain growth, film cracking, etc..
Phase transformation
Poisoning
Degradation of contacts and heaters
Bulk diffusion, including chemical diffusion of oxygen vacancies
Errors in design
Change of humidity
Variations on flow rate
Fluctuations of temperature in the surrounding atmosphere
System sampling nonspecific adsorption
Interference effects

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All of these factors can modify both the baseline and sensitivity of the sensors in different ways,
depending on sensor technology. Considering factors influencing sensor parameters, one can
conclude that in general sensor drift (temporal instability) can be attributed to two predominant
sources [78-80]. First, the real-drift (so-called, first-order drift) due to the chemical and physical
interaction processes of the chemical analytes, in gas phase, occurring at the sensing film
microstructure, such as aging (e.g. the reorganization of the sensor surface over long periods of
time) and poisoning (e.g., irreversible binding due to external contamination). And second, the
second-order drift (or measurement system drift, among many other names), produced by the
external and uncontrollable alterations of the experimental operating system, including, but not
limited to, changes in the environment (e.g., temperature and humidity variations); measurement
delivery system noise (e.g., tubes condensation, sample conditioning, etc.); and thermal and memory
effects (e.g., hysteresis or remnants of previous gases). We have to note that so far, it is not possible
to fabricate chemical sensors without drift. More detailed discussion of mentioned above reasons of
sensor parameters instability one can find in [36,60,63,81].
One should note that it is impossible to determine the main reason for gas sensor
instabilities, in a general sense; the task is too complicated. In addition, the reasons for instability
could depend on the constructive and/or technological features of the sensor fabrication, or on
temperature modes of exploitation. Therefore, at present there is a great deal of approaches, all of
whichaccording to the authors opinioncan be effective in resolving instability problems in gas
sensors. These approaches can be divided into two main groups. In the first group, an improvement
of gas sensor operation is achieved by searching for new gas sensing materials and optimization of
sensors manufacturing process. While in the second group the improvement is attained by
optimizing the sensors exploitation process, for example several solutions are based on periodically
changing the sensor working temperature [82,83]. However, this general treatment only constitutes
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one facet of the problemthe so-called short-term drifta substantial study of the sensor
variability over longer periods of time is also necessary.
Taking into account directivity of our review, let us consider approaches which are
promising for resolving problem of sensor instability and are not connected with material
engineering. Analysis of main approaches to sensor parameter stabilization based on material
engineering one can find in recently published review by Korotcenkov and Cho [36,60].

2.1. Correct gas system components

In [60] it was indicated that mistakes in design of both sensor package and measurement unit can
also be responsible for instability of sensor parameters. Wrong choice of materials, i.e. the use of
materials prone to outgassing during operation, can lead to a change in the composition of the
controlled gas atmosphere or poisoning of the sensor. This means that the materials utilized to
package the sensor and materials used to build gas systems have to be selected with care to avoid
unexpected pollution of an initially clean gas mixture, i.e. these materials cannot emit gaseous
components or be permeable for gases and vapors during sensor operation [84]. Moreover, these
materials have to be inert in relation to the atmosphere and conditions in which the sensor will
operate. Thus, the material choice should include the selection of materials which are low
outgassing and chemically compatible with the gas mixture. At that these principles should be used
to assemble, not only the final gas mixer, but also any system supplying gas during gas sensor
exploitation [85]. Results presented in Fig. 2 show the importance of this requirement. This Figure
shows the response of an X-ray irradiated ATLAS transition radiation tracker (TRT) straw tube
operated in a clean gas system supplying Ar-CF4-CO2 [63-10-27]. The ATLAS TRT is one of the
three subsystems constituting the ATLAS Inner Detector installed in CERN: it combines charged-
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particle track reconstruction with electron-identification capability. This detector senses formation
of ion pairs in the gas due to passage of charge particles or interaction of photons. When a standard
flow meter, constructed with a lubricated valve and few greasy Viton O-rings, is inserted in the gas
stream after about 70 hours of continuous irradiation, the gain of the straw falls very fast due to
immediate polymerization processes triggered by released pollutants. Other complex components,
such as valves and cylinder pressure regulators are also potential polluting sources. Components
used for ultra high purity applications are usually assembled following strict cleanliness
requirements. However, a careful selection of joints still has to be made in terms of gas
compatibility and outgassing [85].

Table 1 shows the results of some outgassing tests carried out for materials that can be used
to assemble gaseous detectors and gas systems. A list of low outgassing assembly materials exists
and includes epoxy compounds, rigid materials, sealants, elastomers, etc. The effect of materials
that outgas at the ppm level has to be tested for each particular case. That is the case for materials
such as Viton, Teflon, Polyurethane, etc. Viton, one of the most common materials, has shown some
outgassing at the ppm level, though it has been satisfactorily used in very clean gas systems.
Capeans [85] believes that in general, there is no good or bad material. A material is adequate or not
for a very particular type of gas detector and conditions of use. Existing data, obtained either from
systematic outgassing studies or experience gained with detectors, has only a pre-selective character
that can help designing a gas detector before carrying out more time-consuming tests. It seems, on
the other hand, rather universal that silicone compounds that easily migrate (lubricant-type) should
be meticulously avoided, especially with some gas mixtures. One should note that the sources of
silicone contamination are enormous and hard to find.
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***Table 1*** near here [85]

Plastic piping is often used because of its insulating properties, elasticity, low density and
price as compared with the reliable, electropolished, stainless steel pipes. In order to obtain the
desired physical characteristics, these complex materials are frequently modified chemically or with
additives. As a result, they are often made more susceptible to outgassing.
Plastics are also not gas-tight, since gases are able to diffuse through the walls of tubing and
containers made of plastic [85,86]. Calculations carried out by Kjeldsen [86] have shown that
diffusion of oxygen through plastic can be a serious problem for a number of plastic materials.
Permeation data for several polymers used in gas sensing system are summarized in Table 2.
Therefore, the use of some plastic materials, particularly silicone rubber, in experimental and
sampling equipment should be prohibited by gas and water vapor diffusion. Because stainless steel
and glass are inert substances, sampling equipment made of these materials should be preferentially
selected over equipment made of other materials [87]. However, at test laboratories, nylon piping
can be used, for instance, as a clean and simple way of adding a small concentration of water to the
gas mixture, due to the natural outgassing of water from or diffusion through the tube walls.
***Table 2*** near here [88-93]
It is necessary to take into account that incorrect installation of gas sensor can also lead to
instability of sensor parameters. For example, one should avoid installing sensors too close to walls
or floors. These surfaces can absorb and emit gases with changes in temperature, affecting the
reading of the sensor. Care should also be taken to avoid blockages in the sampling line. These can
be caused by particulates, water condensation, or liquids with high boiling points. To minimize this
effect, a filter may be needed to remove particulates and a trap to remove entrained liquid. It may
also be necessary to heat the sampling line.
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2.2. Drift compensation
As we mentioned before, structural and phase transformations, poisoning, interference effects, air
humidity and temperature variations, surface and bulk properties changes are the main reasons of
sensor parameters drift [60]. Mechanisms of these factors influence on gas sensor parameters were
discussed in Refs. [2,36,39,40,60,94-99]. Information related to air humidity influence on gas sensor
parameters can be found in Refs. [41,100-113].
One can assume that the drift compensation using additional processing algorithms, which
account for observed drift lows, is the simplest way to improve stability of sensor parameters.
Algorithms to mitigate the negative effect of gas sensor drift are not new in the field; the first
attempt to tackle this problem dates back to the early 90s [114]. Nevertheless, the study of sensor
drift is still a challenging task for the gas sensor community. A description of several approaches,
pertaining to drift compensation can be found in Refs. [77,80,114-123]. They are signal pre-
processing (response variable including the base line signal), univariate (one single sensor) or
multivariate (multiple sensors), linear or non-linear, adaptive or not, based in reference samples or
based in component removal. For these methods Di Carlo and Falasconi [77] proposed the
classification shown in Fig. 3. The main steps and concepts of the proposed drift correction process
are summarized in Fig. 4.

In particular, the signal pre-processing considers as useful response the difference between
the base line, obtained by presenting the sensor array to pure reference air, and the signal obtained
after stabilization in the polluted atmosphere. However, such solution requires cycling operation
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between reference air and tainted air, which is not convenient for on-site applications. That requires
carrying in the field heavy gas cylinders. Alternatively, generating the reference air by a simple
filtering of the ambient atmosphere produces only partial drift compensation and a lack of purity of
the reference gas, increasing the data dispersion. Drift counteraction algorithms could be applied
either for each individual sensor or for the whole pattern correction, using multivariate methods.
Univariate methods based on baseline manipulation are simple and widely used in the
industry [120]. For the univariate correction, a multiplicative correction factor q(t) is used. This
factor is determined on etalon measurements, at regular intervals within the real atmosphere
measurement or based on a regression model [124]. The continuous temporal signal variation of the
calibration gas is considered to determine a correction factor that is multiplied by the sensor
response Y(t) on the real atmosphere:

Y
corrected
= Y(t)q(t) with (1)

where Y
Std
(t
0
), sensor signal in standard gas at time 0 and Y
Std
(t), sensor signal in standard gas at
time t with t inferior to t. These methods, however, do not take profit of correlated drift effects.
For this purpose, other multivariate methods have been proposed.
Multivariate methods capture more complex or non-linear drift effects using the information
from several sensors in order to model the drift, at the cost of increasing the number of the
parameters involved in the correction [125]. The multivariate methods also require prior calibration
gas measurements. After this step, the main direction of the drift is determined in the first
component space of the multivariate method, such as the principal component analysis (PCA), or by
selecting time as a dependant variable of a partial least square regression (PLS). The drift
component (s) can then be removed from the sample gas data, correcting thus the final score plot of
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the multivariate method [126]. Different multivariate methods can be found in the literature [125-
127] Most of the methods are linear, which allows capturing the most drift variance component, but
more complex non-linear approaches have also been reported [128].
We need to note that different teams have different opinions about optimal approaches to
drift compensation. Every paper tends to show good results related to the newly proposed approach.
For example, Romain and Nicolas [63] believe that a univariate sensor correction gives the best
results for complex data like off-odours measurements, while adaptive models, such as multiple
self-organizing maps, are not well adapted for sensor replacement [129,130]. However, according to
Di Carlo and Falasconi [77], univariate calibration methods, like a multiplicative drift correction
(MDC), are first-order approximations that do not exploit sensor cross-correlations. Empirically
they provided good performance. However, they have several intrinsic limitations. The most
important limitation is that the MDC method assumes that the relative percentage (increase or
decrease) of the sensor response due to the drift is the same for the reference samples and test
samples. This can be true for sample chemical compositions and concentrations very close to the
reference gas but not otherwise. Therefore the amount of drift may be different for different samples,
i.e., the drift for the reference gas and some samples is not same. The consequence of this is that the
sensor drift does not have to be the multiplicative factor estimated from the reference gas, which the
MDC method assumes. In addition it should be noted that in many reported researches,
measurements are collected during few days, thus neglecting long term drift effects, or drift was
simulated. Signal preprocessing techniques seem attractive for their simplicity, but cannot be
considered an effective drift correction approach for gas sensors. More detailed comparison of
methods used for drift correction one can find in a review prepared by Di Carlo and Falasconi [77].
An important assumption for drift compensation methods in chemical sensor signal
processing, however, is that the drift observed in the data is considered to have a preferable
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direction, rather than a random distribution (according to the definition of drift) [118]. Therefore, in
spite of the presence of great number of methods, there is still a need for a simple method that can
compensate for both short time drift throughout a measurement sequence and long-term drift (days,
months) and that does not need time consuming and complex learning processes for a calibration
procedure. We need to note that the presence of hysteresis effects [102,131] makes the design of
such method more complicated.
Yamazoe [132] believes that once we have more detailed knowledge on the drift of MOX
characteristics that could be accounted for by using available electronics algorithms, sensor-based
gas analyzers would find a new market in various application fields. However, this approach
requires the ability to perfectly reproduce fabricated sensors. For example, Romain and Nicolas [63]
studied long term stability of metal oxide-based Figaro-type gas sensors and found that the same
TGS sensors placed in the same operating conditions do not have the same behaviour. Two identical
sensors (same label) with the same history have different time stability. Fig. 5 illustrates this
observation for two TGS 2620. This means that the replacement of an old or broken sensor by a new
one, corresponds to having a new e-nose that requires new models of classification and
quantification.

In addition, realizing the control of humidity and surrounding temperature seems to be
necessary for this approach under current sensor tests (see for example Fig. 6). Only in this case a
mathematical model, which could minimize the influence of humidity and temperature, can be
designed and used [133-135]. Examples of such approach realization when temperature, gas and
humidity sensors were fabricated on the same platform one can find in Refs. [111,136]. Experience
has shown that the use of Pt resistor (read Section 2.4) and capacitive sensor are the most successful
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solution for temperature and humidity control, correspondingly. Detailed description of humidity
sensors, which could be incorporated in measurement device together with gas sensors, one can find
in reviews [137-142].
***Figure 6 *** near here [135]

2.3. Incorporation of filters

Building additional filters is other approach which could provide the improvement stability of
sensor parameters [143]. Additional filters could be employed to protect the sensor surface from
contamination, although they not only influence metal oxide surface properties, but could also
provoke an electrical short circuit [143].
The presence of catalytically active filters could also reduce parameter instabilities
connected to interference effects. Unfortunately, metal oxide gas sensors, including SnO
2
-based
devices, are highly sensitive to volatile organic compounds (VOCs) like long chain hydrocarbons,
alcohols or ethyl acetate. Therefore various standard of sensor using require negligible interference
in cross-sensitivity tests of gas sensors [144]. In particular, this approach is widely used in CO
sensors at present. For example, the concept of filtering upstream is now used for different
commercial CO sensors, where charcoal is used to avoid the interfering effects of HC and alcohols
[144,145]. Of course, the efficiency of such approach depends on the thickness of the filters. For
example, charcoal filters with a diameter of 8 mm and a thickness of 10 mm were found to be
sufficient for preventing a false alarm by interfering gases within the required exposure time of 2 h
[144]. Smaller filter thickness led to a breakthrough of the test gases already during this time.
Unacceptable breakthrough occurs during the exposure to filters below 4 mm thickness: after gas
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exposition, a chromatographic breakthrough of the filter caused a shift of the sensor base line and
later on false alarm.
Kitsukawa et al. [145] have shown that Nafion-based filter specially prepared can also be
used in CO sensors to eliminate alcohol interference. In particular, Fig. 7 shows the responses of the
carbon monoxide sensor with Nafion filter exposed repeatedly to 1000 ppm ethanol and air. The
output of sensor without Nafion (curve 1) corresponded correctly to ethanol exposure. However,
with Nafion (curve 2), the response to ethanol exposure was reduced to zero, and no effect of
ethanol was observed. Other catalysts such as SiO
2
-Al
2
O
3
, zeolites and -Al
2
O
3
have elimination
effect considerably smaller. Fig. 8 shows the dependence of elimination rate on ethanol
concentration for various catalysts. The elimination rate (R
e
) is defined by R
e
=(C
0
-C
a
)/C
0
(where,
C
0
denotes the initial concentration of ethanol and Ca denotes the apparent concentration of ethanol).
In the case of superbase (i.e., barium oxide and calcium oxide), no effect of elimination was
observed. Zeolitic materials and Pt porous films can also be used for these purposes [146,147].
Some aspects of filters using for mentioned above purposes were discussed earlier in Part 1 of our
review [61]. As filters that promote an improvement of exploitation sensor parameters, one can
consider dehumidifiers, which decrease the content of water vapor in a measurement camera, as
well as decrease the influence of humidity on sensor parameters. Sample drying in fixed gas
detection systems can be achieved by cooling the gas down below its dew point.

However, it is necessary to note that the lifetime of filters is limited, and therefore, in the
absence of control for their conditions, changes in their filtering capacities could be a reason for the
observed drift in sensor characteristics. For example, Schweizer-Berberich et al. [144] established
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that charcoal filters with a thickness of 10 mm were effective only during 2 hours. This means that
after 2 hours of operation the filter should be reactivated. In addition, the adsorption capacity of
filters is often decreased with temperature [144]. In particular, at temperature of 50
o
C the adsorption
capacity of the charcoal filter is reduced by 20%30% compared to the capacity at 15
o
C [144] (see
Fig. 9). Thus, the filter sorption capacity becomes dependent on both the surrounding temperature
and the heater temperature. In this regard, it is necessary to know that filters with larger surfaces
have longer lifetimes. Taking all these considerations into account, one should carefully interpret
any results pertaining to improvement of the temporal stability of sensor parameters, especially at
the expense of adding filtering layers to the gas-sensing layer [148]. Most of the results stated here
were obtained in clean lab conditions, and therefore it is unknown how these filtersespecially
ones with small pore sizeswould behave in a highly polluted atmosphere, and how long time the
improvement of sensor characteristics will be.

2.4. Temperature stabilization

As it was shown in previous Sections, the temperature variation of ambient air also contributes to a
temporal instability of sensors parameters [149,150]. As it is known, ambient temperature during the
year can change in a very wide range. For example, in North Europe ambient temperature during the
year can range from -30
o
C to +30
o
C. At a constant microheater power, the variation of the ambient
temperature causes fluctuations in the operating temperature, and as result, fluctuations in
parameters of sensing material take place (see Fig. 10). For example, in the summer, high
temperature cause the stationary increased operating temperature of gas sensors, while in the winter
an opposite tendency prevails. These temperature changes affect both the concentration of the
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charge carriers within the grains of the oxide semiconductor and the average thermal energy of the
carriers which are to overcome the potential barriers, which present at the grain boundaries.

The kinetics of the gas-surface interactions are also strongly temperature dependent
[109,151], and therefore a small changes in T
oper
of course can be accompanied by instability of
sensor output signal. This means that temperature stabilization is one of the requests to
measurement device used for gas concentration measurement [149].
Undoubtedly, for this purpose one can use the stabilization of the temperature of the whole
measurement cell. However, this approach is energetically cost-is-no-object one. The resistance of
Pt heater can also be used for temperature control. For example, in most commercial gas sensors,
the change in heater resistance with temperature is used to determine the temperature of the heater
itself. However, it can be difficult to measure accurately small changes in resistance when applying
high currents to the heater particularly when it is being driven in a pulse mode. It was established
that modern approaches based on the incorporation of a temperature sensor in the gas sensor are
more attractive and effective [152,153]. Experience has shown that often designers prefer to use a
separate temperature sensor rather than relying on the heater itself, as it allows for an optimized
sensor design and gives flexibility in designing interface circuitry without disturbing the heater
drive. For example, Gong et al. [149] have shown that a built-in platinum temperature sensor can
precisely detect the sensor's working temperature and provide feedback information for controlling
microheater's current necessary to maintain the sensor's working temperature constant, regardless of
ambient temperature change. As a result, Gong et al. [149] achieved significant improvement of gas
sensor stability in comparison with gas sensors operated without temperature compensation under
the same ambient variation.
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It was found that thin film technology, especially in micromachining design, and modern
electronics give great opportunities for the implementation of this approach. Temperature sensors
might be fabricated by number of microelectronic protocols under single-sided or double-sided
design. Usually, either a silicon resistor or a silicon diode is embedded in the heater area and used to
measure the temperature of the sensing element. A temperature sensitive bipolar transistor (diode-
connected bipolar transistor) is possible up to 125
o
C as well [154]. Later work by Santra et al. [155]
has shown that a silicon diode temperature sensor can be used reliably up to very high temperatures
of 550
o
C, by employing SOI rather than standard bulk or epi CMOS technology, together with high
temperature metallization. A temperature sensors can also be made from a metal but they require
higher currents, due to their low resistivities (which can cause long-term stability issues because of
electromigration). The example of the double-sided sensor with incorporated resistive temperature
sensor is drawn in the Figure 11. Such configuration was proposed by Miller et al. [156].

A popular principle [157,158] of temperature sensors incorporation in integrated gas
sensors is to have one temperature sensor on a thin membrane (where the heater is embedded) and
an identical sensor off the membrane (to offset changes in room temperature and any nonidealities
of the temperature sensor). The signal from a temperature sensor is often amplified using an
instrumentation amplifier (IA). The instrumentation amplifier will therefore amplify the difference
of signals coming from these two temperature sensors. Also, the IA can have gain control and offset
adjustment from outside the chip.
However, it is necessary to take into account that incorporation of a temperature sensor will
add both complexity and costs of gas sensors. The calibration of temperature sensors needed to
obtain good accuracy will also incur additional costs.
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2.5. Exploitation mode optimization

It is known that water molecules, presented in the humid air, electronically interact with metal oxide
surface upon chemisorption and cause changes in both resistance and sensor response [100-
113,159]. Essentially, instability via the influence of air humidity can be decreased at the expense of
increasing the working temperature [107]. For example, at T
oper
> 400 C the role of water in gas
sensing is considerably decreased; this approach was used while characterizing Ga
2
O
3
-based gas
sensors [160] and SnO
2
-based sensors [107] (see Fig. 12)]. Due to the high working temperatures
(T
oper
> 500
C) good stability was also attained in a sulfur-containing atmosphere [160]. But while
deciding to use high operating temperatures it is necessary to take into account that the application
of this method is accompanied by tradeoffsan increase in power consumption and a drop in both
contact and heater reliabilitynotably undesirable for devices designed for long-term operation.

Periodic reactivation of MOX is other approach which can give the improvement of sensor
stability [62,161]. For instance, the conventional operating temperature of most conductometric gas
sensors is not high enough to completely burn organic deposits or to desorb certain adsorbates that
inhibit the adsorption of oxygen and the target gas, and consequently leads to long-term instability
over time. As such, a periodic cleaning performed at high temperature in an oxygen-containing
atmosphere can restore the initial properties of the MOX surface. For example, depending on the
oxidation conditions, i.e., the oxygen partial pressure, most sulfur can be removed between 150 and
300 C, with only a small portion remaining up to 500
o
C, whereas various types of carbon are
eliminated between 250 and 550
o
C [162]. Regeneration can also convert a sulfide phase, which
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could have partially sintered, back to an oxide phase quite similar to the original one of the fresh
catalyst. Annealing can also promote the restoration of Pd cluster catalytic activity, which at low
temperature could drop due to poisoning by CO molecules [163]; this effect was also observed for
SnO
2
Pt sensors [164]. Wurzinger and Reinhardt [164] found that treatment in air at 750
o
C was
accompanied by a full regeneration of the sensor characteristics, independent of the sintering
temperature of the active layer. As such, it is recommended that regeneration operations be
performed at a temperature high enough for C, S, and other poisoning elements to be removed, but
low enough to avoid damaging the sensing layer and supporting platform.
Using this criterion, one can conclude that the operating window seems to be rather wide,
between about 400 and 750
o
C; however, the reality is not so trivial. When the temperature is well
below 500
o
C, combustion kinetics is usually too low to efficiently oxidize C and S during an
acceptable time. On the other hand, when temperature is well above 500
o
C, even if the surface area
of the metal oxide can in some way be preserved, the noble metal catalysts can be partially sintered
[162].
Impulse heating can be used for water desorption from the surface of metal oxides as well.
This effect is important for low temperature sensors, especially for sensors operated at room
temperatures. In particular, such approach was used by Adamyan et al. [165] during design SnO
2
-
based hydrogen sensors operated at 150
o
C. An example of a simple system that illustrates some of
the principles of temperature-pulsing for water desorption is presented in Fig. 13. This Figure shows
a set of step-shaped drops in conductance as a function of pulse temperature. The conductance G
was measured between pulses, while the sample is at room temperature. It is known that exposure of
the SnO
2
to dose of water increases the conductance. Heating the surface to a high enough
temperature (above 200
o
C) causes desorption of water and a decrease in the room temperature
conductance to the pre-dosed value. A decrease in conductance was observed when the duration and
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height of a pulse are sufficient to cause a significant desorption from the film. So, impulse heating
can be used for sensor regeneration from wetting.

However, during application of impulse mode of operation it is necessary to take into
account that the rapid and frequent change in temperature can cause additional stress in both gas
sensing film and membrane layers which can shorten the life time of a sensors. In particular,
cracking and scaling of gas sensitive layer can be observed.

2.6. Integration of conductometric gas sensors

Another research thrust is the full integration of microfabricated or MEMS-type (Micro
Electro Mechanical Systems) conductometric gas sensors with the managing and signal
conditioning electronics at a single chip [167-172]. The Fig. 14 shows the example of such an
integrated conductometric gas sensor.

There are a multitude of reasons to combine a gas sensor and associated electronics at the
same package. In general, the major goal is getting higher signal/noise ratio, but further issues are
also addressed as impedance matching, elimination of parasitic capacitances, reduction of lead
connections, compensation of cross-sensitivity, excitation control, analog-to-digital conversion, and
standardization of the output levels by means of individual adjustment of the sensor signal. These
issues could be addressed, in particular, with hybrid circuits developed in frames of thick-film
technologies [173,174]. Such integration makes easier and cheaper producing the final gas-
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analytical units or gas alarms. Gardner et al. [153]also believe that there are several mass markets
that could open when the gas sensor (including read-out interface) falls below $10 and many more
when it falls below $1. Once the unit cost falls below $1, then the gas sensor could be embedded
into laptop computers, personal digital assistants (PDAs), cell phones, and even wrist watches.
Therefore, the only way in which the potential mass market can be penetrated is to employ low-cost
manufacturing technologies (i.e., CMOS technology) and integrate the drive and interface circuitry
into a single smart chip. A related success story is that of a low-cost IC humidity sensor, which
incorporates the sensing element with integrated electronics, and sells for around $10
(http://www.sensirion.com/en/00_home/00_home.htm). It has been considered that microfabrication
and cointegration increase the long-term reliability and stability of the final units as well
[153,170,172,175]. Gardner et al. [153] believe also that the intelligent design and integration of the
electronic circuitry (for drive, signal conditioning/compensation, and read-out) with the gas sensing
element can mitigate some of the significant issues inherent in solid-state gas sensors, such as strong
temperature and humidity dependence, signal drift, aging, poisoning, and weak selectivity.
According to Hagleitner et al. [173,176], the microfabrication and integration of
conductometric gas sensors give the following advantages. The microsensors frequently generate
microsignals which could be better processed under monolithic scheme designs (filters,
amplifiers, etc.) directly at the site of generation so that the influence of parasitic and crosstalk
effects is reduced. On-chip analog-to-digital conversion is another feature that helps to generate a
stable sensor output that can be easily transferred to off-chip units. The minute analog signal of
hybrid or discrete microsensors is sometimes very difficult to read out.
The response time of a gas sensor array is, in most cases, determined by the volume and
flow rate through the sensor measurement chamber. The integrated approach makes possible to
employ such packaging techniques, as for example the flip-chip one, which makes the measurement
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chambers to be rather small. Among others, the small chambers allow one to realize some
modulations of the gas flows spatially and temporarily. In addition, if the silicon on insulator (SOI)
technology is used, the performance and design of the microsystems are so improved that allows
producing good sensors which often offset the higher costs of the starting SOI material [175].
However, it should be noted that despite the efforts towards integration of gas sensors, gas
sensors fully integrated in CMOS technology for the detection of almost all gases, is still not
implemented. It was found that in case of monolithic designs of the integrated systems on silicon
microchips developed via CMOS technology, the selection of materials is rather restricted to few
ones which are compatible with the technology routs [153]. For example, heater materials formed
from doped polysilicon and aluminium can have poor long term stability at higher temperatures
temperatures causing heater resistances to increase significantly during use, thus affecting
calibration. Electrode materials formed from aluminium do not make good electrical contact with
gas sensing layers, due to native oxide formation. Many pre- and post-treatments for sensing
material deposition contain highly reactive chemicals that can attack either the CMOS metal, silicon
or even passivation layers. Post-deposition anneals are often close to or above the melting point of
aluminium (660
o
C). The high-temperature processing, for instance, at higher than 400C, can be
detrimental to make the metallization and may alter the semiconductor characteristics.
In addition, prior to sensor fabrication, it is necessary to take into account that this
fabrication requires a complicated technological process and high-cost equipment. In addition, the
packaging of integrated sensors may also be more complicated as there is a need to reduce sensor
interference with the surroundings, minimize electric crosstalk, and optimize the critical
connections. Finally, the integration is not always cheap and may even increase the cost of the final
unit because of additional processing which results in lower yield and more designing efforts.

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2.7. Artificial or forced aging

It is necessary to note that the use of preliminary (accelerated) aging prior to sensor tests is the most
effective method to improve temporal stability of conductometric gas sensors. For example, Itoh et
al. [177] have found that annealing in air at temperatures exceeding their operating temperature, can
reduce the drift of the resistance. Jung et al. [178] also reported that thermal annealing improved the
stability of gallium indium zinc oxide thin film transistors. As it was shown in various papers
[41,179], in the presence of a finely dispersed phase small grains can coalesce during the
exploitation process with bigger grains, initiating structural changes as well as a change in the gas-
sensing properties of the gas-sensing matrix. Preliminary annealing promotes the phase coalescence
at this stage of fabrication, preventing similar changes during the exploitation process. Annealing
also activates other processes that commonly induce a temporal drift in characteristics [180-182].
For example, annealing improved the homogeneity and stabilized the size of noble metal clusters
[180,183]. At that, Zampiceni et al. [183] have shown that short annealing during 1 hour at T=400
o
C
affects the stability of gas sensing parameters in gold-catalyzed samples, while Pt catalyzed sensors
do not show noticeable modification of electrical properties after such aging. In [184] it was shown
that annealing decreased the density of microstrains and dislocations in the film, leading to a
reduction in the concentration of lattice imperfections. In [181], improvements in stability were
ascribed to the reduction of trap sites in the metal oxide layer.
Thus, mentioned above results testify that additional annealing of a sufficiently long period
promotes the stabilization of sensor properties [182]. Results presented by Papadopoulos et al. [185]
confirm this conclusion. Based on tests of In
2
O
3
- and SnO
2
-based sensors, fabricated using
sputtering technology, it was established that if devices were not exposed to a preliminary aging,
sensors only become stable after 100150 measurement cycles, including heating up to 450
C.
According to results obtained by Adamyan et al. [186], the stabilization of parameters of SnO
2
-based
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hydrogen sensors takes place after five days of continuous working at the 150
o
C operation temperature
under 5000 ppm hydrogen containing atmosphere (see Fig. 15). In [181] the duration of post-thermal
annealing was established to be about 65 h at 250
o
C. An important requirement of such thermal
treatments is that annealing temperatures have to be higher than the operating temperature; also, it
should be noted that this method is the easiest and most efficient for improving sensor stability.
Nelli et al. [187] have found that for achieving stable parameters the aging of the SnO
2
-Au-based
gas sensors at T=400
o
C should be at least during 20 days. At that this duration depends on the gas
surrounding atmosphere (see Fig. 16). In [146], the sensors were aged for several weeks on a
laboratory test bench prior to use. Of course, the artificial aging of sensors makes the technological
process of their fabrication longer, because it often includes several long annealing periods in
different atmospheres at various temperatures [186]. But the instability problem for such aged
sensors is not as strong as for as-fabricated devices. Therefore, in many cases the appearance of
temporal instability of sensor parameters is considered to be a consequence of the insufficient
treatment of samples prior to sensor exploitation, in terms of temperature and duration. No doubt, it
should be noted that this may be an overly simplified view of the instability problem, because
annealing by itself cannot exclude all factors influencing the stability of gas sensor characteristics.

Preliminary high-temperature annealing of an as-synthesized powder before forming gas
sensitive layer by thick-film or ceramic technologies can also be seen as a kind of artificial aging.
As is known, sufficient stabilization of gas sensing material is not always possible at substrate
compatible temperatures. Usually the temperature used for annealing of the films deposited on gas
sensing platforms, due to their constructional and technological limitations, does not exceed 400
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600
o
C. Whereas for full crystallization and the removal of tensions in the crystallites, as was
indicated previously, the annealing at temperatures exceeding 700
o
C is required (see Fig. 17) [188-
190]. According to Hillhouse et al. [191], for extremely high thermal stability of structural
parameters it is desirable to carry out the annealing at T > 1000
o
C. The same result was reported by
Lee et al. [192]. It was established that additional annealing as-synthesized powders at T
an
~ 1000
o
C
for 10 h before forming a gas sensing layer using methods of thick film technology considerably
improved their thermal and temporal stability. Kocemba and Rynkowski [193] also used high-
temperature calcinations of as-synthesized SnO
2
powders and found that this treatment increased the
response of SnO
2
:Pt-based sensors to CO and H
2
, in spite of the increase of the grain size and the
decrease of catalytic activity of metal oxides used. Thus, from the present short analysis one can
conclude that the use of high-temperature annealing of the metal-oxide powders at a stage prior to
the formation of the gas sensing layer can really be an effective method for the improvement of
sensor parameters.
***Figure 17*** near here [189, 190]

2.8. The use of 1D structures
At present, the use of individual 1D nanostructures for gas sensor design is considered as one of the
most promising approaches to develop a new generation of gas sensors with improved stability and
reduced temporal drift of the parameters in comparison with conventional devices [194-198].
However, we have to note that a review of the literature data has show that the above statement has
not been proved by a detailed analysis of the experimental results. Of course, one should admit that
some processes, responsible for instability of polycrystalline materials, are impossible in individual
nanowires. One-dimensional structures are single crystals with perfect crystallinity and a well-
defined geometry; they have clear faceting with a fixed set of planes [195,199]. Sensors constructed
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on the base of individual 1D nanostructures do not contain interfaces or grain boundaries, and
therefore the operation of such devices is not accompanied by any mass transfer, which could
promote structural changes in sensors, as is the case of sensors designed on the base of
polycrystalline materials. It is for this reason that one can expect the improvement of thermal and
therefore, temporal stability of device parameters using a base concept, in comparison with devices
fabricated on a base of nanoparticles. Therefore, recent research has been carried out in many
laboratories to synthesize and characterize NWs and to explore their to integration in proof-of-
concept gas sensors [196-198,200-203]. Some examples of gas sensor prototypes developed with
single NWs are shown in Fig. 18.
***Figure 18*** near here [203,204]

These studies confirmed that 1-D-based sensors operating at low temperatures have better
temporal stability in comparison with standard nanostructured devices [196-198] (see Fig. 19).
However, all those statements regarding experimental confirmation of the high stability of sensors
on a base of 1-D structures relate to sensors designed on the base of nanowires with characteristic
sizes exceed 2030 nm. For comparison we should note that in sensors designed on the base of
polycrystalline materials, where the problems of thermal and temporal stability are relevant, the
grain size does not exceed 510 nm. For example, results presented in Fig. 19 were obtained for
nanowires with diameter 200-900 nm and nanograins with diameter ~ 4 nm. Unfortunately, at
present nobody wants to work with individual nanowires with a size less than 2030 nm
[196,197,205207]. Separation and manipulation of such small objects is too difficult [196]. Besides
that, there are technological difficulties with the growth of such thin nanowires (d < 10 nm) with
bigger length. Low temperatures are necessary for the growth of such nanowires. But in this case the
length of nanowires will be insufficient for the creation of a bridge between two bonding pads on
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the measurement platform [207]. As a result, at present the response of sensors fabricated on a base
of single nanowires with d > 3050 nm is considerably smaller than the response of conventional
sensors designed on a base of nanocrystallites with the grain size less than 10 nm [197,206,208].
Comparable results on conductivity response were obtained only for nanowires with a modulated
diameter [209] (see Fig. 20), or for a network of nanowires, where like in the ceramics-based sensor
the functionality is controlled by inter-nanowire interfaces [194,205,209].

Of course, in the future, attempts to increase the response of 1-D structures-based gas
sensors by reducing the diameter of the nanowires will be made. However, in this case, we must be
ready to the fact that if one is able to fabricate sensors based on nanowires with a diameter of less
than 10-20 nm, it is quite possible that we are also be faced with the problem of reduced stability of
these devices. For example, studies carried out on the basis of metal and semiconductor nanowires
have shown that 1-D structures in the range of sizes of 10-20 nm are also unstable [210-215]. With a
decrease in the diameter of nanowires their melting temperature drops sharply, the same as it does in
the case of nanocrystallites. It has been established that the significant decrease of the melting point
takes place accordingly to the theory established for nanoparticles, i.e. is inversely proportional to
the diameter of nanowires [216]. For example, for a spherical nanoparticle, the melting temperature
is given by [217]

(2 )

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where T
m,
is the bulk melting temperature (K) and H
m,
is the melting enthalpy (J m
3
), whereas
l
and s are the surface tensions in the liquid and solid phases (J m
2
), respectively. For structures
with lower symmetry shapes such as non-spherical nanoparticles (NPs), nanowires (NWs) and
nanotubes (NTs) this equation can be presents as

(3)

where the shape parameter
shape
is dened as , where A and V are the surface
area (m
2
) and volume (m
3
), respectively, for a given shape, and L is the smallest dimension of the
structure.
Moreover, it was shown that this effect takes place for all types of nanowires, including
semiconductor nanowires, and especially for nanotubes. Experiment has shown that a considerable
drop of melting temperature of semiconductor nanowires could be observed for noticeably larger
diameters of nanowires, than was established for metal and metal-oxide nanoparticles. For example,
the melting of a Ge nanowire with a diameter of 55 nm starts at around 650
o
C, while the melting
point of bulk Ge is 930
o
C [210].
Due to the ability to cut, link and welding nanowires at relatively low temperature, we need
to recognize that the thermal stability of the devices designed on a base of 1-D nanowires may also
be limited, and this limitation should be taken into account when analyzing the prospects of the
development of nanoscale electronics. For example, Guisbiers and Pereira [215] basing on
theoretical simulations predicted that the use of ZnO nanotubes in electronics is restricted to sizes
above 10 nm, since for smaller dimensions the energy dissipation of the circuit can raise the
operating temperature close to T
m
. For devices, operating at higher temperatures (see Fig. 21),
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which is typical for conductometric metal-oxide sensors, such a working environment is

unacceptable.
***Figure 21 near here*** [215]

The creation of a reliable low-resistance electric contact with such thin nanowires is also an
essential problem [196,218], and that problems associated with sensor parameter instability incurred
by contact instability still remain. Moreover, the reduced contact area between metal electrodes and
NWs magnifies the contribution of the contact electrical properties and may hide the phenomena
which take place on the surface of NWs [197,219-222]. Instability connected to the mobility of
surface clusters could also be sufficiently increased, because 1D structures do not contain edges and
stages, which can serve as particle pinning centers that hinder the diffusion of noble metal clusters
on the surface of metal oxide supports. In addition, in a network of nanowires [205], which are often
being considered as an alternative to polycrystalline materials for fabricating metal-oxide sensors,
processes responsible for instability of polycrystalline materials are possible, and the consequences
of these processes should be the same as in case of nanoparticles. As it is also known, nanowires
have dispersion in their diameter.
Note also that the use of 1D structures does not exclude the influence of other factors, such
as humidity, poisoning, and so on. The SnO
2
nanowire responses, measured as resistance variation,
follow a logarithmic behavior such as it is shown in Fig. 22. Although the observed influence of
humidity on the characteristics of 1D structure-based sensors is considerably lower than in the case
of nanocrystalline sensors [218]. This behavior could be connected to the size of nanocrystalline
materials, but not generally to the structure of the gas-sensing material [36]. If the 1D structures
usually have a diameter exceeding 3050 nm, in nanocrystalline sensors the grain size could be in
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the range of 515 nm; as mentioned above, nanocrystalline metal oxides with their smaller grain
size are subjected to a stronger influence of water vapor [41].

One can expect that for nanowires, in comparison to nanocrystallites, the influence of effects
such as surface diffusion of electrode material along nanowires and migration of surface clusters,
used for surface functionality, could become stronger as well [212]. This diffusion can modify the
surface properties of metal oxides and make a contribution to the temporal instability of sensors
parameters. In comparison with polycrystalline materials nanowires do not have any steps and edges,
which could restrain surface diffusion. At present this question has not been studied yet, because the
majority of sensors designed on a base of nanowires are being tested at room temperature. But so far
as the working temperatures of sensors will increase, the importance of the above processes of
surface diffusion could well increase, especially under conditions of a temporal gradient, which is
constantly presented in the case of metal-oxide resistive sensors.
Thus, the above discussion gives credence to the view that the problems of thermal stability
will be peculiar to 1-D structure. Whilst, the laws of physics are universal one can only hope that
these problems will be not as strong as for polycrystalline materials. Based on arguments so far
presented one can conclude that the prospects of 1-D structures fabricated for use in connection with
sensors intended for work at higher temperatures (such as conductometric gas sensors) should be
considered more realistically.
In addition we need to take into account that the controlled separation, manipulation, and
characterization of individual NWs are not straightforward processes due to the intrinsic problems
of working at the nanoscale. These procedures are complex and require well-established
methodologies which are not yet fully developed. Several promising techniques, however, have
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been reported to align or orientate NW assemblies with the help of microfluidics, electrostatic or
magnetic fields, surface prepatterning, self-assembly, and templating. These architecture principles,
which have made it possible to design prototype devices, have been comprehensively reviewed
recently [223-226]. All these fabrication routes, however, are still in a preliminary stage of
development. Thus, the use of NWs in real devices needs a breakthrough in order to integrate them
with low-cost industrial processes [203].

2.9. Other approaches

Of course, in addition to the above mentioned approaches used to improve the stability of the
parameters of sensors, there are probably other effective approaches, which, however, are not
reflected in our survey. For example, in a recently published paper we have found an interesting
approach proposed by Ishikawa and Hara [227]. They proposed planar gas sensors operating in a
perpendicular current mode.
It is known that cracking in sensing layer is one of the reasons of instability and lack of
reproducibility in gas sensors parameters. In case of the film cracking the electroconductivity and
gas-permeability of the film could change fundamentally, depending on the depth and length of the
cracks. Illustration of cracking effect is shown in Fig. 23. For example, resistance of the film could
increase strongly due to the break in the conductivity networks, while both response and recovery
times in such sensors could decrease due to improvement of gas-permeability of these films.
However, it is necessary to take into account that the process of cracking is hard to control. This
effect was observed for all metal oxides and was particularly strong in the thick-film and ceramic
sensors [228-233]. These micro-cracks are usually generated perpendicular to the surface of the
sensing film by the shrinkage associated with the sintering of the film during the high-temperature
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annealing process. Micro-cracks perpendicular to the surface because the internal stress of the film,
which is parallel to the substrate, is released by developing cracks while the stress, which is
perpendicular to the surface, is released by the shrinkage of the film thickness. Some cracks are also
created by the contraction and expansion caused by the difference of the thermal expansion
coefficients between the sensing film and the substrate during periodic heat cycle. During
exploitation the cracks propagate slowly causing a temporal drift of sensor characteristics [234].
***Figure 23*** near here

Much effort has been devoted to the reduction of cracking effect. For decreasing micro-
cracks Tang et al. [228] and Sharma et al. [230] have proposed to use some additives to sensing
films, for example Cu to a SnO
2
film. Yu et al. [229] have shown that patterning of the sensing film
as narrow strips also effectively decreases micro-cracks. Adoption of double-layered structure has
also been effective in reducing the effects of micro-cracks in an upper sensing layer made of SnO
2
-
based or WO
3
-based films, which were deposited on a lower conducting layer made of Fe
2
O
3
-based
film [235]. Nagasawa et al. [236] established that the formation of a thin-film with a columnar
texture by controlling the ambient atmosphere during film deposition successfully diminishes the
internal stress and thus stress-induced microcracks. Optimization of the substrate temperature during
film deposition has also been proved to be effective in decreasing microcracks [231]. Smoothing the
underlying surface roughness has been shown to reduce micro-cracks as well [229]. However, we
have to note that mentioned above approaches are more or less dependent on materials. Namely,
these attempts are satisfactory in certain cases with some materials, but they are not in other cases
with different materials.
Ishikawa and Hara [227] have suggested more general approach, which does not depend on
the sensing material used. In particular to avoid the adverse effects of micro-cracks, they proposed
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to use planar gas sensors operating in a perpendicular current mode (see Fig. 24). To achieve this
mode, a porous top electrode is deposited on a sensing film instead of an electrode that is normally
deposited on a substrate. The sensor current flows perpendicular to the substrate surface, i.e. parallel
to the cracks, and thus is not subject to the influence of the micro-cracks. As a result, the resistance
change in time of the sensor was stable compared to a traditional sensor operating in a parallel
current mode.

However, it should be noted that the disadvantages are also inherent in this method. In
particular, it is necessary to provide good gas permeability of top electrode, which can be achieved
only with the use of very thin metal films (Fig. 25). In addition, top electrode can act as a catalyst
for detecting gas inhibiting its interaction with the gas sensing layer.

3. ENGINEERING APPROACHES ALLOWING TO DECREASE
DISSIPATED (CONSUMABLE) POWER

First conductometric gas sensors fabricated using ceramic and thick-film technologies are generally
consumed 1-5 W of electrical power. Of course such a big power required for gas sensor operation
significantly limited their use. Therefore, the minimization of power consumption is one of the main
requirements for sensor technology, especially when the designed devices are aimed for application
in portable systems. In this regard, much of the research conducted in the field of gas sensors were
related to the searching new technologies that improve this parameter of gas sensors.
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A significant reduction in power consumption can be achieved by lowering the operating

temperature. For example, the experiment has shown that the lower operating temperatures can be
achieved by the use of UV irradiation, which was discussed in the Part 1 of our review [61].
However, reducing the operating temperature is usually accompanied by such effects as the growing
influence of air humidity and accelerated poisoning of sensing material. As is known, these effects
are the source of the temporal drift of sensors parameters, which significantly affects their
performance [60].
Calculations showed that the main heat losses in sensing element are associated with such
effects as heat exchange with the air (thermal conduction and convection), radiation and heat loss
through the holder, in particular the thermal conductivity of the wire contacts [237,238]. It is known
that sensors based on suspended miniature chips are the most common approach in the manufacture
of sensors with low power consumption. Thus, the task of reducing the power consumption is
transformed into the problem related to reducing heat losses. The importance of this statement can
be seen from results of computer simulation, which showed that at 500 C almost 2/3 of the heater
power is dissipated in the air. Moreover, modeling of heat losses in the sensor heater with an area of
0.75 mm
2
[239] revealed that for the small crystal mounted in the housing with a volume of about
0.5 cm
3
the heat loss due to convection can be neglected. The same conclusion was made by Kim
and coworkers [237,240]. They stated that when the sensor operates near an unheated surface,
thermal conduction from the sensor chip into the unheated surface dominates over thermal radiation
and convection. According to Kim and King [240], radiative heat loss from the sensor to the
environment is estimated to be only 0.5% of the total heat dissipation in the heater when the sensor
is heated to 300
o
C. This means that thermal radiation is expected to be negligible in heat transfer
modes between the sensor and the surrounding air environment. The sensor must heat to 470
o
C
before the loss due to radiation reaches more than 1% of the overall heat losses. For micron-scale
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devices the role of natural convection is even less. Studies carried out by Xu et al. [241], Guo and Li
[242], Siegel and Howel [243] reported that heat conduction might be a dominant mode in heat
transfer around a microstructure immersed in air, due to the smaller thermal capacitance and the
greater ratio of the surface area to volume than conventional structures. However, for flow-through
systems, the statement seems to be insufficiently convincing.
Experiment and simulation have also shown that thermal loss associated with both heat
exchange with the air, and radiation depends on the chip size. The larger the chip is, the heat loss is
more. For example, according to Vasiliev et al. [238], for the crystal size of 1.5 0.5 mm, the total
heat losses at 450 C are approximately 180 mW. This means that the reduction in the size of gas
sensitive elements is an important trend in the gas sensor design associated with a reduction in
power consumption. For example, simulations carried out by Courbat et al. [244] established that
the decrease of micro-hotplate side length from 100 m to 15 m was accompanied by the decrease
of power consumption by the factor 2. However, this direction also has its limitations, especially
when the thick film technology is used. The relatively large area of such sensor chip, and
consequently, its high power consumption is associated with the necessity to have contact pads for
connection with the wires [245]. The decrease of its size makes the task of connection more difficult
and the binding joint less reliable.
It was found that the losses due to the thermal conductivity of both platinum wires used in
sensors, and substrates being in contact with the housing, also are significant and should be
optimized. For example, according to Vasiliev et al. [238], the heat loss in ceramic sensors due to
the thermal conductivity of platinum wire diameter of 20 m and a length of 3 mm is about 50 mW.
Using a thinner wire reduces heat loss, but the use of the wire with diameter less than 10 m is
almost impossible for gas sensors fabrication because of unacceptable mechanical properties of the
wire.
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It is necessary to note that when the heated sensor operates in an air environment with strong
thermal coupling of its chip with a substrate (holder), the heat flow from the sensor into the holder is
much larger than the heat flow from the sensor chip into the nearby air, and nearly all of the heat
that flows into the nearby air ends up in the substrate [246,247]. In this case, the most efficient
solution is to reduce the thickness and thermal conductivity of the substrate used in gas sensor
fabrication. Increasing the ratio of length to width crystal also has a positive effect [238].
Decrease of the power consumed by sensor can also be achieved by better thermal
insulation, when the part of heat energy is successfully retained [248]. For example, the sensor may
have an additional thermal insulating cover. In particular, Ma et al. [248] offer to use hydrophobic
silica aerogel, which has excellent low thermal conductivity and high gas permeability. Such
covering has also restricting effect on the free airflow near the heated sensor. Ma et al. [248] have
used this approach in the design of pellistor-type methane sensors and achieved a significant power
decrease of approximately 30%. These experimental results strongly indicate that the packaging
thermal insulation enhancement is an alternative approach for power minimization.
Impulse mode of operation, when the sensor operates at optimum (high) operating
temperatures a short period of time, and the remaining time is in waiting (sleep) mode at low
temperatures, is also an effective approach that guarantees a significant decrease in electrical power
of the sensor. This approach we have considered in Part 1 of our review [61]. Vasiliev et al. [249]
reported that if the CH
4
sensor with an optimized membrane consumes about 25 mW during
continuous heating of the sensitive layer, the application of pulsed more gives possibility to reduce
consumed power to about 1 mW. However, we should recognize that sensors operated in pulse
mode do not achieve the same accuracy as in the common mode (constant heat). In addition,
implementing such an approach requires a smart measurement algorithm and recalibration of the
sensors from time to time.
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3.1. Gas sensors microfabrication and its resources

In previous Section we considered various approaches which can be used for decreasing
consumption power of gas sensors. We should note that many of these approaches may be realized
most efficiently in sensors fabricated using micromachining technologies [250-253]. The major
element in sensors fabricated using micromachining technologies is microhotplate produced using
Si technology as shown in the Fig. 26.

Usually the microhotplates are based on suspended membranes configured after etching of
cavities at the Si substrates. The several options of hotplates employed to develop gas sensors are
given in Fig. 27. As one can see from Figs. 27a,b,d, the microhotplates could be configured to
design either a closed membrane (see Fig. 27) or a suspended membrane (Figs. 27a,b,d). However,
in the most cases the micro-hotplates are designed under 3-D concept employing suspended bridges.
So, the heating and sensing element are thermally isolated from the substrate. The suspended
membranes allow one improving a thermal isolation of the functional layers. This design allows one
getting uniform and fast heating of the sensor surface. We need to note that microhotplates make
great demands of membranes. The membrane needs to be very robust to allow metal-oxide
deposition and heating up to high temperatures. The materials chosen for the membrane of the
microhotplate should combine low thermal conductivity, in other words - small thickness, with high
mechanical strength, in other words - large thickness [255]. The first issue is crucial because the
gas-sensing properties of semiconducting MOXs are temperature dependent. The second issue
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requires reliable producing the device, in particular when the sensing layer is deposited and
annealed.
***Figure 27 *** near here [256, 257, 258, 259]

Under original construction developed by NIST (National Institute of Standards and
Technology, USA), the interdigital metal electrodes are patterned over the membrane and covered
by the MOX gas-sensing layer by known microelectronic technologies as sputtering, drop coating,
CVD, PVD, etc. The whole structure is finally stabilized via annealing at high temperatures up to
700
o
C [260]. Possible variants of planar and stack-type structures of gas microsensors developed
with microhotplates and the influence of microhotplate structures on their temperature parameters
are shown in Figs. 28 and 29. Heater and thermometer are integrated usually in the same layer of the
electrodes (horizontal approach) or in different layers (vertical approach), for example between two
layers of oxidized Si. The first approach is realized under a single deposition step but yields the
temperature uniformity over the structure that is not desirable. In contrast, the second approach
which still requires a number of processes allows one fabricating various configurations and
maintaining well-defined temperature distribution. The more detailed description one can find
elsewhere [261].

The most of microhotplate designers consider the polycrystalline Si doped with B or P
impurities to be very appropriate material to make heaters and the temperature sensors because it
does not contaminate the IC processing equipment. When the poly-Si layer is doped with B under
concentration close to 110
20
atoms/cm
3
, its electrical resistance becomes to be almost independent
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on temperature. If such poly-Si is employed as a heater it generates a uniform heat flow which is not
affected by temperature variations. When the poly-Si layer is doped with B under concentration
close to 210
19
atoms/cm
3
, its electrical resistance is a linear function of temperature that makes
possible to design the reliable thermometer. The boron is frequently selected as a doping because its
amount can be accurately controlled in order to predict the electrical resistivity of the poly-Si layer.
Following the implantation, the structures are annealed to let the B to diffuse and to re-crystallize
the Si layer.
In order to fabricate the hotplates one can use the technologies of silicon bulk or surface
micromachining [262-264]. The features of membranes developed under these two approaches are
shown in Fig. 30.

In the framework of bulk micromachining technology, the silicon wafer is etched at the
backside of the silicon wafer to build the required cavities under masking layer structured by
photolitography [263,265,266]. The typical procedure to produce micromachined substrates
includes, (1) the coverage of silicon bulk substrate, of hundreds m thickness, by a dielectric layer,
(2) the deposition of a metal layer to form heater and electrodes by patterning, (3) the passivation of
the heater, and (4) the backside etching in order to reduce the thermal mass of the heated part. The
bulk micromachining by anisotropic silicon etching is intensively employed by the NIST to study
MOX gas sensors and sensor arrays [267-269]. Still, however, many other groups employ surface
micromachining technology to design freestanding membranes using sacrificial layers (see, for
example, Zeitschel et al. [270]). The sacrificial layer is deposited over the substrate surface and
covered by a second layer which is intended to form a membrane. Then, the sacrificial layer is
removed by etching leaving a cavity underneath of the membrane layer. The drawback of this
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method is a limited distance between the membrane and substrate which is typically of several
microns defined by thickness of the sacrificial layer. Although this distance is rather sufficient to
design other functional units, as, for example, micromotors, the gas sensors often require the
thickness of the sacrificial layer to be in order of several dozens of microns to reduce a heat transfer
to the substrate.
The advantages of the bulk and surface micromachining technologies which have been
numerously discussed by many authors [256,264,271-273] could be combined in frames of porous
silicon (PS) technology [263,265,266] as shown in Fig. 31.
***Figure 31*** near here

The PS technology has the following specific features [263,265,266,273,274]:
The very thick layers could be produced which extend over the whole wafer thickness. This
property is employed to develop thermal sensor membranes which need a sacrificial layer to
be thicker than 50 m which cannot be obtained using such conventional layers as silicon
dioxide or doped silicate glasses. Due to the large thickness the PSi gives options to design a
wide air gap between the membrane and substrate;
The chemical reactions occurred at internal surfaces of PS layer are very fast. This permits
quick and easy removal of the sacrificial layer even at room temperature with low
concentrated alkaline solutions instead of aggressive HF employed in other cases;
The backside lithography is not necessary that, (i) makes easier the packaging of the final
sensor and the using of adhesives; (ii) gives higher yield; (iii) provides better mechanical
stability of the wafer;
The heat conductivity of the PSi is lower than that of bulk silicon by two or three orders of
magnitude in dependence on the preparation of the PSi layers [259];
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There are no geometrical restrictions caused by the crystallographic orientation of the

substrate used. Unlike anisotropic etching, the geometry of the PSi layers is not limited by
certain planes and so they can be designed locally on a wafer with controlled undercutting.
This has been a major hindrance in the development of special sensors, e.g., for optical
applications where circular designs are required;
The formation of PSi layer is very selective to type and doping level of the substrate. This
property is used to define a finish of silicon etching;
Any geometries of the PSi layer can be designed via appropriate surface masking layers;
The PSi layers could be further covered with other thin films by, for instance, epitaxy
processes which are widely employed under Complementary-Metal-Oxide-Semiconductor
(CMOS) technologies.
The using PSi as a sacrificial layer requires it to contain pores with sizes in the range of 4 -
50 nm which ensures a mechanical stability of the layers [256,271,272].

Thus, the surface micromachining technology based on PSi layers allows one producing chips of
small sizes with a low cost. However, still the PSi layers are subject of stresses and sticking to the
substrates because of narrow gap that limits their applications [263]. In addition, the PSi structures
could not be made by lateral undercutting and free standing planes need making holes to enter an
etchant.
The removal of PSi to make a sacrificial layer is conventionally carried out with highly diluted
alkaline solutions, like KOH or NaOH in a concentration of 0.5-5 wt. %, at room temperature or
employing high-density plasma [259]. The etching of the sacrificial layer made of PSi with low-
concentrated alkali at room temperature makes possible to keep other chip components. It is
especially important when this layer is removed as the last one under the chip production.
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Recently, it has been suggested that for some applications the PSi may not be removed to
build the air gap [275], as it was originally demonstrated over a decade ago for flow sensors [276].
Due to low thermal conductivity, the porous silicon may provide sufficient thermal isolation from
the substrate. As a result, such approach provides improving the mechanical strength of the device
with an almost identical thermal isolation function.
It was established that the microhotplates may operate at temperatures in the range of 20-
1000
o
C and these temperatures are limited by material employed as the thermometric layer [277].
For example, Al allows one getting 550
o
C while polycrystalline Si and tungsten 800
o
C and 1000
o
C, respectively. The ratio of temperature to the power consumption in microhotplates in air is in the
range from 8
o
C/mW to 300
o
C/mW. Some achievements in the field of micro-hotplates fabrication
are summarized in the Table 3. It is seen that the hotplate platforms designed by Furjes et al. [257]
drawn in Fig. 27b allow one to get temperatures at the range of 100800
o
C under power of 330
mW. The same parameters had hotplate designed by Han et al. [278]. The operating temperatures
higher than 800
o
C in this platform achieved in the under power consumption below 35 mW. It was
found that dissipated power depends strongly on the membrane thickness. Thinner membrane, less
power dissipation is (see Fig. 32). However, the excessive decrease in thickness leads to a sharp
degradation of the mechanical properties of the membrane and shortening the lifetime of the
microhotplates.
Figure 32 near here [279]

Besides, it was shown that free-standing membranes have a low thermal capacity that allows
varying fast the operating temperature. For example, the temperature response time of the hotplate
designed by Furjes et al. [257] was smaller than 5 ms. Such options have been considered by some
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authors to bring a new measurement concept based on the temperature cycling to enhance the gas
sensor selectivity and to analyze multicomponent gas mixtures (for example, Splinter et al. [256].
** Table 3*** near here [257, 259, 280, 281]

Table 4 gives an overview of recently presented microheaters and micromachined
microhotplates (MHPs) for gas sensor applications. The size of the active membrane, materials used
for the (membrane and heater) and the process technology. It is also indicated in the table whether
the device was only simulated (S) or fabricated (F) or both, the maximum operating temperature to
which the device was heated, the power dissipation at maximum operating temperature, the thermal
time constant ()
** Table 4*** near here [279]

The fact that the sensor element placed on the top of membrane is thermally isolated against
the bulk of Si substrate allows one to design a sensor array with thermally decoupled sensors at the
single chip so that each sensor operates at different temperature. When compared to hybrid
integrated sensor array the advantages to employ such single-chip monolithic integration are
reduced overall dimensions of the array, small production costs, and low power consumption of the
whole array.
Thus, the micromachining technologies offer following opportunities for the gas sensors as,
(i) lower power consumption, (ii) smaller size, (iii) higher mechanical and thermal strength, (iv) a
compatibility with standard ICs, (v) the possibility to integrate large systems, and (vi) faster thermal
response. The last option is required to realize the fast pulsed temperature operation [254,282] and,
in some cases, to perform on-chip annealing of the gas sensitive layers after packaging [261,283].
Besides that the micromachining technique provides higher flexibility in lateral geometry design
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(i.e. size, density) and offers more possibilities for integration of sensors and read-out circuits in a
large array [280].
However, experiment has shown that such approach has disadvantages as well [284]. Firstly,
fabrication of the membrane and the membrane micro-heater using micromachining technology
requires a large number of additional operations, and a long production cycle. Therefore, the use of
this technology becomes cost-effective only at very large output of sensors, since minimum quantity
of plates even in the experimental production has at least 10,000 sensors chips. Industrial
production becomes profitable at a much larger scale of production. Secondly, the thermo-
mechanical properties of the materials used for fabrication micromachined membranes and micro-
heaters are in poor agreement with each other. Therefore, there is a need for production of
multilayer structures to compensate this mismatch. Furthermore, there is the problem of poor
adhesion of the heater and sensitive layer to the surface of silicon oxide, which till now is not
resolved completely. Third, the production of sensors using this technology requires the use of
different processing methods such as silicon bulk or surface micromachining, screen printing, etc.,
and materials (platinum), which are not peculiar to silicon microelectronics.
It is necessary to note, that the deposition of the gas-sensitive layer is one of the most
important aspects in the fabrication of micromachined gas sensors. Therefore, at present a
significant part of the overall researches related to design of such sensors is directed toward
adaptation of the conventional methods of metal oxides deposition to micromachined technology
[285]. This is hard task because micromachining requires micrometer resolution [286-289]. In
addition, as the pre-fabricated micro-heaters already contain etch troughs and do not exhibit flat
surface, the lithographic processing of the sensing layers is no longer possible [290]. The sensing
layers needs therefore to be deposited over shadow masks, which should allow one placing the
layers exclusively onto the predefined spots between the electrodes. Still, this requires only a
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moderate precision so that the masks could be made of mechanically stiff ceramics, which is
conventionally produced in the MEMS foundry in the form of micro-machined silicon wafers.
Another method to deposit gas-sensitive layer is using drop dispensers which allow placing small
volumes of gas sensitive materials as a sol on top of the hotplates following by thermal annealing to
form a gel [291-294]. Because of good thermal insulation the center regions of the hotplates can be
heated up to temperatures of 300700
o
C which are required to transform the colloidal suspension
into the solid film.
The local CVD processes could be also applied to develop micromachining sensors
[295,296]. Due to peculiarities of CVD process the deposition of MOXs takes place only in the
heated area, i.e. on the surface of the hotplate. It is considered that this technique may also prove to
become useful to grow MOX nanorods or NWs at the microhotplates [254,282,297].
The direct writing of powders via ink jets is another promising technology for local
deposition of MOXs over microhotplates. This method gives the possibility to combine advantages
of thick films and micromachining technologies. A general review of the state of the art in ink-jet
printing of different materials can be found elsewhere [298]. The scheme of the method is drawn in
Fig. 33. In contrast to parallel processes like photolithography, ink-jet printing makes possible to
fabricate individually each sample that, although, contradicts to requirements of mass-scale
production. Still, the modern computer-driven setups could help to build such individual devices
with a required automatics and accuracy. The designing of 3-D volume components is often termed
as a free-form fabrication [299]. At present, such ink-jet technology has been utilized to print
aqueous 2-D MOX suspensions with a particle size of ~37 m [300] which is enough to design
sensors under micromachining technology.

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It is worth noting that the gas sensors need to operate under air conditions. So, the
micromachined structures should be packaged to have openings. These openings are frequently
made as porous seals that prevent air flows going across the heated membrane but still allow analyte
molecules from the ambient air to enter the sensor [290].

3.2. Self heating of 1-D nanostructures
As it was shown in previous sections, micromachining technology gives possibility to reduce
considerably the power consumed by gas sensors. Instead of 1-5 W typical for conventional ceramic
and thick-film sensors, micromachined sensors even at operating temperatures above 500 C
consume less than 30-50 mW. Such a significant reduction in consumable power opens great
opportunities to develop a wide variety of portable devices. However, research has shown that even
such decrease of consumption power achieved for gas sensors is not the limit. Studies carried out in
recent years demonstrated that through the use of 1D structures, in particular the use the Joule self-
heating effect for operation of metal oxide nanowire sensor, further reduction of energy consumed
by sensors can be achieved and ultra-economic sensors can be designed [302-309]. In addition, this
avoids the need of external heaters. It is necessary to note that this idea of self-heating has already
been successfully tested for thin film-based gas sensing devices (see as an example, Salehi [310]).
However, the inevitable significant thermal losses to the support of the thin film sensing element
impeded the implementation of this method. Very recently Joule heating was used for gas sensing
with conducting multi-walled carbon nanotubes [311] and for selective surface functionalization
[312]. The major advantage of the semiconducting nanowires with respect to self-heated thin film
sensors [310,313] is their small thermal capacitance and drastic reduction of thermal losses to
electrodes and gas environment [302] (Fig. 34).
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Kolmakov and co-workers [302] and Morante and co-workers [306] have shown that this
approach gives possibility to design self-heating sensors which operate at temperatures up to 300-
400
o
C and consume power in the range from 2-5 W [302] to 20-30 W [306] (see Fig. 35).
Likewise, it has been observed that the thermal response time of these devices, due to small thermal
inertia, is very fast [309] (only a few milliseconds). This enables the use of higher modulation
frequencies of their temperature profile, making available the direct observation of the kinetics
associated with the chemical interactions between the metal oxide and the gases of interest [309].
These features pave the way to employ the self-heating effect in pulsed operation mode to improve
the selectivity and analytical capabilities of metal oxide-based sensors [203,308,309], keeping
moderate power requirements. Due to application of self-heating, both the increase of sensor
response and the decrease of response time can be achieved as well [305,306] (see Fig. 36). As it is
known, low sensitivity and long response and recovery times are main disadvantages of room
temperature nanowire-based gas sensors.
***Figure 36*** near here [306].

However, in the same papers Kolmakov and co-workers [302] and Morante and co-workers
[306] have noted that there are some principal differences with respect to the sensors heated
indirectly, which may impose some limitation on their application. There are two size domains in
the self-heating approach depending on the ratio between nanowire diameter, D, and space charge
width, W, at the nanowire surface:
(i) under D >> W , the redox reactions will not significantly affect the Joule heating of the nanowire;
(ii) while, under condition D<<W , the adsorption of gases and redox reactions at the nanowire
surface would open the conducting channel. The latter enhances the local temperature of the
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nanowire due to the Joule heat increase under constant bias condition. This means that the
temperature of nanowires, due to nanowire resistance variations during interaction with gas
surrounding, may be significantly changed when exposed to the different concentrations of gas
[306]. This change brings uncertainty to the sensors response, opposite to conventional sensors,
whose temperature remains constant during the operation. Prades et al. [306] have established that
during interaction with NO
2
(0.5 ppm) such power variations in 1D SnO
2
-based sensors were about
of a factor of 1.8 under the optimum working conditions.
One should also to take into account that due to nonlinearity of the I V characteristics
and because of self-heating effect during interaction with reducing gases, the Joule power
dissipated inside the nanowire can be increased even under the constant bias [305]. Indicated
processes form a positive feedback and therefore they may eventually destroy the nanowire resistor.
This effect was commonly observed for metal and highly doped semiconductor nanowires with
moderate melting points [314,315].
In addition, during the Joule heating, the steady-state temperature is not homogeneous along
the nanowire length, what complicates the sensor signal and response time of self-heated
chemiresistor [305]. The precise modeling of the temperature distribution along the length of the
nanowire sensing elements has shown that in vacuum conditions one can neglect radiation losses
and losses to the ambient gas and there remain only metal leads where the Joule heat dissipates from
the nanostructure (see Fig. 37). The increase of the ambient pressure to normal atmospheric
conditions drastically enhances the heat dissipation into the gas environment. However, for this
particular nanostructure, the heat dissipation into the metal leads still dominates [305].

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We need also to note that self-heating makes great demands of electrical contacts. As it is
seen in Fig. 36 from the electrical point of view, a SnO
2
nanowire and the two PtSnO
2
contacts can
be modeled by two back-to- back Schottky diodes (D
FW
and D
RV
) in series with a resistance [306].
These three components dissipate electrical power that contributes to the heating of the whole
structure. In a first approximation, the voltage drop at the forward biased junction V
DFW
is
negligible, whereas the reverse biased contact contribution V
DRV
is comparable to the voltage drop
along the nanowire V
NW
. The dependence of these two last terms with the temperature together with
the evaluation of the heat dissipation processes at the nanoscale makes modeling these self-heating
effects rather complex. Thus, for excluding contacts influence, contacts should be ohmic with very
low resistance. Otherwise, the heating will takes place in the area of contacts with following their
degradation.

4. OUTLOOKS
Thus, our analysis shows that engineering approaches are really effective methods to improve the
parameters of conductometric gas sensors. Of course, these optimization methods cannot replace
conventional approaches based on the search for new materials and the development of new
technologies that improve and optimize the gas-sensing layers. However, one cannot deny that
engineering approaches in a number of situations can give the best effect, and their use can
eliminate some genetic disadvantages of conductometric gas sensors. Therefore, we believe that
development of new engineering approaches and upgrading of existing ones is a promising direction
in gas sensor design, which can give a significant improvement of exploitation parameters of gas
sensors and expand their application in various fields.

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5. ACKNOWLEDGEMENTS
This work was supported by the Korea government (MSIP) (grant No. 2011-0028736), by the
Korean Science and Engineering Foundation (KOSEF) (NCRC grant No. R15-2008-006-01002-0)
funded by the Ministry of Science, ICT and Future Planning (MSIP), and by Basic Science
Research Program through the National Research Foundation of Korea (NRF) funded by the
MSIP (2012R1A1A2041564).

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Figure captions

Fig. 1. Conductance time evolution of the six tested TGS sensors during 3 years. (Reprinted from
Romain and Nicolas [63]. Copyright 2010 Elsevier.)

Fig. 2. Effect of pollutants released by a standard flowmeter assembled with lubricated joints and
needle valve on the gain of an ATLAS/TRT (CERN) straw tube. The gas gain, or simply "gain"
(G/G
0
) describes the amplification factor of an avalanche process occurring in the intense field
formed inside of the detector, relative to the initial one. (Data from Capeans [85].)

Fig. 3. Taxonomy of drift correction methodologies published in the scientific literature. (Reprinted
from Di Carlo and Falasconi [77]. Published by InTech as open access.)

Fig. 4. Conceptual steps of the drift correction process. (Reprinted with permission from Di Carlo et
al. [123]. Copyright 2011 Elsevier.)

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Fig. 5. Time evolution of two identical sensors (TGS 2620). (Reprinted with permission from
Romain and Nicolas [63]. Copyright 2010 Elsevier.)

Fig. 6. A block diagram describing different parts of the measurement system proposed for
compensation of temperature and humidity changes. (Reprinted with permission from
Hajmirzaheydarali and Ghafarinia [135]. Copyright 2011 IOP.)

Fig. 7. Response of CO sensor exposed repeatedly to ethanol. (Reprinted with permission from
Kitsukawa et al. [145]. Copyright 2000 Elsevier.)

Fig. 8. (a) The model sensor unit. (b) Elimination effect of filtering materials. (Reprinted with
permission from Kitsukawa et al. [145]. Copyright 2000 Elsevier.)

Fig. 9. Adsorption capacity of charcoal cloth as a function of the temperature. Ethanol was applied
with 1.2%, heptane with 0.9% and ethyl acetate with 2%. (Reprinted with permission from
Schweizer-Berberich et al. [144]. Copyright 2000 Elsevier.)

Fig. 10. Influence of ambient temperature on the baseline resistance of SnO
2
-based gas sensor
operated at fixed power corresponding to T
oper
=120
o
C. (Data from Gong et al. [149].)

Fig. 11. The scheme of conventional sensor architecture based on thin or thick gas-sensing SnO
2

films. The dimensions provided at the scheme indicate thick film sensors. (Idea from Miller et al.
[156].)
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Fig. 12. Influence of humidity on the temperature dependence of response to ozone of SnO
2
-based
thin film gas sensors: SnO
2
films were deposited by spray pyrolysis at T
pyr
= 390 C. (Reprinted
with permission from Korotcenkov et al. [107]. Copyright 2007 Elsevier.)

Fig. 13. Conductance measurement of water desorption from SnO
2
into vacuum. (a) Conductance
versus pulse temperature for three different pulse widths: 1- 6 ms, 2 - 100 ms, and 3 - 300 ms. (b)
the temperature pulse sequence used to desorb water and produce the data. (Data from Cavicchi et al.
[166].)

Fig. 14. Micrograph of monolithic MO-based gas sensor system fabricated via CMOS technology.
(Reprinted with permission from Graf et al. [172]. Copyright 2004 American Chemical Society.)

Fig. 15. Hydrogen sensor resistance changes during long-term exposure in hydrogen containing
environment at operation conditions. (Data from Adamyan et al. [186].)

Fig. 16. R
air
and R
gas
for a SnO
2
:Au thin film vs. the aging time, the sensor is operated at 400
o
C. (a):
The gas is 500 ppm CO in 30% RH; (b): the gas is 5000 ppm CH
4
in 30% RH. (Reprinted with
permission from Nelli et al. [187]. Copyright 2000 Elsevier).

Fig. 17. Influence of annealing on structural parameters of SnO
2
: 1 and 2 atomic bond length (Sn
O) variations as a function of annealing temperature. Data from [189]; 3 and 4 distortion of the
samples versus stabilization temperature. Data from [190].

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Fig. 18. (a) SEM image of hydrogen sensors based on single SnO
2
nanobelts synthesized via
catalyst-free thermal evaporation. (Reprinted with permission from Fields et al. [204]. Copyright
2006 American Institute of Physics.) (b) Single-nanowire sensor. (Reprinted with permission from
Hernandez-Ramirez et al. [203]. Copyright 2009 Royal Society of Chemistry.)

Fig. 19. The change of sensing characteristics of median sensor segment of SnO
2
3-D mesoporous
nanograin layer and 2-D nanowire mat versus measurement day: (a) sensitivity or response to 1ppm
of 2-propanol vapors; (b) background resistance in air. Open and filled circles correspond to NP and
NW samples. (Reprinted with permission from Sysoev et al. [194]. Copyright 2009 Elsevier.)

Fig. 20. Response of straight and segmented nanowires as a function of their radius at various
contact resistances (b = 0, 0.025, 0.25). For segmented nanowires (SNWs), the curve is drawn
versus the radius of the smaller segment. The solid curve (top) corresponds to the nanowire with no
contact resistance; the dashed curve corresponds to the SNW with thick segments of 500 nm
diameter and b = 0.025; the solid curve marked with circles corresponds to the SNW with b = 0.025;
the dotted curve corresponds to the SNW with b = 0.25. The depletion width is ~10 nm at all cases.
(Reprinted with permission from Dmitriev et al. [208]. Copyright 2007 IOP.)

Fig. 21. Calculated melting temperature T
m
(K) for different shapes of ZnO and metallic Zn
nanostructures versus R
1
, where R is radius and the length of the nanowires and nanotubes is equal
to 100 nm. (Reprinted with permission from Guisbiers and Pereira [215]. Copyright 2007 IOP.)

Fig. 22. Dependences of the nanowire resistance response with the relative humidity concentration.
The nanowire response to pulses of wet synthetic air with controlled relative humidity has been
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obtained at 295C using a nanowire of 70 nm of radius. (Reprinted from Hernandez-Ramirez et al.

[218]. Copyright 2007 Elsevier.)

Fig. 23. Illustration of cracking effect in metal oxide films.

Fig. 24. (a) Traditional gas sensor operating in a parallel current mode and (b) gas sensor operating
in a perpendicular current mode. (Idea from Ishikawa and Hara [227].)

Fig. 25. Temperature dependence of the response to hydrogen for WO
3
-based sensors with different
thicknesses of the top Pd electrode: 1-10 nm; 2- 100 nm. The hydrogen concentration is 300 ppm.
(Data from Ishikawa and Hara [227].)

Fig. 26. Micro-hotplate gas sensor: (a) SEM image of micro-hotplate suspended in a cavity with
contact electrodes on top; (b) scheme of deposition of the multilayered structure. (Reprinted with
permission from Meier et al. [254]. Copyright 2007 Elsevier.)

Fig. 27. (a) SEM view of thermally decoupled membrane array. (Reprinted with permission from
Splinter et al. [256]. Copyright 2004 Elsevier.) (b) SEM view of a free-standing sensor platform
fabricated using a sacrificial layer of porous silicon. (Reprinted with permission from Furjes et al.
[257]. Copyright 2004 Elsevier.) (c) Optical microscope photograph of a three-section heater sensor
array. (Reprinted with permission from Francioso et al. [258]. Copyright 2008 Elsevier.) (d)
Suspended porous silicon micro-hotplate with a Pt heater. The thickness of the membrane is 4 m.
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The depth of the cavity under the membrane is more that 60 m. (Reprinted with permission from
Tsamis et al. [259]. Copyright 2003 Elsevier.)

Fig. 28. Gas microsensors of (a) planar structure and (b) stacked structure. (Reprinted with
permission from Chung et al. [251]. Copyright 2000 Elsevier.)

Fig. 29. Comparison of heating power consumption between the three structures. Reprinted with
permission from Chung et al. [251]. Copyright 2000 Elsevier.)

Fig. 30. Micromachined membranes fabricated using (a) porous silicon as sacrificial layer material
and (b) bulk micromachining technology. (Adapted with permission from Splinter et al. [256].
Copyright 2001 Elsevier.)

Fig. 31. Fabrication of a membrane using porous silicon as a sacrificial layer: 1, photolithography;
2, Si porosification; 3, porous silicon etching.

Fig. 32. Simulated and theoretical modeling results of power dissipation vs.Si
3
N
4
membrane
thickness at an operating temperature of 700
o
C. (Reprinted with permission from Dennis et al. [279].
Copyright 2010 IJENS Publishers.)

Fig. 33. Ink-jet printing of ZrO
2
structures with 170-m resolution. The inks have a solids loading
of 14 vol%. (Idea from Zhao et al. [301].)

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Fig. 34. The sensor setup and principal thermal losses in the suspended nanowire heated by the
Joule heat: P
L
-losses to the contacts, P
G
- losses to the ambient gas, and P
R
-radiation losses; (b)
SEM image of the suspended SnO
2
chemiresistor. (Reprinted with permission from Strelcov et al.
[302]. Copyright 2009 American Institute of Physics.)

Fig. 35. The reactivity and reaction kinetics () as a function of the bias voltage. The straight dashed
line depicts no self-heating effect. 300 nm wide and 50 nm thick SnO
2
nanobelts were used in these
experiments. (Reprinted with permission from Strelcov et al. [305]. Copyright 2008 IOP.)

Fig. 36. Estimated temperature of the devices at different I
m
. (r
nw
~35 nm) (inset) SEM image of a
SnO
2
nanowire connected to two Pt microelectrodes fabricated with focused ion beam. The
equivalent circuit of this structure corresponds to two back-to-back diodes in series with the
nanowire resistance. These three components dissipate electrical power and contribute to the self-
heating of the device. (Reprinted with permission from Prades et al. [306]. Copyright 2008
American Institute of Physics.)

Fig. 37. Theoretical evaluation of the partitioning of thermal losses in individual nanowire-based
sensor between different channels: radiation, metal leads, and gas environment at 760 Torr and 10
3

Torr. (Reprinted with permission from Strelcov et al. [305]. Copyright 2008 IOP.)
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Table 1. Results of outgassing tests carried out for some commonly used polymer materials.

Material Type Outgas Global Result
KALREZ Fluoropolymer NO OK
VITON Fluorinated copolymer YES BAD
EPDM Copolymer ethylene propylene YES BAD
PVDF Fluorinated polyvinyldene YES BAD
PP Polypropylene NO OK
RILSAN (NYLON) Polyamide Water OK
PEEK Crystalline Polyetherether ketone NO OK
PEEK Amorphous Polyetherether ketone YES BAD
PUR Polyurethane YES BAD

Source: Data from Capeans [85].
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Table 2. Permeability of polymeric materials.

Sour
ce:
Data
from
[88-
93]
Permeability (Kx10
8
cm
2
/s)
Polymer Nitrogen Oxygen Carbon dioxide Water
Polyimide 0.03 0.1 0.2 0.01-0.16
KEL-F 0.004-1.0 0.02-0.7 0.04-1.0 0.22
PTFE 2.5 4.8 - 24
Teflon 0.14 0.04 0.12 27
Fluoroelastomer 0.05-0.3 1.0-1.1 5.8-6.0 40
Viton 0.5 1.14 2.3 218
Buna-n 0.2-2.0 0,7-6.0 5.7-48 760
Neoprene 0.8-1.2 1.5-4 19-20 1400
Buna-s 4.8-5.0 13 94 1800
Polyurethane 0.4-1.1 1.1-3.6 10-30 260-9500
Silicone - 76-460 460-2300 8000-28000
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Table 3. The thermal characterization of designed micro-hotplates

Parameter
Reference Dimension of the
sensor element (m
2
)
Maximum
temperature (C)
Dissipation
power,
(C/W)
t
T
(ms)*
Furjes et al. [257] 100 100 550 27 4.2
Adam et al. [280] 300 300
Tsamis et al. [259] 100 100 600 20
Triantafyllopoulou
et al. [281]
100 100 900 180340
*Time necessary to obtain maximum operating temperature.
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Table 4. Microhotplate specifications.

Membrane
size (m
2
)
Membrane
type
Heater
type
Process T
oper

(C)
Power
(mW)
Time constant
() ms
N/A SiO
2
/ Si
3
N
4
Poly Si bulk 500 68 0.6
324111 Si
3
N
4
Pt bulk 500 250 N/A
150 150 SiO
2
Poly Si bulk 300 12 3
150 150
100 100
Si
2
N
2
O Poly Si bulk 500 220/75 N/A
180 180 Si
3
N
4
Pt bulk 170 75 65
100 100 SiC HfB
2
bulk 380 35 N/A
100 100 SiC HfB
2
Bulk/SiC 250 20 50
80 80 SiO
2
Pt/Ti bulk 400 9 1
150 150
100 100
Si
3
N
4
Pt bulk 300 50/75 10/25

Source: Data from Dennis et al. [279].

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Figure-1
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Figure-2
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Figure-3
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Figure-4
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Figure-5
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Figure-6
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Figure-7
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Figure(s)
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Figure-9
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Figure-10
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Figure-11
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Figure-12
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Figure-13
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Figure-14
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Figure-15
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Figure-16
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Figure-17
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Figure-18
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Figure-19
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Figure-20
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Figure-21
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Figure-22
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Figure-23
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Figure-24
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Figure-25
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Figure-26
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Figure-27
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Figure-28
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Figure-29
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Figure-30
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Figure-31
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Figure-32
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Figure-33
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Figure-34
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Figure-35
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Figure-36
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Figure-37

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Title: Engineering approaches to improvement of

ENGINEERING APPROACHES TO IMPROVEMENT OF

ENGINEERING APPROACHES TO IMPROVEMENT OF

***Table 1*** near here [85]

2.7. Artificial or forced aging

which is typical for conductometric metal-oxide sensors, such a working environment is

A significant reduction in power consumption can be achieved by lowering the operating

There are no geometrical restrictions caused by the crystallographic orientation of the

[32] G. Korotcenkov, V. Tolstoy, J. Schwank, Successive ionic layer deposition (SILD) as a

[100] N. Yamazoe, J. Fuchigami, M. Kishikawa, Interaction of tin oxide surface with O

[115] F. Hossein-Babaei, V. Ghafarinia, Compensation for the drift-like terms caused by

[161] G. Korotcenkov, V. Brinzari, J. Schwank, A. Cerneavschi, Possibilities of aerosol

[189] J.A. Toledo-Antonio, R. Gutierrez-Baez, P.J. Sebastian, A. Vazquez, Thermal stability

[203] F. Hernandez-Ramirez, J.D. Prades, R. Jimenez-Diaz, T. Fischer, A. Romano-Rodriguez, S.

[218] F. Hernandez-Ramrez, A. Tarancon, O. Casals, J. Arbiol, A. Romano-Rodriguez, J.R.

[266] W. Lang, P. Steiner, A. Richter, K. Marusczyk, G. Weimann, H. Sandmaier, Applications

hazards with temperature-programmed microsensors, Sens. Actuators B 121 (2007) 282

obtained at 295C using a nanowire of 70 nm of radius. (Reprinted from Hernandez-Ramirez et al.

Table 2. Permeability of polymeric materials.

Table 3. The thermal characterization of designed micro-hotplates

Table 4. Microhotplate specifications.

Anda mungkin juga menyukai

Table 1 near here [85]