KR101776610B1 - Manufacturing method for indium tin oxide film with excellent electrical properties - Google Patents
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Abstract
Discloses a method for producing an ITO transparent conductive film excellent in transmittance and electrical characteristics.
(A) a step of forming a first solution by dissolving an indium (In) precursor and a tin (Sn) precursor in a first solvent capable of improving the electrical characteristics according to the present invention; ; (b) adding a second solution having a pH of 8 to 10 to the first solution to form a hydroxide containing indium and tin; (c) drying the hydroxide, followed by first microwave annealing to form ITO (Indium Tin Oxide) nanoparticles; (d) dissolving the indium precursor and the tin precursor in a second solvent to form an ITO sol; (e) mixing ITO nanoparticles with ITO sol to form an ITO nanoink; And (f) spin-coating the ITO nano ink on the substrate, followed by a second microwave annealing, wherein the first solvent and the second solvent include a hydroxyl group (OH) .
Description
The present invention relates to a method for manufacturing an ITO transparent conductive film, and more particularly, to a method for manufacturing an ITO transparent conductive film having excellent electrical characteristics by microwave annealing at a low temperature of 100 to 400 ° C.
Transparent Conductive Oxide (TCO) has a high visible light transmittance (> 80%) and low resistance (<10 -4 Ω · cm) There is considerable interest in use in optoelectronic fields such as reflectors, flat panel displays, touch screens and electrochromic devices.
Many studies on TCO materials such as In 2 O 3 : Sn (ITO), SnO 2 : Sb (ATO), SnO 2 : F (FTO), ZnO: Al (AZO), ZnO: Ga It has been progressed. Of the various TCO materials, ITO (Indium Tin Oxide) is used in various fields due to its excellent electrical and optical properties.
In general, the ITO ink is an ITO ink in which the ITO particles are dissolved in a solvent. The ITO ink is coated on the substrate using inkjet-printing, dip-coating, spin-coating, However, a high-performance ITO transparent conductive film can be formed through a high-temperature heat treatment at 400 ° C or higher.
However, in the conventional ITO ink, since the ITO particles are clustered together in the process of dissolving the ITO particles in the solvent, the dispersing agent is added to improve the dispersion power, thereby stabilizing the ITO ink. In addition, the ITO transparent conductive film formed by the above methods has a problem in that it is not efficient in terms of time and cost because it is heat-treated at a high temperature of 400 DEG C or more for a long time to have excellent electrical characteristics.
Accordingly, a method for forming an ITO transparent conductive film at a low temperature of 400 DEG C or less by forming a stabilized ITO ink is required.
A related art related to the present invention is Korean Patent Laid-Open Publication No. 10-2006-0020575 (published on March, 2006, 2006), which discloses a method for producing polycrystalline ITO films and polycrystalline ITO electrodes.
An object of the present invention is to provide a method for producing an ITO transparent conductive film having excellent electrical characteristics by performing microwave annealing at a low temperature of 100 to 400 ° C.
According to an aspect of the present invention, there is provided a method of manufacturing an ITO transparent conductive film, comprising: (a) dissolving an indium (In) precursor and a tin (Sn) precursor in a first solvent to form a first solution step; (b) adding a second solution having a pH of 8 to 10 to the first solution to form a hydroxide containing indium and tin; (c) drying the hydroxide, followed by first microwave annealing to form ITO (Indium Tin Oxide) nanoparticles; (d) dissolving the indium precursor and the tin precursor in a second solvent to form an ITO sol; (e) mixing ITO nanoparticles with ITO sol to form an ITO nanoink; And (f) spin-coating the ITO nano ink on the substrate, followed by a second microwave annealing, wherein the first solvent and the second solvent include a hydroxyl group (OH) .
In the step (e), the ITO nanoparticles may be mixed in an amount of 15 to 30% by weight based on the total weight% of the ITO sol.
The first microwave annealing may be performed at 600 to 800 < 0 > C.
The second microwave annealing may be performed at 100 to 400 < 0 > C.
The indium precursor and the tin precursor in steps (a) and (d) may be mixed at a molar ratio of In: Sn of 5: 1 to 20: 1.
The ITO transparent conductive film manufacturing method according to the present invention can form ITO nanoparticles of high crystallinity by spin coating and microwave annealing to produce an ITO transparent conductive film with improved density.
Also, by performing microwave annealing at a low temperature of 100 to 400 ° C using an ITO nano ink mixed with ITO nanoparticles and ITO sol, ITO sol improves the dispersion degree of ITO nanoparticles, so that high density ITO transparent A conductive film can be produced.
In addition, an ITO transparent conductive film having excellent transmittance and electrical characteristics can be manufactured through the manufacturing method of the present invention, and the manufacturing cost can be reduced.
1 is a photograph showing the stereogram (b) of an ITO nano ink (a) and an ITO transparent conductive film according to an embodiment of the present invention.
2 is a photograph of an ITO transparent conductive film according to an embodiment of the present invention observed by FE-SEM (Field Emission-Scanning Electron Microscopy).
FIG. 3 is a photograph of the thickness of the ITO transparent conductive film according to the embodiment of the present invention observed by FE-SEM.
FIG. 4 is a photograph of the surface roughness of an ITO transparent conductive film according to an embodiment of the present invention, observed by AFM (Atomic Force Microscopy).
5 is a TEM (Transmission Electron Microscopy) image of ITO nanoparticles according to an embodiment of the present invention.
6 is a graph showing an X-ray diffraction (XRD) pattern of an ITO transparent conductive film according to an embodiment of the present invention.
FIG. 7 is a graph showing the chemical bonding state of In, Sn, and O of an ITO nano ink according to an embodiment of the present invention by XPS (X-ray Photoelectron Spectroscopy) analysis.
8 is a graph showing electrical characteristics of an ITO transparent conductive film according to an embodiment of the present invention.
9 is a flowchart illustrating a method of manufacturing an ITO transparent conductive film according to an embodiment of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention and the manner of achieving them will become apparent with reference to the embodiments described in detail below with reference to the accompanying drawings. The present invention may, however, be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Is provided to fully convey the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims. Like reference numerals refer to like elements throughout the specification.
Hereinafter, a method of manufacturing an ITO transparent conductive film having excellent electrical characteristics according to a preferred embodiment of the present invention will be described in detail with reference to the accompanying drawings.
Referring to FIG. 9, a method for manufacturing an ITO transparent conductive film according to the present invention includes forming ITO nanoparticles (S110); Forming an ITO sol (S120); ITO nanoink formation step S130; And an ITO transparent conductive film forming step (S140).
ITO (Indium Tin Oxide) nano-particle forming step (S110)
An indium (In) precursor and a tin (Sn) precursor are dissolved in a first solvent to form a first solution. The first solvent may be a solvent capable of ionizing an indium precursor and a tin precursor, and a solvent containing a hydroxyl group (OH) may be used. Examples thereof include alcohols such as ethanol, methanol, and isopropanol, distilled water, and the like.
The indium precursor can be used without limitation as long as it is a commonly used precursor, and examples thereof include indium (III) chloride tetrahydrate (InCl 3 .4H 2 O).
The tin precursor can be used without limitation as long as it is a commonly used precursor. Examples thereof include tin (II) chloride dehydrate (SnCl 2 .2H 2 O), tin (IV) chloride pentahydrate (SnCl 4 .5H 2 O) (ⅳ) include acetate (Sn (CH 3 CO 2 ) 4), tin (ⅱ) acetate (Sn (CH 3 CO 2) 2).
It is preferable that the indium precursor and the tin precursor are mixed in a molar ratio of In: Sn of 5: 1 to 20: 1. When the indium precursor is mixed at less than 5 times the tin precursor, the addition amount of the indium precursor is insufficient, so that the formation of the ITO nanoparticles may be incomplete. On the contrary, when the amount exceeds 20 times, the indium precursor is excessively added, and there is a problem in that incomplete formation of the ITO nanoparticles occurs due to insufficient doping of tin ions.
A second solution is added to the first solution to form a hydroxide comprising indium and tin. The hydroxide may be formed and precipitated in a solution in which the first solution and the second solution are mixed. The second solution is preferably added until the pH of the mixed solution is approximately 6 to 7, and may be stirred for approximately 5 to 30 minutes. This can be done for the uniform formation of the ITO nanoparticles to be formed. The second solution may be a weakly basic solution having a pH of 8 to 10, and the number of ammonia (NH 4 OH) and the like.
Impurities and unreacted matters remain in the solution containing the precipitated hydroxide, and a centrifuge can be used to remove the impurities. The solution may be stirred at a speed of about 2000-4000 rpm in a centrifuge, after which the hydroxide may be washed with distilled water. As a result, a hydroxide containing indium and tin from which impurities are removed can be obtained.
The impurity-depleted hydroxides form highly crystalline ITO nanoparticles through drying and heat treatment.
The drying can be carried out at about 40 to 60 占 폚.
The heat treatment is performed by first microwave annealing in a gas atmosphere in which nitrogen and oxygen are mixed. The first microwave anneal may be a suitable process for forming ITO nanoparticles of high crystallinity because of the superior heat treatment efficiency over the commonly used thermal annealing. The first microwave annealing is preferably performed at 600 to 800 ° C to form ITO nanoparticles of high crystallinity. When the temperature is lower than 600 DEG C, the crystallinity of the ITO nanoparticles may deteriorate. On the contrary, when the annealing is performed at a temperature exceeding 800 ° C., rapid grain growth of ITO occurs due to the high temperature, and the ITO particle size becomes large, and the physical properties of the ITO transparent conductive film deteriorate.
ITO sol forming step (S120)
An indium precursor and a tin precursor can be dissolved in a second solvent to form an ITO sol. The indium precursor and the tin precursor can be mixed at a molar ratio of In: Sn of 5: 1 to 20: 1, as described above.
The second solvent may be a solvent containing a hydroxyl group (OH), such as 2-propanol, ethanol, methanol, or the like, as in the first solvent.
ITO nanoink formation step (S130)
1 is a photograph showing the stereogram (b) of an ITO nano ink (a) and an ITO transparent conductive film according to an embodiment of the present invention.
1 (a) is a photograph showing an ITO nano ink mixed with ITO nanoparticles and ITO sol.
Fig. 1 (b) shows the stereoscopic view of the composition of the ITO transparent conductive film formed using microwave annealing.
Referring to FIG. 1 (a), an ITO nanoink may be formed by mixing ITO nanoparticles with ITO sol.
Referring to FIG. 1 (b), when ITO nanoparticles and ITO sol are mixed, an ITO transparent conductive film having a matrix shape in which ITO nanoparticles are connected to each other by ITO sol can be formed. At this time, ITO nanoparticles can have a uniform dispersibility by ITO sol.
2 (a) is a photograph of the ITO nanoparticles observed by FE-SEM (Field Emission-Scanning Electron Microscopy).
Referring to FIG. 2 (a), it can be seen that ITO nanoparticles have a diameter of 16.7 to 47.5 nm and an irregular shape. In general, ITO nano-ink without ITO sol stabilizes ITO nano ink by adding dispersion agent to ITO nanoparticles because ITO nanoparticles are clustered together in solution.
In the case of the present invention, the ITO sol serves as a dispersant, so that an ITO nano ink having improved dispersion of ITO nanoparticles can be formed.
The ITO sol and the ITO nanoparticles are preferably mixed in an amount of 15 to 30% by weight based on the total weight% of the ITO sol. More preferably 20 to 25% by weight. When the ITO nanoparticles are mixed in an amount of less than 15% by weight, the density of the ITO transparent conductive film is lowered and electrical characteristics are lowered. On the contrary, when the amount exceeds 30% by weight, the electrical properties of the ITO transparent conductive film may be deteriorated due to the aggregation of the ITO nano-particles.
ITO transparent conductive film forming step (S140)
The ITO transparent conductive film may be formed by spin-coating an ITO nano ink on a substrate, followed by a second microwave annealing.
The spin coating can be performed at a speed of approximately 1000 to 3000 rpm for 10 to 60 seconds.
The second microwave annealing may be performed at 600 to 800 ° C like the first microwave annealing, but is more preferably performed at 100 to 400 ° C in consideration of the matrix form of the ITO nano ink
If the second microwave annealing is performed at less than 100 캜, the effect of improving the density improvement inside the matrix may be insufficient due to the low temperature. On the contrary, when the temperature is higher than 400 ° C, the ITO sol contained in the ITO nano ink forms independent ITO nanoparticles due to the high temperature, and the physical properties of the ITO transparent conductive film deteriorate.
During the second microwave annealing, the denseness of the ITO transparent conductive film is further improved by the ITO sol between the ITO nanoparticles, so that the electrical characteristics of the ITO transparent conductive film are excellent.
As described above, in the method of manufacturing the ITO transparent conductive film of the present invention, the ITO nano ink and ITO sol mixed ITO nano ink are spin-coated on the substrate, and then microwave annealing is performed at a low temperature of 100 to 400 ° C, The transmittance and electrical characteristics of the ITO transparent conductive film are excellent.
In addition, the dispersion of the ITO nanoparticles is improved by the ITO sol, so that the stabilized ITO nano ink can be formed. In addition, an ITO transparent conductive film having improved denseness can be formed by microwave annealing at a low temperature (100 to 400 ° C), and it can be efficient in terms of process cost.
The method of manufacturing the ITO transparent conductive film of the present invention may further include a transparent conductive oxide such as ATO (Antimony Tin Oxide), FTO (Fluorinated Tin Oxide), AZO (Aluminum Zinc Oxide), GZO (Gallium Zinc Oxide) Conductive oxide (hereinafter referred to as " conductive oxide ").
Referring to FIG. 1 (b), an ITO transparent conductive film manufactured by the manufacturing method of the present invention is formed on a substrate and includes ITO nanoparticles. The resistivity ( ρ ) of the ITO transparent conductive film is 1.5 × 10 -2 to 1.18 × 10 -2 Ω · cm and the figure of merit (FOM) is 13 × 10 -4 to 19.9 × 10 -4 Ω - 1 < / RTI > A detailed description will be given later with reference to Fig. 8 and [Table 1].
A specific example of the method for manufacturing the ITO transparent conductive film will be described as follows.
1. Fabrication of ITO transparent conductive film
Manufacturing example
In: dissolving 1 mole ratio of indium (Ⅱ) chloride tetrahydrate (InCl 3 · 4H 2 O, aldrich) and tin (Ⅱ) chloride pentahydrate (SnCl 4 · 5H 2 O, aldrich) is mixed with the in distilled water: Sn 9 Afterwards, ammonia water (NH 4 OH, duksan) was added to form a solution having a pH of 6.75. Hydroxide containing indium and tin was formed and precipitated in the solution. The mixture was stirred at a speed of 3000 rpm in a centrifuge, and then washed with distilled water to obtain a hydroxide containing indium and tin from which impurities were removed. The hydroxide was dried at 60 DEG C and microwave annealed at 700 DEG C for 5 minutes to form ITO nanoparticles of high crystal.
Indium (II) chloride tetrahydrate (InCl 3 .4H 2 O, aldrich) and tin (Ⅱ) chloride dehydrate (SnCl 2 .2H 2 O, aldrich) were mixed in a molar ratio of In: Sn of 9: (CH 3 ) 2 CHOH, aldrich) to form ITO sol.
Example 1
Using the above production example, the ITO nano ink was composed only of ITO sol without ITO nanoparticles.
The ITO nano ink was spin-coated on a glass substrate (Corning EAGLE XG TM glass) at 2000 rpm for 30 seconds and then microwave annealed at 250 ° C to produce an ITO transparent conductive film.
Example 2
An ITO transparent conductive film was prepared under the same conditions as in Example 1, except that ITO nano-particles were mixed in an amount of 6% by weight based on the total weight% of the ITO sol in ITO nano-ink.
Example 3
An ITO transparent conductive film was prepared under the same conditions as in Example 1, except that the ITO nano-particles were mixed in an amount of 12% by weight based on the total weight% of the ITO sol in the ITO nano-ink.
Example 4
An ITO transparent conductive film was prepared under the same conditions as in Example 1, except that ITO nano-particles were mixed in an amount of 24% by weight based on the total weight% of the ITO sol in the ITO nano-ink.
2. Property evaluation method and result
The specimens of the ITO transparent conductive films of Examples 1 to 4 were measured by the following methods.
FIG. 2 is a photograph of an ITO transparent conductive film according to an embodiment of the present invention observed by field emission scanning electron microscope FE-SEM (Field Emission-Scanning Electron Microscopy, Hitachi S-4800).
2 (b) to 2 (e) are surfaces of the ITO transparent conductive film corresponding to Example 1 (b), Example 2 (c), Example 3 (d), and Example 4 (e). Since only ITO sol is used in Example 1 (b), it can be seen that the surface of the ITO transparent conductive film is irregular, rough, and discontinuous. From this, it can be seen that the ITO transparent conductive film of Example 1 has a high sheet resistance due to an increase in electron scattering. It can be seen from Example 2 (c) to Example 4 (e) that as the weight ratio of ITO nanoparticles to ITO sol is increased, the surface of the transparent conductive film is formed at a high density. The diameter of the ITO nanoparticles of Example 4 (e) was 28.0 to 63.6 nm, which was slightly larger than that of Example 1 (b). It can be seen that ITO sol improves the connection between the ITO nanoparticles during the second microwave annealing and is also a matrix of the ITO transparent conductive film.
FIG. 3 is a photograph of the thickness of the ITO transparent conductive film according to the embodiment of the present invention observed by FE-SEM.
3 (f) to 3 (i) are thicknesses of the ITO transparent conductive film corresponding to Example 1 (f), Example 2 (g), Example 3 (h), and Example 4 (i) 1 (f) is 311.7 nm, Example 2 (g) is 447.6 nm, Example 3 (h) is 609.2 nm, and Example 4 (i) is 877.6 nm. From the above results, it can be seen that the thickness of the ITO transparent conductive film is increased as the weight ratio of ITO nanoparticles to the ITO sol is increased. In Example 4 (i), the transparency of relatively high density It shows that it is the whole film.
FIG. 4 is a photograph of the surface roughness of an ITO transparent conductive film according to an embodiment of the present invention, observed by AFM (Atomic Force Microscopy).
R ms and R a were measured to measure surface roughness, that is, surface roughness.
R ms (root mean square) can be defined as the standard deviation of the height of the ITO transparent film within a given area, and R a is defined as the average value of the surface height. These factors can affect the electrical properties of the ITO transparent conductive film. More specifically, as R ms and R a decrease, the electrical characteristics of the ITO transparent conductive film are improved.
Referring to FIG. 4, as the weight ratio of ITO nanoparticles to ITO sol in Examples 1 (a), 2 (b), 3 (c) and 4 (d) Thereby reducing the surface roughness (surface roughness) of the interface width and height. As a result, the distance from the ITO nanoparticles to the ITO nanoparticles is shorter than that of the ITO nanoparticles, and the electron scattering at the interface of the ITO nanoparticles is reduced.
FIG. 5 is a photograph of the ITO nanoparticles according to an embodiment of the present invention observed with a transmission electron microscope TEM (transmission electron microscopy, JEOL-2100F operated at 200 kV, Gwangju Center).
Figure 5 was performed to further investigate the particle size and crystallinity of ITO nanoparticles. FIGS. 5 (a) and 5 (c) show specimens of ITO transparent conductive film containing only ITO nanoparticles, and FIGS. 5 (b) and 5 (d)
Referring to FIGS. 5 (a) and 5 (c), the ITO nanoparticles have irregular shapes and have a diameter of 15.8 to 45.5 nm. In addition, the particles are not in a form to be connected to each other but in an independent dispersed form. On the other hand, in the case of Example 4 in (b) and (d), the connected form of the particles can be seen, and it can be seen that the point having a diameter of 24.5 to 60.6 nm is due to the ITO sol.
5 (a) and 5 (b), the SAED (Electron Diffraction in selected region) pattern shows that Example 4 (b) shows a spot and ring pattern. These results indicate that polycrystalline, i.e., ITO nanoparticles of high crystal and low crystal are included. The high crystal is a highly crystalline ITO nanoparticle formed by performing microwave annealing at 700 ° C. The low-crystalline ITO nanoparticles formed by performing microwave annealing at 250 ° C may mean relatively low-crystalline particles as compared to the high-crystalline ones.
FIG. 6 is a graph showing an X-ray diffraction (XRD) pattern of an ITO transparent conductive film according to an embodiment of the present invention. FIG. 6 is a graph showing a pattern of a Cu K radiation of a Rigaku D / Max-2500 diffractometer.
Referring to the graphs of Example 1 (sample A), Example 2 (sample B), Example 3 (sample C), and Example 4 (sample D) in FIG. 6, a broad peak at 23 ° And a sharp peak occurred at 30.66 DEG and 35.54 DEG corresponding to the (222) and (400) planes. (JCPDS cards No. 06-0416) These peaks are slightly shifted to higher angles compared to the pure In 2 O 3 peaks. These results to mean that the Sn 4+ ions are doped into In 2 O 3 lattice, it can be described by the Bragg equation (nλ = 2dsin θ). That is, since the Sn 4+ (0.69 Å) radius is smaller than In 3+ (0.80 Å), the diffraction peaks of the ITO transparent conductive films of Examples 1 to 4 were shifted by 2θ angles. It is also confirmed that as the thickness of the ITO transparent conductive film increases and the weight of the ITO nanoparticles increases, the peak intensity increases.
7 is a graph showing the chemical bonding states of In, Sn and O of an ITO nano ink according to an embodiment of the present invention by X-ray photoelectron spectroscopy (ESCALAB 250 equipped with an Al K? X-ray source) FIG.
Referring to Figure 7 (a), In 3d 5/2 and In 3d 3/2 photoelectrons were emitted at 444.1 eV and 451.6 eV, respectively. This means that In exists on In 2 O 3 .
Referring to Figure 7 (b), Sn 3d 5/2 and Sn 3d 3/2 photoelectrons were emitted at 485.9 eV and 494.4 eV, respectively. This means that Sn 4+ exists on SnO 2 . These results indicate that Sn 4+ acts as a donor in the In 2 O 3 lattice and the ITO transparent conductive film is formed of In 2 O 3 phase doped with Sn.
Referring to FIG. 7 (c), peaks of indium hydroxide and tin hydroxide are observed. In general, when the annealing is carried out at a temperature of 330 ℃, In (OH) 3 and Sn (OH) 4 is In 2 O 3, respectively, and SnO 2 . The presence of the indium hydroxide and tin hydroxide of the present invention may be by microwave annealing at a low temperature of 250 ° C.
The carrier concentration and hall mobility, electrical characteristics in Table 1, were measured using a Hall effect meter (Ecopia, HMS-3000). The resistivity was measured using a resistance meter and the sheet resistance was measured using a CMT-SR surface resistance meter. Transmittance was measured by UV-vis spectroscopy (Scinco, S-3100) at a wavelength of 550 nm.
[Table 1]
Referring to FIG. 8 and Table 1, it can be seen that the carrier concentration of Example 4 is higher than that of Example 1, indicating that the thickness of the ITO transparent conductive film increases as the weight of the ITO nanoparticles increases. The hole mobility was the highest in Example 4 in which the ITO transparent conductive film was formed at a high density.
The resistance can be calculated by the following equation.
ρ = 1 / (Ne μ )
Where N is the carrier concentration, e is the electron charge (1.602 × 10 19 C), and μ is the hole mobility.
In Examples 1 to 4, the ITO transparent conductive film of Example 4 exhibited the lowest resistance, and the sheet resistance showed the lowest value in Example 4 as well. The sheet resistance can be defined as the resistance to the ITO transparency film thickness.
The transmittance is generally decreased as the thickness of the ITO transparent film increases. However, as can be seen from FIG. 8 (b), when Examples 1 to 4 are compared, it can be seen that the transmittance of the conductive film is slightly decreased by the high density of the conductive film even though the thickness of Example 4 is rapidly increased.
In the present invention, an ITO transparent conductive film having excellent electrical characteristics can be produced despite microwave annealing at 250 캜. The figure of merit (FOM) of the ITO transparent conductive film can be calculated by the following equation.
FOM (Ω -1 ) = T 10 / R s
And wherein, T is the membrane permeability, R s is the sheet resistance.
The performance indices of Examples 1 to 4 were 2.3 × 10 -4 , 4.0 × 10 -4 , 10.3 × 10 -4 and 19.3 × 10 -4 , respectively, and the ITO transparent conductive film of Example 4 had the best electrical characteristics can confirm.
While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It is to be understood that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.
Claims (5)
(b) adding a second solution having a pH of 8 to 10 to the first solution to form a hydroxide containing indium and tin;
(c) drying the hydroxide, followed by first microwave annealing at 600 to 800 ° C to form ITO (Indium Tin Oxide) nanoparticles;
(d) dissolving the indium precursor and the tin precursor in a second solvent to form an ITO sol;
(e) mixing ITO nanoparticles with ITO sol to form an ITO nanoink; And
(f) spin-coating the ITO nano ink on the substrate, and then performing a second microwave annealing,
Wherein the first solvent and the second solvent include a hydroxyl group (OH)
Wherein the ITO nanoparticles are mixed in an amount of 15 to 30% by weight based on the total weight% of the ITO sol.
Wherein the second microwave annealing is performed at 100 to 400 < 0 > C.
Wherein the indium precursor and the tin precursor in the steps (a) and (d) are mixed at a molar ratio of In: Sn of 5: 1 to 20: 1.
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| KR101776610B1 true KR101776610B1 (en) | 2017-09-11 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109234711A (en) * | 2018-09-25 | 2019-01-18 | 桂林电子科技大学 | A kind of method that sol-gal process prepares (400) Solute Content in Grain ito thin film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010155743A (en) * | 2008-12-26 | 2010-07-15 | Mitsui Mining & Smelting Co Ltd | Method for producing tin-doped indium oxyhydroxide particles |
| JP2011028861A (en) | 2009-07-21 | 2011-02-10 | Sumitomo Metal Mining Co Ltd | Manufacturing method of transparent conductive film, transparent conductive film, transparent conductive substrate, and device using the same |
| JP2011126746A (en) * | 2009-12-18 | 2011-06-30 | Tohoku Univ | Ito powder, method for producing ito particle, coating material for transparent conductive material, and transparent conductive film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010155743A (en) * | 2008-12-26 | 2010-07-15 | Mitsui Mining & Smelting Co Ltd | Method for producing tin-doped indium oxyhydroxide particles |
| JP2011028861A (en) | 2009-07-21 | 2011-02-10 | Sumitomo Metal Mining Co Ltd | Manufacturing method of transparent conductive film, transparent conductive film, transparent conductive substrate, and device using the same |
| JP2011126746A (en) * | 2009-12-18 | 2011-06-30 | Tohoku Univ | Ito powder, method for producing ito particle, coating material for transparent conductive material, and transparent conductive film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109234711A (en) * | 2018-09-25 | 2019-01-18 | 桂林电子科技大学 | A kind of method that sol-gal process prepares (400) Solute Content in Grain ito thin film |
| CN109234711B (en) * | 2018-09-25 | 2020-06-02 | 桂林电子科技大学 | Method for preparing (400) crystal face preferred orientation ITO film by sol-gel method |
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| KR20170051833A (en) | 2017-05-12 |
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