JP2013533378A - Transparent conductive film, target for transparent conductive film, and method for producing target for transparent conductive film - Google Patents

Abstract

  Transparent conductive film that is also crystallized by low-temperature heat treatment process, has low resistance characteristics at low temperature, has excellent electrical conductivity, stable specific resistance value at various process temperatures, and excellent thermal stability, transparent A method for producing a target for a conductive film and a target for a transparent conductive film is provided. In the present invention, 0.01 to 10% by weight of an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound with respect to the total weight of the transparent conductive film; and indium tin oxide ( ITO) It is related with the transparent conductive film characterized by including 90-99.99 weight%.

Description

  The present invention relates to a transparent conductive film, a target for transparent conductive film, and a method for producing a target for transparent conductive film.

  The present invention claims the benefit of the filing date of Korean Patent Application No. 10-2010-0052772 filed with the Korean Patent Office on June 04, 2010, the entire contents of which are included in this specification.

  The transparent conductive film is used for a transparent electrode, an automobile window, a heat reflecting film for buildings, an anti-static film, or a anti-fogging used in a freezer showcase. It is also widely used for transparent heating elements.

Meanwhile, the transparent electrode is required to have high light transmittance and electrical conductivity. More specifically, the transparent electrode preferably has a light transmittance in the visible light region of 85% or more and a resistivity of 1 × 10 ⁻³ Ω · cm or less. The transparent electrode that satisfies the above conditions is suitable for a solar cell, a liquid crystal display device, an organic light emitting electric field display device, an inorganic light emitting electric field display device, a touch panel, or the like.

On the other hand, as the transparent conductive film, a tin oxide (SnO ₂ ) -based thin film, a zinc oxide (ZnO) -based thin film, an indium oxide (In ₂ O ₃ ) -based thin film, or the like is known. Among these, the tin oxide thin film includes an antimony tin oxide (ATO) thin film containing antimony as a dopant or a fluorine tin oxide (FTO) thin film containing fluorine as a dopant. Examples of the zinc oxide-based thin film include an aluminum zinc oxide (AZO) thin film containing aluminum as a dopant and a gallium zinc oxide (GZO) thin film containing gallium as a dopant. Examples of the indium oxide-based thin film include an indium tin oxide (Indium Tin Oxide, hereinafter referred to as “ITO”) thin film and an indium zinc oxide (Indium Zinc Oxide, hereinafter referred to as “IZO”) thin film. The ITO and IZO thin films have good optical characteristics and electrical characteristics, and are currently widely used as materials for transparent electrodes.

  The transparent conductive film is mainly manufactured by a sputtering method or an ion plasma method. In particular, the sputtering method is effective when the deposition of a material having a low vapor pressure or when it is necessary to precisely control the thickness, and is widely used because the operation is very simple and convenient. The sputtering method uses a target which is a raw material for a thin film. The target is a solid containing a metal element that is formed into a thin film, and the target is manufactured using a sintered body such as metal, metal oxide, metal nitride, metal carbide, or the like. Single crystal is used.

  The sputtering method generally uses an apparatus having a vacuum chamber in which a substrate and a target can be disposed. More specifically, after placing the substrate and the target in the vacuum chamber, a high vacuum is applied. Next, an inert gas such as argon is injected into the vacuum chamber to control the gas pressure to about 10 Pa or less. Then, argon plasma is generated by glow discharge between the base material as an anode and the target as a cathode. At this time, argon cations in the argon plasma collide with the target which is a cathode, and target constituting particles ejected by the collision are deposited on a substrate to form a transparent conductive film.

  On the other hand, an ITO thin film, which is one of typical transparent conductive films, requires a crystallization process in order to reduce the specific resistance value. In the case of the ITO thin film, it is crystallized by heat treatment after being deposited on a substrate such as glass or plastic. However, when an element is manufactured using the ITO thin film, the characteristics of the element are affected by a change in specific resistance value due to process temperature.

  An object of the present invention is to provide a transparent conductive film that is crystallized even by a low-temperature heat treatment step.

  An object of the present invention is to provide a transparent conductive film having low resistance characteristics at low temperatures and outstandingly excellent electrical conductivity.

  An object of the present invention is to provide a transparent conductive film having stable specific resistance values at various process temperatures and excellent in thermal stability.

  An object of the present invention is to provide a target for a transparent conductive film having a dense structure.

  The objective of this invention is providing the manufacturing method of the target for transparent conductive films which can form the ultrafine synthetic powder with a uniform particle size distribution of 50 nm or less by a coprecipitation method.

  An object of the present invention is to provide a method for producing a target for a transparent conductive film, in which an ultrafine synthetic powder has a high sintering driving force and can produce a high-density target.

  The present invention relates to an additive of 0.01 to 10% by weight containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound with respect to the total weight of the transparent conductive film; and indium tin oxide A transparent conductive film comprising (ITO) 90 to 99.99% by weight is provided.

  The present invention relates to an additive of 0.01 to 10% by weight containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound with respect to the total weight of the transparent conductive film target; and indium tin Provided is a target for a transparent conductive film, comprising 90 to 99.99% by weight of an oxide (ITO).

  The present invention includes a step of producing a solution containing an indium precursor and a tin precursor; a step of forming an ITO by adding an alkali compound to the solution; and a group consisting of a tantalum compound, a niobium compound, and a vanadium compound. For producing a transparent conductive film, comprising: a step of mixing a selected additive containing one or more selected types to form a molded body; and a step of sintering the molded body to produce a sputtering target. A method for manufacturing a target is provided.

  The transparent conductive film according to the present invention is crystallized by a low temperature heat treatment process. The transparent conductive film according to the present invention has a low resistance characteristic at a low temperature and has an excellent electrical conductivity. The transparent conductive film according to the present invention has a stable specific resistance value at various process temperatures, thereby realizing excellent thermal stability.

  Moreover, if the transparent conductive film target of the present invention is used, a transparent conductive film having a denser structure can be produced.

  Moreover, according to the method for producing a target for a transparent conductive film of the present invention, an ultrafine synthetic powder having a uniform particle size distribution of 50 nm or less can be formed by a coprecipitation method. The ultrafine synthetic powder has a high sintering driving force and can produce a high-density target excellent in densification.

It is a result graph which measured the surface resistance value by the heat processing temperature of the thin film of Example 1- Example 3 of this invention, and the comparative example 1. FIG. It is the graph which showed XRD before the heat processing of the thin film of the comparative example 1 (a), and after the heat processing (b). It is the graph which showed XRD before the heat processing of the thin film of Example 1, and (b) after heat processing. It is the graph which showed XRD before the heat processing of the thin film of Example 3, and (b) after heat processing. It is the photograph which showed SEM of the thin film of the comparative example 1 before heat processing (a) and after heat processing (b). The SEM before (a) and after heat processing (b) of the thin film of Example 1 is shown. The SEM before (a) of heat processing of the thin film of Example 3 and after heat processing (b) is shown.

  Hereinafter, the present invention will be described in detail.

I. Transparent conductive film The transparent conductive film of the present invention has an additive of 0.01 to 10 weights including one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound with respect to the total weight of the transparent conductive film. And indium tin oxide (ITO) 90-99.99% by weight.

  If the additive is included in the above-described range, the ionic radius of the group 5 element such as tantalum, niobium, vanadium is about 15 to 30% smaller than the indium ionic radius, so that the solid solution between the thin film mixtures is more efficient. Make it well done. Therefore, the transparent conductive film can be crystallized even by a low-temperature heat treatment step of 150 ° C. or lower, and the thermal stability can be improved. And the thin film which has a specific resistance value of the level equivalent to the specific resistance value of the transparent conductive film obtained at the temperature of 200 degreeC or more can be formed.

  If the additive is contained below the above range, crystallization cannot be achieved at a low temperature, and the specific resistance value cannot be lowered. If the additive is included beyond the above-mentioned range, ionized tantalum, niobium, vanadium, etc. cause scattering of indium tin oxide (ITO), thereby causing high carrier concentration. Therefore, there arises a problem that the resistance is increased by reducing the mobility of electrons.

  The additive is preferably an oxide, and more preferably contains one or more selected from the group consisting of tantalum oxide, niobium oxide and vanadium oxide.

The transparent conductive film of the present invention preferably has a transmittance of 85% to 100% and a specific resistance of 5 × 10 ⁻⁵ to 1 × 10 ⁻³ Ω · cm. The reason is that it is an appropriate condition that can be used as a flat transparent electrode. The flat panel display device is not particularly limited as long as the transparent conductive film of the present invention can be used as a transparent electrode. For example, a liquid crystal display device (LCD), a plasma display panel (PDP), an organic electroluminescence display device ( OLED), touch screen (TOUCH SCREEN), and the like.

  The transparent conductive film according to the present invention is also crystallized by a low-temperature heat treatment process. The transparent conductive film according to the present invention has a low resistance characteristic at a low temperature and has an excellent electrical conductivity. The transparent conductive film according to the present invention has a stable specific resistance value at various process temperatures, thereby realizing excellent thermal stability.

II. Target for transparent conductive film The target for transparent conductive film of the present invention is an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound with respect to the total weight of the target for the transparent conductive film. 0.01 to 10 wt%; and indium tin oxide (ITO) 90 to 99.99 wt%.

  If a transparent conductive film target containing the additive in the above-described range is used, the ionic radius of a group 5 element such as tantalum, niobium, and vanadium is about 15 to 30% smaller than the indium ionic radius. Solidification between the mixtures can be made more efficiently. Therefore, when forming a thin film with the said target, a transparent conductive film can be crystallized also by the low-temperature heat treatment process of 150 degrees C or less, and thermal stability can be improved. Then, a thin film having a specific resistance value equivalent to the specific resistance value at a temperature of 200 ° C. or higher can be formed.

  If the transparent conductive film target containing the additive in less than the above range is used, the transparent conductive film manufactured thereby cannot be crystallized at a low temperature, and the specific resistance value cannot be lowered. If a transparent conductive film target containing the additive beyond the above range is used, ionized tantalum, niobium, vanadium, etc. cause scattering to indium tin oxide (ITO), resulting in high carrier concentration. Make. As a result, the mobility of electrons in the transparent conductive film manufactured thereby decreases, and the resistance increases.

  The additive is preferably an oxide, and more preferably contains one or more selected from the group consisting of tantalum oxide, niobium oxide and vanadium oxide.

  If the target for transparent conductive films of the present invention is used, a transparent conductive film having a denser structure can be produced.

III. The manufacturing method of the target for transparent conductive films The manufacturing method of the target for transparent conductive films of this invention includes the step which manufactures the solution containing an indium precursor and a tin precursor.

  The indium precursor and tin precursor are not particularly limited as long as they are used in the technical field of the present invention, but are preferably metal alkoxide precursors. More specifically, examples of the indium precursor and the tin precursor include indium nitrate, indium chloride, tin chloride, and tin sulfide.

  The pH of the solution is preferably 1 to 4. If the above range is exceeded, problems may occur in the reaction rate of the solution, so it is preferable to maintain the above range.

  In order to adjust the pH of the solution to the above-described range, a pH adjusting agent can be added and stirred at 30 to 80 ° C. for 5 to 20 hours. As the pH regulator, ultrapure water or weak alkali can be used, and in some cases, weak acid can be used.

  The method for producing a target for a transparent conductive film of the present invention includes a step of forming an ITO by adding an alkali compound to the solution.

  More specifically, the step of forming an ITO by adding an alkali compound to the solution includes adding an alkali compound to the solution; the solution to which the alkali compound is added is 15 to 25 at 10 to 80 ° C. Preferably, the method includes a step of reacting for a time to form a precipitate; and a step of heat-treating the precipitate at 500 to 800 ° C. for 1.5 to 2.5 hours to form ITO.

  Here, the pH of the solution to which the alkali compound is added is preferably 7 to 10. Moreover, it is preferable to maintain the temperature at 10 to 80 ° C. after maintaining the pH of the solution to which the alkali compound is added at 7 to 10. If the pH and temperature described above are satisfied, the formation of a precipitate is promoted by the coprecipitation reaction of the indium and the tin precursor.

  If the pH of the solution to which the alkali compound is added is less than the above range, crystallization is difficult and the yield of the precipitate is lowered. Moreover, if it exceeds the above-mentioned range, it is not preferable because a long time is required in the washing filtration process.

  After adjusting the pH of the solution to which the alkali compound is added, if the temperature is maintained below the above-described temperature, the reaction time becomes longer. And if it maintains beyond the temperature mentioned above, since it will cause the growth of particle | grains, it is difficult to manufacture fine synthetic powder below 50 nm.

The alkali compound is not particularly limited as long as it is used in the technical field of the present invention, and examples thereof include NH ₄ OH.

  The average particle size of the precipitate is preferably 10 to 50 nm. If the above-mentioned range is satisfied, processing in a subsequent process is advantageous.

  The precipitate can be obtained by filtration and can be washed and dried. The precipitate can be separated by filtration using a filter press or a centrifuge. The washing of the precipitate can be performed using ultrapure water or alcohol. The precipitate can be dried by a method such as hot air drying. At this time, the temperature is preferably 80 to 200 ° C.

  If the precipitate is heat-treated at 500 to 800 ° C., residual moisture and chemically bonded salts present in the precipitate are decomposed and removed. If heat treatment is performed below the above range, the chemically bonded salt cannot be completely volatilized. If the heat treatment exceeds the above range, the particles are sintered (growth of particles), which is not preferable. If the particles are sintered, pulverization, which is a subsequent process, becomes difficult. Therefore, it is difficult to produce a sintered body having a dense structure by increasing the sintering driving force targeted by the present invention.

The ITO preferably has an average particle size of 1.0 to 10.0 μm and a specific surface area of 10 to 30 m ² / g. When the average particle size is larger than the above range and the specific surface area is less than the above range, it is difficult to form a dense structure with high density. If the average particle size is smaller than the above range and the specific surface area is larger than the above range, there is a risk of cracking during molding, and internal residual stress increases due to excessive shrinkage and generation of residual cracks during sintering. Can happen.

  In the method for producing a target for producing a transparent conductive film of the present invention, the ITO is mixed with an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound to form a molded body. Including stages.

  In more detail, the step of mixing the ITO with an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound to form a molded body is performed on the ITO. Mixing an additive containing one or more selected from the group consisting of a compound, niobium compound and vanadium compound to form a first mixture; mixing the first mixture with polyvinyl alcohol to form a second mixture; Preferably, the method includes a step of forming a slurry by wet ball pulverizing the second mixture; and a step of pressing the slurry to form a formed body.

  The additive is preferably an oxide, and more preferably contains one or more selected from the group consisting of tantalum oxide, niobium oxide and vanadium oxide.

  The polyvinyl alcohol is a substance that increases the molding density and the sintering density during target molding, and is coated on the surface of the first mixture, that is, the surface of ITO.

  When the second mixture is crushed by wet balls, water can be included as a medium. The slurry can be produced in a powder form by spray drying before pressing.

  The manufacturing method of the target for transparent conductive film manufacture of this invention includes the step which sinters the said molded object and manufactures a sputtering target.

More specifically, the step of producing the sputtering target by sintering the compact is a step of producing the sputtering target by sintering the compact at 1,250 to 1,600 ° C. for 10 to 20 hours. It is preferable that In sintering, it is more preferable to raise the temperature of the sintering furnace at a rate of 1.0 to 1.5 ° C./min and set the temperature range. It is more preferable to proceed in an oxygen atmosphere of 200 to 500 liters per 1.0 m ³ of the internal volume of the sintering furnace.

  The sintered body can be manufactured as a sputtering target by a grinding and cutting process.

  Meanwhile, it is preferable to perform a burn-out process for removing polyvinyl alcohol before sintering the molded body. In the burnout process, the temperature is raised to 900 ° C. in an air atmosphere or high-purity air atmosphere, and then the oxygen concentration is increased using oxygen gas in an atmosphere inside the chamber of the electric furnace at 1,000 ° C. or higher where shrinkage behavior occurs. Is preferably carried out while maintaining it higher than the oxygen concentration in the atmosphere.

  Next, in the method for producing a target for a transparent conductive film of the present invention, a cooling step can be further performed after sintering.

According to the method for producing a target for a transparent conductive film of the present invention, an ultrafine synthetic powder having a uniform particle size distribution of 50 nm or less can be formed by a coprecipitation method. The ultrafine synthetic powder has a high sintering driving force, and can produce a high-density target excellent in densification. More specifically, a substantial numerical range corresponding to the relative density measured by Archimedes principle, that is, a density of 98% or more, more specifically, if the theoretical density of ITO is 7.15 g / cm ³ . For example, when the density is measured using Archimedes' principle, an ITO target of 7.007 g / cm ³ (7.15 × 98%) or more, which is 98% of 7.15 g / cm ³ , can be produced. In addition, since it is sintered after being synthesized by coprecipitation and phase separation due to high temperature does not occur, a uniform conductive film can be formed without generating cracks or nodules during sputtering. it can. At the same time, a target having excellent electrical conductivity that is thermally and chemically stable and having a surface specific resistance of 1 × 10 ⁻³ Ω · cm or less, preferably 5 × 10 ⁻⁴ Ω · cm or less is manufactured. Can do.

  According to the method for producing a target for a transparent conductive film of the present invention, an ultrafine synthetic powder having a uniform particle size distribution of 50 nm or less can be formed by a coprecipitation method. Since the ultrafine synthetic powder has a high sintering driving force, a high-density target excellent in densification can be produced.

IV. Production of Transparent Conductive Film A step of forming the transparent conductive film using a sputtering apparatus equipped with the transparent conductive film target of the present invention will be described below.

After adjusting the initial vacuum in the chamber of the sputtering apparatus used to form the transparent conductive film to 1 × 10 ⁻⁶ Torr or less, the gas concentration and the deposition pressure are adjusted, and the process is performed at room temperature. Membranes can be manufactured.

  Next, the manufactured transparent conductive film can be heat-treated at a temperature of 300 ° C. or lower in an oxygen, nitrogen, vacuum, or air atmosphere. Preferably, the heat treatment is advanced at a temperature of 50 to 250 ° C. for 1 to 5 hours.

  Since the transparent conductive film manufactured as described above has thermal stability, it can be used for a transparent electronic device, and can be used for a liquid crystal display (LCD), a plasma display panel (PDP), an organic electroluminescent display. It is used for a flat panel display device such as a device (OLED) or a touch screen (TOUCH SCREEN) or a surface light source illumination device.

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, examples and comparative examples of the present invention will be illustrated. The following examples are provided only for the purpose of understanding the present invention, and are not intended to limit the technical scope of the present invention.

Examples 1 to 3 and Comparative Example 1: Production of Sputtering Target <Example 1>
After dissolving 1730 g of indium nitrate (In (NO ₃ ) ₃ .6H ₂ O) and 36.5 g of tin chloride (SnCl ₄ .3H ₂ O) in 60 ml of ethyl alcohol, ultrapure water was added as a pH regulator, The mixture was stirred at 50 ° C. for 12 hours to obtain a pH 3 solution.

Next, an NH ₄ OH aqueous solution was added to the solution to adjust the pH to 9. Then, it was made to react at 40 degreeC for 20 hours, and the deposit was manufactured. The precipitate was separated, washed with ultrapure water three times, and dried with hot air at 120 ° C. to produce a powder. Thereafter, the powder was put into an electric furnace and heat treated (calcined) at a temperature of 750 ° C. for 2 hours to obtain ITO.

  On the other hand, the average particle diameter and specific surface area of the ITO are shown in Table 1 below.

  Next, 998 g of the ITO was put in a port together with 2 g of tantalum oxide and 0.07 g of polyvinyl alcohol, and wet balls were pulverized for 20 hours using water as a medium to obtain a slurry. At this time, the crushing medium was a YTZ ball.

  On the other hand, the average particle size of the slurry was 0.5 to 1.0 μm, and the average particle size of 90% or more of the powder was 1.0 μm or less.

Subsequently, the slurry was spray-dried to obtain a spherical powder of 50 to 80 μm. The spherical powder was produced into a predetermined shape by applying a pressure of 2.5 ton / cm ² by CIP. Thereafter, the molded body was put into an electric furnace, heated to 1,550 ° C. at a temperature rising rate of 1.2 ° C./min, and then sintered for 12 hours to produce a sintered body. At this time, the electric furnace was supplied with 400 liters of oxygen per 1 m ³ of the internal volume, and the inside of the electric furnace was configured in an oxygen atmosphere. The sintered body was manufactured as a sputtering target by grinding and cutting process. As a result of the ICP component inspection of the sputtering target, a weight ratio of Ta: In: Sn = 0.205: 97.004: 2.927 was confirmed. The density and surface resistivity of the sputtering target are shown in Table 2 below.

Next, the sputtering target was mounted on an RF magnetron sputter, and the initial vacuum degree in the chamber was adjusted to 1 × 10 ⁻⁶ Torr or less, and then the In—Sn—Ta film was formed on the glass substrate to a thickness of 100 nm at atmospheric temperature. A -O-based thin film was deposited.

<Example 2>
In Example 1, except that 5 g of tantalum oxide was added to 995 g of the ITO, the rest was obtained in the same manner as in Example 1 to obtain a sputtering target. As a result of the ICP component inspection of the sputtering target, a weight ratio of Ta: In: Sn = 4.902: 92.37: 2.728 was confirmed. The density and surface specific resistance of the sputtering target are shown in Table 3 below.

Next, the sputtering target was mounted on an RF magnetron sputter, and the initial vacuum degree in the chamber was adjusted to 1 × 10 ⁻⁶ Torr or less. Thereafter, an In—Sn—Ta—O-based thin film was deposited on the glass substrate to a thickness of 100 nm at atmospheric temperature.

<Example 3>
A sputtering target was obtained in the same manner as in Example 1 except that 2 g of niobium oxide was added to 998 g of the ITO in Example 1. As a result of the ICP component inspection of the sputtering target, a weight ratio of Nb: In: Sn = 0.174: 96.979: 2.847 was confirmed. The density and surface specific resistance of the sputtering target are shown in Table 4 below.

Next, the sputtering target was mounted on an RF magnetron sputter, and the initial vacuum in the chamber was adjusted to 1 × 10 ⁻⁶ Torr or less, and then the In—Sn—Nb film was formed on the glass substrate to a thickness of 100 nm at atmospheric temperature. A -O-based thin film was deposited.

<Comparative Example 1>
In Example 1, the ITO was 1000 g, and the remainder was obtained in the same manner as in Example 1 except that tantalum oxide was not added.

  The density and surface specific resistance of the sputtering target are shown in Table 5 below.

Next, the sputtering target was mounted on an RF magnetron sputter, and the initial vacuum degree in the chamber was adjusted to 1 × 10 ⁻⁶ Torr or less, and then the In—Sn—O film was formed on the glass substrate to a thickness of 100 nm at atmospheric temperature. A system thin film was deposited.

<Comparative example 2>
In Example 1, except that 12 g of tantalum oxide was added to 988 g of the ITO, the rest was obtained in the same manner as in Example 1 to obtain a sputtering target. As a result of the ICP component inspection of the sputtering target, a weight ratio of Ta: In: Sn = 12.32: 85.16: 2.52 was confirmed. As a result of measuring the density of the target, a relative density of 90% of the theoretical density was shown, and the surface specific resistance was shown in Table 6 below.

Test example: Thin film characteristics evaluation <Electrical characteristics evaluation>
The sheet resistance values of the thin films of Examples 1 to 3 and Comparative Example 1 were measured. And after heat-treating at 180 degreeC, 250 degreeC, and 350 degreeC for 2 hours, respectively in the atmospheric condition of the thin film of Examples 1-3 and the comparative example 1, the sheet resistance value was measured.

  FIG. 1 is a graph showing the results of measuring the sheet resistance before and after the heat treatment of the thin films of Examples 1 to 3 and Comparative Example 1 of the present invention.

  Referring to FIG. 1, it was confirmed that the thin film of Examples 1 to 3 had less change in surface resistance due to temperature than the thin film of Comparative Example 1. And even if it heat-processes at 180 degreeC which is comparatively low temperature, it turns out that it was excellent in the sheet resistance value. And the thin film of Examples 1-3 by this invention shows that surface resistance is excellent compared with the comparative example 1 even if it does not heat-process (As axis | shaft of x-axis).

<Evaluation of crystallization>
The degree of crystallization of the thin films of Example 1, Example 3, and Comparative Example 1 was measured. And after heat-processing for 2 hours at 180 degreeC in the atmospheric condition of the thin film of Example 1, Example 3, and the comparative example 1, respectively, the crystallization degree was measured.

  2 is a graph showing XRD before and after heat treatment of the thin film of Comparative Example 1. FIG. FIG. 3 is a graph showing XRD of the thin film of Example 1 before (a) and after (b) heat treatment. FIG. 4 is a graph showing XRD before (a) and after (b) heat treatment of the thin film of Example 3. FIG. 5 is a photograph showing an SEM of the thin film of Comparative Example 1 before (a) and after (b) heat treatment. FIG. 6 shows the SEM before (a) and after (b) heat treatment of the thin film of Example 1. FIG. 7 shows SEM before (a) and after (b) heat treatment of the thin film of Example 3.

  2 to 7, it can be seen that the thin film of Comparative Example 1 exhibits amorphous characteristics, but crystallization becomes weak after heat treatment at 180 ° C. However, in the case of the thin films of Examples 1 and 3 of the present invention, it can be confirmed that the crystallinity is exhibited even in the absence of heat treatment, and it is confirmed that the crystallization becomes clearer by the heat treatment at 180 ° C. be able to. Moreover, in the case of the thin film of Example 1, it turns out that a crystal | crystallization smaller than the thin film of Example 3 is produced | generated at the same manufacturing temperature.

Claims (10)

For the total weight of the transparent conductive film,
Containing 0.01 to 10% by weight of an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound; and containing 90 to 99.99% by weight of indium tin oxide (ITO) A transparent conductive film.   2. The transparent conductive film according to claim 1, wherein the additive includes one or more selected from the group consisting of tantalum oxide, niobium oxide, and vanadium oxide.   The transparent conductive film according to claim 1, wherein the transparent conductive film has a transmittance of 85% to 100%. 2. The transparent conductive film according to claim 1, wherein the transparent conductive film has a specific resistance of 5 × 10 ⁻⁵ Ω · cm to 1 × 10 ⁻³ Ω · cm. For the total weight of the target for transparent conductive film,
Containing 0.01 to 10% by weight of an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound; and containing 90 to 99.99% by weight of indium tin oxide (ITO) A target for a transparent conductive film.   2. The transparent conductive film target according to claim 1, wherein the additive includes one or more selected from the group consisting of tantalum oxide, niobium oxide, and vanadium oxide. Producing a solution comprising an indium precursor and a tin precursor;
Adding an alkali compound to the solution to form ITO;
Mixing the ITO with an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound to form a molded body; and sintering the molded body to form a sputtering target The manufacturing method of the target for transparent conductive film manufacture characterized by including the step which manufactures. The step of forming an ITO by adding an alkali compound to the solution comprises:
Adding an alkali compound to the solution;
Reacting the solution to which the alkali compound has been added at 10 to 80 ° C. for 15 to 25 hours to form a precipitate; and heat-treating the precipitate at 500 to 800 ° C. for 1.5 to 2.5 hours. The manufacturing method of the target for transparent conductive film manufacture of Claim 7 characterized by including the step of forming. The step of mixing the ITO with an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound to form a molded body,
Mixing the ITO with an additive containing one or more selected from the group consisting of a tantalum compound, a niobium compound and a vanadium compound to form a first mixture;
Mixing polyvinyl alcohol into the first mixture to form a second mixture;
The target for producing a transparent conductive film according to claim 7, comprising: a step of wet ball pulverizing the second mixture to form a slurry; and a step of pressing the slurry to form a formed body. Production method. Sintering the molded body to produce a sputtering target includes:
The method for producing a target for producing a transparent conductive film according to claim 7, wherein the shaped body is sintered at 1,250 to 1,600 ° C. for 10 to 20 hours to produce a sputtering target. .