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Scheme of the different stages of the spin coating process.

Scheme of the different stages of the spin coating process.

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Stable suspension made of fully redispersable In2O3:Sn (ITO) conducting nanoparticles were developed to obtain single thick transparent conducting films (up to 500nm) on different substrates using wet chemical deposition methods. The coatings can be processed at high sintering temperature process on glass substrates up to 1000°C to get electrical r...

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... coating is used for many applications in different technological fields. Thin films can be obtained by depositing drops of the solution on the surface of a flat substrate and then spun it to leave a uniform layer for subsequent processing stages and ultimate use. The stages of forming thin films are described as the followings below (34) (Fig. ...
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... density of ITO particles calcined at T = 350 °C as a function of the Sn-doping concentration and that of particles doped with 8 at % Sn as a function of the calcination temperature are shown in Fig. 13. Pure indium oxide particles heat treated at 350°C are quite dense, ρ ~ 6.93 g/cm 3 , about 96.5 % of the theoretical value (7.18 g/cm 3 ) but their density decreases gradually with the increase of the Sn concentration down to 6.6 g/cm -3 (12 at. % Sn) (Fig. 13 a). This means that the tin doping leads to a lower packing within the ...
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... doped with 8 at % Sn as a function of the calcination temperature are shown in Fig. 13. Pure indium oxide particles heat treated at 350°C are quite dense, ρ ~ 6.93 g/cm 3 , about 96.5 % of the theoretical value (7.18 g/cm 3 ) but their density decreases gradually with the increase of the Sn concentration down to 6.6 g/cm -3 (12 at. % Sn) (Fig. 13 a). This means that the tin doping leads to a lower packing within the particles (larger ...
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... a given doping concentration, the ITO particles become denser as a function of the sintering temperature (Fig. 13 b). This means that the pores inside the particles are gradually removed and that the grains building the particles become more tightly packed. 14 shows that the specific surface area (BET) of the powders decreases gradually by increasing the calcination temperature from 64 m 2 /g at 250 °C down to 21 m 2 /g at 550 °C. This result is due ...
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... measurements were carried out in order to investigate the structural properties of pure ITO coatings made of redispersable indium tin oxide nanopowders. Fig. 30 shows typical XRD patterns made with the the ITO350 sol and spin coated on fused quartz substrates and then heat treated in air at 130, 550, and 1000°C. The layer heated at low temperature 130°C was deposited on borosilicate glass. As expected all the films are polycrystalline. They show the same cubic bixbyite In 2 O 3 phase crystal ...
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... surface morphology of the coatings sintered at different temperatures and post annealed in a reducing atmosphere is shown in Fig. 31. As expected, all films consist of nano- crystalline particles, which have approximately a regular granular shape. The growth of the particles with the sintering temperature is clearly observable. The grain size of the film sintered at 550°C ranges between 35-45 nm, that of films sintered at 750°C between 50-60 nm and that sintered at ...
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... electrical properties of indium tin oxide coatings were characterised as a function of the doping concentration (Fig. 32), the heat treatment (Fig. 34, Fig. 35) and the type of the coating sol (Fig. 32). As shown in Fig. 32, the specific resistivity of spin coated ITO layer sintered in air at T = 550 °C first decreases with increasing Sn concentration, passes by a minimum at around 6 to 8 mol % and then increases. The ITO layers made of ITO350 particles show a minimum of the resistivity at a ...
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... in the case of the particles sintered at lower temperature. In addition the ITO350 particles were found to have larger crystallite size than the ITO250 ones, so that the electron scattering at grain boundaries is smaller. The specific resistivity, carrier density and mobility of ITO350 layers as a function of the doping concentration is shown in Fig. 33. It is seen that the carrier mobility is low and continuously decreases with increasing Sn doping and, as expected, that the carrier concentration increases, passes by a maximum at 6 wt. % and then decreases. This shows that the decrease of the resistivity of the films with the Sn concentration is essentially due to the increase of the ...
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... scattering centers and do not donate free electrons. Omata et al (295) reported that the increase of Sn concentration in ITO layers results in an increase of the interstitial oxygen ions which behave as a trap of the mobile electrons. The effect of the sintering time on the specific resistivity was tested at 550 °C for spin coated ITO250 layers (Fig. 34). The specific resistivity first decreases, passes by a minimum value for a firing time of about 30 min and then slightly increases. This period of time is sufficient to sinter the particles and to bring them close together. The increase of the resistivity at longer time may be attributed to the oxidation of the film due to a slow ...
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... increase of the resistivity at longer time may be attributed to the oxidation of the film due to a slow oxygen surface chemisorption effect, which removes the oxygen vacancies and reduces the concentration of charge carriers. The sintering of the layers was also tested up to 1000 °C with films deposited by spin coating on fused quartz substrates. Fig. 35 shows the variation of the specific resistivity, ρ, and the sheet resistance, R , of single ITO350 layer fired in air at different temperatures during 30 min and also further post annealed in forming gas (N 2 /H 2 : 92/8) at 350°C during 30 min. The Sn concentration of the coatings was 7 mol%. The resistivity of the film fired in air ...
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... in air at 550°C is 4.8x10 -2 Ωcm and decreases gradually by increasing the firing temperature down to 1.2x10 -2 Ωcm at T = 1000°C. This behaviour is related to a better sintering and to the growth of the particles which improve remarkably the carrier mobility which varies from 1.08 cm 2 / V.s at 550 °C to 4.25 cm 2 / V.s at 1000 °C as shown in Fig. 36. Increasing the sintering temperature also leads to a slight increase of the carrier concentration from 1.19x10 20 cm -3 at 550 °C to 1.55x10 20 cm -3 at 1000 °C. These results are in agreement with the growth of the crystallite size calculated from the XRD pattern (section 5.4.1) which increases from 25 nm at 550°C to 33 nm at 1000°C ...
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... crystallite size calculated from the XRD pattern (section 5.4.1) which increases from 25 nm at 550°C to 33 nm at 1000°C and with the SEM observations of the surface morphology of the coatings where the growth of the particles and a denser structured layer with larger and sharper grain size is clearly observed by increasing the firing temperature (Fig. ...
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... treatment in non oxidizing atmosphere leads to a slight increase (typically 11 %) of the charge mobility but to a significant increase of the carrier concentration as shown in Fig. 37. The mobility and the carrier density for the film sintered at 550 °C in air are 1.08 cm 2 / V.s and 1.2x10 20 cm -3 , respectively (Fig. 36) and increases after post annealing to 1.2 cm 2 / V.s and 3.32x10 20 cm -3 respectively (Fig. 37). The carrier mobility and concentration increase gradually with the sintering temperature up to ...
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... treatment in non oxidizing atmosphere leads to a slight increase (typically 11 %) of the charge mobility but to a significant increase of the carrier concentration as shown in Fig. 37. The mobility and the carrier density for the film sintered at 550 °C in air are 1.08 cm 2 / V.s and 1.2x10 20 cm -3 , respectively (Fig. 36) and increases after post annealing to 1.2 cm 2 / V.s and 3.32x10 20 cm -3 respectively (Fig. 37). The carrier mobility and concentration increase gradually with the sintering temperature up to 5.32 cm 2 / V.s and 7.63x10 20 cm -3 at 1000 ...
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... (typically 11 %) of the charge mobility but to a significant increase of the carrier concentration as shown in Fig. 37. The mobility and the carrier density for the film sintered at 550 °C in air are 1.08 cm 2 / V.s and 1.2x10 20 cm -3 , respectively (Fig. 36) and increases after post annealing to 1.2 cm 2 / V.s and 3.32x10 20 cm -3 respectively (Fig. 37). The carrier mobility and concentration increase gradually with the sintering temperature up to 5.32 cm 2 / V.s and 7.63x10 20 cm -3 at 1000 ...
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... values shown in Fig. 35, 36 were measured at least one week after the production of the coatings and correspond to stable values. Interestingly it was observed that the specific resistivity and the sheet resistance of the post annealed coatings measured immediately after the process was lower and unfortunately increases with time until reaching a stable value. ...
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... Fig. 35, 36 were measured at least one week after the production of the coatings and correspond to stable values. Interestingly it was observed that the specific resistivity and the sheet resistance of the post annealed coatings measured immediately after the process was lower and unfortunately increases with time until reaching a stable value. Fig. 38 shows the sheet resistance of the ITO coatings measured at three different stages: before annealing, immediately after annealing and after storage in air during one week (20 °C, 40 % RH). The time evolution of the sheet resistance of the post annealed layers varies significantly and depends on the temperature at which the layer was ...
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... become more difficult and the specific surface area of the particles become smaller so that the surface chemisorption reactions are reduced. This explains the slighter changes of the sheet resistance of the samples fired at 1000°C comparing to that fired at lower temperatures. This also explain the small variation shown for the carrier density in Fig. 36, where smaller surface results in less interaction with the adsorbed oxygen ...
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... refractive index of the coatings was measured by the VASRA method (see appendix A3.3). Fig. 39 shows the B θ shifts to higher value when the firing temperature raises. The refractive index of the coating at λ = 550 nm increases from 1.52 to 1.62 when the firing temperature raises from 550 to 1000°C respectively. The measurements of the refractive index using the ellipsometry method shows the same trend. All the results are ...
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... information which corroborates the above discussion is the optical behaviour of the coatings sintered at different temperatures and further annealed in forming gas. Fig. 43 and Fig. 44 show some representative T and A curves for coatings sintered between 550 °C and 1000 °C. ...
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... the electrical resistivity strongly decreases with the increase of the sintering temperature (see Fig. 35), a shift of the near IR transmission edge toward lower wavelength was expected, but the contrary is observed. This behaviour is due to the shift of the large IR absorption edge toward longer wavelength (Fig. 44). Equation [41] and the variation of the ratio n /µ obtained from the dc electrical data (see Fig. 37) indicate that such a ...
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... of the sintering temperature (see Fig. 35), a shift of the near IR transmission edge toward lower wavelength was expected, but the contrary is observed. This behaviour is due to the shift of the large IR absorption edge toward longer wavelength (Fig. 44). Equation [41] and the variation of the ratio n /µ obtained from the dc electrical data (see Fig. 37) indicate that such a behaviour should be observed, but the values independent of the frequency can not explain the results. Similar observation was found by Bommel et al (70) for layers made of redispersable ATO particles, however no explanation for the shift toward longer wavelength was ...
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... shift of the optical band gap was observed although the resistivity of the coatings decreased by 3 order of magnitude. A similar behaviour has been observed for coatings sintered at the same temperature and then reduced in forming gas at 350 °C for 30 min, although in this case a much larger variation of n with the temperature has been observed (Fig. ...
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... is worth to remember that the temperature reached by the coated substrates also depends on the conveyor speed (see Fig.8). A heat treatment in a reducing atmosphere ( N 2 /H 2 : 92/8) at 130 °C has however a more drastic improvement on the sheet resistance of the layers which is decreased from about 8 kΩ down to 2 kΩ after a two hours treatment (Fig. 53). An increase of the time slightly degrades the sheet resistance by about 5 %. ...
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... cured MPTS/ITO layer shown in Fig To better investigate the structure of MPTS/ITO coatings on polymeric substrate, TEM spectroscopy was carried out. The preparation of thin cross sections using the conventional ion-milling technique is very difficult because of the ion damage of the polymeric substrates, thus ultramicrotomy was used instead. (Fig. 73 a) and a very loose packing ITO particles in the case of thermally cured sample (Fig. 73 b). ...
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... on polymeric substrate, TEM spectroscopy was carried out. The preparation of thin cross sections using the conventional ion-milling technique is very difficult because of the ion damage of the polymeric substrates, thus ultramicrotomy was used instead. (Fig. 73 a) and a very loose packing ITO particles in the case of thermally cured sample (Fig. 73 b). ...
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... solutions deposited on the surface and was modelled by several authors. The total surface energy σ s consists of two components, a polar part σ p resulting from the different intermolecular forces due to the permanent and induced dipoles and hydrogen bonding and a dispersion part σ d (nonpolar) due to the instantaneous dipole moment (327). Fig. 83 shows the time variation of the contact angle of water and the surface energy of MPTS/ITO film during the UV-treatment and determined using the model of Wu (340). The contact angle of water decreases considerably from 54 ° down to a minimum of 11.4 ° and the surface becomes hydrophilic. The total surface energy of the layer increases ...

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Citations

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Introduction Experimental Coating Sintered at High Temperature Coating Polymerized at Low Temperature Conclusion
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