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M. Hjiri 1,3,*, R. Dhahri 1, 3, K. Omri 1,2, L. El Mir 1,2, S. G. Leonardi 3  and G. Neri 3

1 Laboratory of Physics of Materials and Nanomaterials Applied at Environment, Faculty of Sciences of Gabes, 6072 Gabes, Tunisia.  
2 Al Imam Mohammad Ibn Saud Islamic University (IMSIU), College of Sciences, Departement of Physics, Riyadh 11623, Saudi Arabia. 
3 Dept. of Electronic Engineering, Chemistry and Materials Engineering, University of Messina, Messina 98166, Italy
* Corresponding Author; E-Mail:m.hjiri@yahoo.fr; Tel.: +216 28�241 258;



Abstract
 In-doped ZnO (IZO) nanoparticles have been prepared by sol-gel route. The morphological and microstructural properties were investigated by transmission electron microscopy (TEM) analysis and X-ray powder diffraction (XRD). The structural properties showed that the IZO nanoparticles exhibit hexagonal wurtzite structure. Chemoresistive devices consisting of a thick layer of IZO nanoparticles on interdigitated alumina substrates had been fabricated and their electrical and sensing characteristics were investigated. The sensor performances of the IZO nano-powders for carbon monoxide (CO) were reported. The results indicated that both the sensors exhibited high response and quick response recovery dynamics. The sensing properties were explained in terms of rapid gas diffusion onto the sensing layer surface.

Keywords: In-doped ZnO, Nanoparticles, Sol-gel, Gas sensor, CO.

1. Introduction
Gas sensors based on metal-oxide-semiconductor materials have attracted considerable attention during the past decade [1]. Zinc oxide (ZnO) and tin dioxide (SnO2) have been widely chosen as sensing materials because of their excellent characteristics such as low cost, high sensitivity, rapid response, and fast recovery [2, 3]. In addition, they have potential applications in detecting polluted or toxic gases and other species [4-6]. ZnO, as one kind of wide band gap (3.37 eV) n-type semiconductor material, is of great interest because of its mixed covalent/ionic aspects in the chemical bonding. Recently the high-performance gas-
sensing devices, using ZnO nanoparticles as sensing materials, were realized in sensing gases such as pollutant gases like H2S, benzene, NOx, NH3, etc. [7, 8], and explosive gases like CH4, H2, CO, etc. [9, 10].
In-doped ZnO material, characterized as a wide band gap semiconductor, have wide applications such as optoelectronic devices, solar cell and gas sensors due to their high conduction as compared to the single component oxide of ZnO or SnO2 and as a result only a lower power requirement is needed for them as a gas sensor. Besides, a lower operation temperature may be achieved by the doping effect and a significant resistance change can be obtained in the doping ZnO than undoped ZnO sensor which resulted in a high sensitivity [11].
In this study, IZO nanomaterials were synthesized, characterized and tested in the monitoring of low concentration of CO in air. The monitoring of CO is of utmost importance in the environmental control. CO is a gas produced during incomplete combustion and it is toxic at very low concentrations. In confined environments, such as automotive cabin, garage parking or tunnels, high concentrations of this pollutant can create serious hazard for the health and should be continuously monitored and controlled [12]. The concentrations of pollutant to be monitored in these ambient are very low, 5�50 ppm for CO [13].
We will show, in this paper, the effect of indium dopant on the structural and morphological properties of ZnO nanomaterials. Also, sensing properties of IZO nanoparticles will be discussed.
2. Experimental details
2.1. Samples preparation
IZO nanoparticles were prepared by a sol�gel method under supercritical conditions of ethyl alcohol (EtOH) based on L. El Mir et al. protocol [14-18], where the water for hydrolysis was slowly released by esterification reaction to control the size of the formed nanoparticles.  In this case, 16 g of zinc acetate dehydrate [Zn(CH3COO)2.2H2O; 99%] as a precursor in 112 ml of methanol. After 10 min of magnetic stirring at room temperature, an adequate quantity of indium chloride (InCl3) corresponding to [In]/[Zn] ratios of 0.02 were added. After 15 min under magnetic stirring, the solution was placed in an autoclave and dried in the supercritical conditions of ethyl alcohol (Tc=243 �C; Pc=63.6 bars) according to according to protocol reported in the ref. [18]. 
2.2. Characterization
The crystalline phases of the obtained nanopowders were identified by X-ray diffraction (XRD) using a Bruker D5005 powder X-ray diffractometer using a CuK� source (1.5405 � radiation). Transmission electron microscopy (TEM, JEM-200CX) were used to study the morphology and particle size of the phosphor powders. The specimens for TEM were prepared by putting the as-grown products in EtOH and immersing them in an ultrasonic bath for 15�min, then dropping a few drops of the resulting suspension containing the synthesized materials onto TEM grid.
3.3. Sensing test
Sensors were made by printing films (1-10 �m thick) of the nano-powders dispersed in water on alumina substrates (6mm X 3mm) with Pt interdigitated electrodes and Pt heater located on the backside. The sensors were then introduced in a stainless steel test chamber for the sensing tests. Electrical measurements were carried out in the temperature range from RT to 400�C, under a synthetic dry air total stream of 100 sccm, collecting the sensors resistance data in the four point mode. Gases coming from certified bottles can be further diluted in air at a given concentration by mass flow controllers. The concentration of CO target gas was varied from 5 to 50 ppm. A multimeter data acquisition unit Agilent 34970Awas used for this purpose, while a dual-channel power supplier instrument Agilent E3632A was employed to bias the built-in heater of the sensor to perform measurements at super-ambient temperatures. The gas response, S, is defined as  EMBED Equation.3   QUOTE   where R0 is the baseline resistance in dry synthetic air (20% O2 in nitrogen) and R is the electrical resistance of the sensor at different CO concentrations in dry synthetic air.
3. Results and discussion
Fig. 1 shows X-ray diffraction spectra obtained from the In-doped ZnO nanoparticles. XRD pattern indicates the formation of hexagonal wurtzite phase of ZnO [19, 20], were matched well with space group P63mc (no. 186) (JCPDS No. 36-1451). Second phases such as Zn2In2O3 and In2O3 can be showed [21]. The lattice constants calculated from the XRD pattern, which are very close to ZnO ones, i.e.,  EMBED Equation.DSMT4  and  EMBED Equation.DSMT4  . These results are in a good agreement with those obtained by L. El Mir et al. [22]. For our sample, the (002) diffraction line was, always, narrower than the (101) line and the latter is narrower than the (100) line. This indicated an asymmetry in the crystallite shape. It was supposed that crystallites had a prismatic form. The average grain size was calculated using Scherrer�s formula [23]:
 EMBED Equation.3                                                         (1)
Where � is the X-ray wavelength, �B is the maximum of the Bragg diffraction peak (in radians) and B is the full width at half maximum (FWHM) of the XRD peak. The average grain size of the basal diameter of the cylinder-shape crystallites is about 15 nm, whereas the height of the crystallites is in the range of 20 nm.
The TEM measurements show that very small ZnO particles are present in the as-prepared aerogel powder (Fig. 2). The size of the majority of ZnO particles in this powder varied between 17 and 22 nm [19, 22]. These values are in accordance with those obtained from XRD. 
The absorption spectra of IZO nanoparticles in the UV and visible range are reported in figure 3.  The absorption curve exhibit an intensive absorption in the range 200�380 nm, with the absorption edge in between 300 and 370 nm, owing to the relatively large exciton binding energy. The excitonic absorption for ZnO is at 373 nm as reported earlier [24, 25]. The blue shift in the excitation absorption clearly indicates the quantum confinement property of nanoparticles. In the quantum confinement range, the band gap of the particles increases resulting in the shift of absorption edge to lower wavelength, as the particle size decreases [26].
The optical band gap for In-doped ZnO nanoparticles was evaluated using the relation:
           EMBED Equation.3                                 (2)
where A is a constant, h� the photon energy and Eg is the energy gap. From Eq. (2), a Tauc plot can be drawn of (�h�)2 versus h�. The point of the extrapolation of the linear part that meets the abscissa will give the value of the band gap energy (Eg) of the material. Fig. 4 shows the Tauc plots of the ZnO:In materials. The values obtained for the band gap energies of the ZnO: In (3.25 eV) and undoped ZnO (3.35 eV), corresponding to the violetblue region of the electromagnetic spectrum [25]. The experimental results indicate that the ZnO:In nanoparticles have a wider band gap compared to that of the bigger sized spherical crystals. This can be explained by the characteristics of materials at nanodimension. It is known that at the nanoscale, there is an increase in pressure which results in strong forces towards the interior of the crystallites [27]. As a consequence, the lattice spacing of the ZnO nanoparticles is decreased. It is proposed here that due to the strong internal forces, the band gap is affected and the electrons taking part in the transition from the valence band to the conduction band need greater energy to execute the jump. Thus, it accounts for the observed wider band gap of the ZnO:In nanoparticles [21].
Fig. 5 summarizes the data obtained, reporting the sensors response versus the operating temperature. Initially, increasing the temperature, the response increases. The responses show a maximum around 300�C. When the temperature increases, the sensor response gets decreases. On the other hand, electrical resistance was tested at different CO concentrations and found to be obviously changed upon exposure to CO of as low as 5 ppm at a low operating temperature of 200�C, as shown in Fig. 6. At a higher operating temperature in the range of 300�400�C, the gas response much increased. Fig. 7 shows an example of the response transient of the layer at 300�C. It was found that the injection of 50 ppm CO induced a remarkable decrease in electrical resistance of the layer, leading to response magnitude of 4.80. It is also noted from this figure that the signal could return to its initial value after several cycles. This indicates that the adsorption of CO on the layer surface was reversible. The CO adsorbed on the surface was surely desorbed when CO gas was pumped out.
The sensing properties of the sensing layer at different operating temperatures were also investigated. The results are shown in Fig. 8. At each operating temperature, the response increased when the CO gas concentration increased. The response did not exhibit significant differences at different operating temperatures when CO gas concentration was low. The difference became distinct when the CO concentration increased. It was found that the IZO layer had the highest response to CO at 300�C. 
It is well accepted that the sensitivity of semiconductor gas sensors is attributed to the chemisorption of oxygen on the oxide surface and the subsequent reaction between adsorbed oxygen and tested gas, which causes the resistance change. The same mechanism may be applied for the CO-sensing of the present IZO layer. Thus, more CO molecules can react with more oxygen species on the layer grain surface, and can cause the decrease of barrier height leading to the reduction of electrical resistance. Takata et al. [28] found that the stable oxygen ions were O2" below 100�C, O" between 100 and 300 �C, and O2" above 300 �C. The relevant reactions on the surface area could be as follows:
 QUOTE   EMBED Equation.DSMT4                                                           (3)
 QUOTE   EMBED Equation.DSMT4                                                                (4)
 QUOTE   EMBED Equation.3                                                            (5)
From the knowledge of the catalytic activity, it is anticipated that reducing agents will react rapidly with O" presented on the surface, but very slowly with O2". O2 is essentially nonreactive [29]. At a low temperature of 150 �C, only Eq. (3) plays a major role in the catalytic oxidation of CO. As a result, a low CO response was achieved at that temperature in this work. It is obvious that the surface reaction in Eq. (5) is more desirable for the gas sensing, because the reaction could release more electrons to reduce the resistance of the film and thus increase the gas response. For the gas-sensing test performed at temperatures higher than 300 �C, the surface reaction can be represented mainly by Eq. (5). At 300�C, which would be the threshold temperature, the dominant oxygen species adsorbed on the surface and grain boundaries of the IZO layer may be O" and O2".
Therefore, the sensing mechanism at 300 �C may involve two types of reactions as described by Eqs. (4) and (5). IZO layer showed a decrease of CO response with temperature increasing, this is possibly due to the degradation of ZnO at this temperature [30]. 
Indium as dopant plays a very important role in the CO-sensing like the other dopant (Pt, Al, Cu, �) [31-34]. The In site played a role to adsorb CO molecules at both low and high temperatures. The research work conducted by Chen et al. [35] showed that the coexistence of ZnO with Cu could enhance the capability of Cu to adsorb CO molecules.
 When CO molecules are adsorbed on the layer, they are preferably adsorbed on the In2+ sites to form bonds between them. The CO adsorption mainly took place at the In2+ sites and not at the Zn2+ sites and then CO molecules migrated from the In2+ to the Zn2+ sites. In this way, the In2+ sites enhanced the CO adsorption and thus the reaction of CO with oxygen species.
4. Conclusion
In-doped ZnO powders were synthesized by a sol�gel process. These nanoparticles were investigated as sensing layer for CO sensing. The morphology, size and microstructure investigated, showed the presence of ZnO crystallytes having size varying between 17 and 22 nm. The optical analysis showed a decrease of band gap energy with the incorporation of indium dopant. 
Sensors based on In-doped films, presented a substantially improved CO gas sensitivity with respect the undoped ZnO, which is promising for a future development of these devices for practical applications.  















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Figure captions
Figure 1.   X-ray diffraction pattern of IZO aerogel nanoparticles.
Figure 2. Typical TEM photograph showing the general morphology of In doped zinc oxide nanopowder.
Figure 3. UV-vis-IR absorption spectrum of ZnO:In nanoparticles.
Figure 4. Plots of (�h�)2 versus photon energy h� of ZnO:In nanoparticles.
Figure 5.   CO response of the IZO nanoparticles as a function of the temperature.
Figure 6.   Transient responses of the sensors tested to different CO concentrations in air at the operating temperatup�˨�s�ҩS����G���ɫ.�����d���7�8�9�:�;�<�=�����������������������$d��x�x7$8$H$a$gd�udh�x�xgd��$dh�x�x7$8$H$a$gd��$dh�x�xa$gd��S�U�V���������#�C�E�F�G�H�J�r������ȯȯ���jU@(h��h�N�CJOJQJ^JaJmH	sH	(h��h7m�CJOJQJ^JaJmH	sH	(h��h�%�CJOJQJ^JaJmH	sH	,h��h33
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Figure 7.   Transient responses of the sensors tested to different CO concentrations in air at the operating temperature of 300 �C.
Figure 8.   Response of IZO nanoparticles as a function of CO concentrationsat different temperatures.




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