KR20160051585A - Preparation method of reuse ito target and the reuse ito target prepared thereby - Google Patents

Preparation method of reuse ito target and the reuse ito target prepared thereby Download PDF

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Publication number
KR20160051585A
KR20160051585A KR1020150130444A KR20150130444A KR20160051585A KR 20160051585 A KR20160051585 A KR 20160051585A KR 1020150130444 A KR1020150130444 A KR 1020150130444A KR 20150130444 A KR20150130444 A KR 20150130444A KR 20160051585 A KR20160051585 A KR 20160051585A
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KR
South Korea
Prior art keywords
ito target
ito
target
powder
recycled
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KR1020150130444A
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Korean (ko)
Inventor
유지상
홍길수
양승호
윤원규
Original Assignee
희성금속 주식회사
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Publication of KR20160051585A publication Critical patent/KR20160051585A/en

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
    • B24B7/20—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
    • B24B7/22—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/02—Coating starting from inorganic powder by application of pressure only

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to a method of manufacturing a recycled ITO target in which an ITO target in which a consumable part is present is coated with a powder containing at least one metal by a low temperature injection process and a recycled ITO target produced therefrom.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a method of manufacturing a recycled ITO target and a recycled ITO target produced therefrom,

The present invention relates to a method of manufacturing a recycled ITO target in which an ITO target in which a consumable part is present is coated with a powder containing at least one metal by a low temperature injection process and a recycled ITO target produced therefrom.

Transparent Conductive Oxidie (TCO) is a material that transmits light and electricity. In general, the transparent conductive oxide is used for a transparent electrode of a flat panel display, a solar cell, a liquid crystal display element, a light receiving element, and a light emitting element because of high transmittance in a visible region and excellent conductivity. Examples of the transparent conductive oxide include indium tin oxide (ITO), tin oxide (SnO 2 ), and zinc oxide (ZnO), and indium tin oxide is mainly used. The indium tin oxide is excellent in transparency, electrical conductivity and stability, has a relatively low resistivity, is capable of deposition at a low temperature, and is easy to wet-etch.

The indium tin oxide-containing ITO target is generally manufactured through a molding and sintering process using ITO powder. In Korean Patent Publication No. 2008-0056974, a slurry ITO mixture containing ITO powder and ITO sol is sprayed A method of manufacturing an ITO target through a molding and sintering process using granular powder formed after drying is disclosed. The ITO target produced by this method can be used for sputtering vacuum deposition to form a transparent thin film and exhibits a target efficiency of about 30%. At this time, an erosion of an elliptical shape called a race track appears on the surface of the ITO target used for sputtering, which causes a problem that the efficiency of the ITO target is lowered.

In order to improve the efficiency of the ITO target, the ITO target used for sputtering must be recycled, but the manufacturing process for recycling the ITO target has not been developed so far. Specifically, the ITO target recycled so far has a crack in the ITO target, and the density of the ITO target is uneven, so it is difficult to expect a high-quality ITO transparent thin film when the recycled ITO target is sputtered again to form a thin film.

Korea Patent Publication No. 2008-0056974

 In order to solve the above problems, it is an object of the present invention to provide a method of manufacturing a recycled ITO target having a high density and uniformity.

 It is another object of the present invention to provide a recycled ITO target having the same physical properties (fine grain, high density, and high purity) as that of a conventional ITO target.

According to an aspect of the present invention, there is provided a method of manufacturing an ITO target, comprising the steps of: (a) debonding an ITO waste target to obtain an ITO target having a consumable portion; (b) coating the consumable portion of the debonded ITO target with a powder comprising at least one metal using a low temperature spray process; And (c) processing the surface of the ITO target coated with the consumable part.

The present invention also provides a recycled ITO target produced by the above production method.

The present invention can increase the efficiency of a target by 60% or more by using an unused ITO target portion by coating a metal powder on a consumable portion of the ITO target by using a cold spray process, It is possible to provide a recycled ITO target having the same physical properties as the target.

Further, by recycling the ITO waste target by the above-described manufacturing method, the present invention can be economical by reducing the raw material and manufacturing time required for the target production.

In addition, since the recycled ITO target manufactured according to the manufacturing method of the present invention is uniformly produced without cracking, when the recycled ITO target is used for sputtering, a high quality ITO transparent thin film can be expected.

1 is a cross-sectional FE-SEM photograph of a coating layer of a recycled ITO target prepared according to Example 1 of the present invention.
2 is a graph showing the thickness of a thin film of a recycled ITO target prepared according to Example 1 of the present invention and an ITO target of HSM Company of Comparative Example 1. FIG.

Hereinafter, a method of manufacturing a recycled ITO target according to the present invention will be described. However, the manufacturing method of the recycled ITO target of the present invention is not limited to the following method, and the steps of each process may be modified or optionally mixed as necessary.

(a) ITO The lung target By debonding Consumption department  Existing ITO Target  Steps to Obtain

The ITO waste target is a target already used for sputtering, and a backing plate is bonded. Thus, this step separates the ITO target in which the consumable part is present from the backing plate.

As a method of debonding the ITO waste target (backing plate separation), a conventional debonding process known in the art can be used without limitation, and a hot plate can be used. At this time, the debonding temperature is not particularly limited, but may be 150 to 250 ° C. Specifically, the de-bonding means that the ITO waste target is heated on a hot plate to melt the indium to separate the backing plate. Through the debonding, an ITO target in which a consumable part exists can be obtained.

(b) Debonded  ITO Target Consumption  Coating with a powder comprising at least one metal using a low temperature spray process

The consumed portion of the ITO target is consumed by sputtering the existing ITO target. Impurities such as oxides and carbides generated during the stuffer may be adhered to the ITO target, and the impurities should be removed before coating. The impurities can be removed by a conventional impurity removal method known in the art. By removing such impurities, it is possible to prevent contamination of impurities in manufacturing a recycled ITO target.

The cold spray process is a method of spraying raw material powder using an operating gas at a temperature lower than the melting temperature of the raw material powder. Unlike the thermal spray process in which the raw material powder is melted and sprayed in a solution state, coating can be performed at a low temperature in the low temperature spray process. The low-temperature spraying process is advantageous in that deformation and deterioration of the target can be prevented by injecting the raw powder at a low temperature, and a target having a desired shape can be manufactured at a desired position in a short time.

The 'low temperature' is a temperature within a range that does not melt the raw material powder normally used. Therefore, the 'low temperature' of the low-temperature dispersion process means a temperature at which the raw powder is not melted. In the present invention, the temperature range of 'low temperature' is preferably lower than the recrystallization temperature of the raw material powder, and when ITO powder is used, it may be lower than 1600 ° C.

In such a low temperature injection process, conventional low temperature injection equipment known in the art can be used without limitation. The low temperature injection equipment may comprise, for example, a powder charger, a gas heater, and a spray gun. Specifically, in the low-temperature spraying step, raw powder to be coated is charged into the powder charger, pre-heated gas used in the gas preheater is injected into the consumable part of the debonded ITO target using the injector, Lt; / RTI >

At this time, the powder includes at least one metal, and the metal may be at least one selected from the group consisting of Al, Ti, In, Cu, Sn, Zn, Ni ). ≪ / RTI > When such a powder contains two kinds of metals, it is preferable that the content of one kind of metal is 1 to 90% by weight based on 100% by weight of the powder and the remaining amount of one kind of metal is remaining amount.

When the consumable portion of the ITO target that has been debonded using the low-temperature injection process is coated with the powder, the distance between the ITO target and the injector, the gas pressure, the gas temperature, and the moving speed of the injector may be adjusted.

The distance between the ITO target and the injector is not particularly limited, but is preferably 30 to 80 mm. When the distance between the ITO target and the injector is less than 30 mm, cracks may be generated on the ITO target surface due to the pressure of the powder to be sprayed. When the distance is more than 80 mm, the sprayed powder hardly forms a coating layer The manufacturing efficiency can be reduced to 30% or less.

The gas pressure is not particularly limited, but is preferably 30 to 40 bar, and the gas temperature is preferably 450 to 550 DEG C though not particularly limited. If the gas pressure and temperature are in excess of 40 bar and 550 캜, the powder may be oxidized or agglomerated.

The gas is not particularly limited, but at least one selected from the group consisting of nitrogen (N 2 ), hydrogen (H 2 ), helium (He) and argon (Ar) can be used.

The moving speed of the injector is not particularly limited, but it is preferably 150 to 250 mm / s. If the moving speed of the injector is more than 250 mm / s, powder spraying may not be smoothly performed and the coating yield may be lowered.

(c) Consumption department  Coated ITO Target  Step of machining the surface

As a method of processing the surface of the ITO target coated with the consumable part, a conventional surface processing process known in the art can be used without limitation and a grinder can be used. Specifically, the surface of the ITO target coated with the consumable part can be planarized using silicon carbide (SiC) grinding stone. Through such surface processing, it is preferable to process the surface roughness to 0.3 μm or less.

Meanwhile, the method for manufacturing a recycled ITO target according to the present invention may further include bonding the recycled ITO target and the backing plate.

As the method of bonding the recycled ITO target and the backing plate, a conventional bonding process known in the art can be used without limitation, and a hot plate can be used. For example, a recycled ITO target and a backing plate can be placed on a hot plate and the indium-coated backing plate and the recycled ITO target can be bonded after the temperature is raised. At this time, the bonding temperature is not particularly limited, but it may be 150 to 250 ° C. Thereafter, the temperature of the hot plate is lowered to room temperature and cooled.

Meanwhile, the present invention provides a recycled ITO target produced by the above production method. This recycled ITO target is manufactured using a low-temperature injection process, so that the density is uniform without cracking.

Hereinafter, the present invention will be described concretely with reference to Examples. However, the following Examples are intended to illustrate one embodiment of the present invention, but the scope of the present invention is not limited by the following Examples.

[ Example  1] Recycling ITO target

The backing plate was debonded in the ITO waste target to obtain an ITO target in which the consumed portion was present. The consumable portion of the debonded ITO target was coated with ITO powder (90% indium, 10% tin) using a cold spray process. At this time, a coating layer was formed on the ITO target by setting the distance between the ITO target and the injector to 35 mm, the gas pressure to 35 bar, the gas temperature to 450 ° C, and the moving speed of the injector to 200 mm / s. The ITO target on which the coating layer was formed was surface-processed with a grinder to obtain a surface roughness of 0.3 μm. Thereafter, a ITO target with a surface processed and a backing plate were bonded with indium to prepare a recycled ITO target.

[ Comparative Example  1] ITO target

It is an ITO target produced by molding and sintering process in HSM, Korea without low temperature injection process.

[ Experimental Example  One]

The impurity content, density and bonding ratio of the ITO target of the recycled ITO target prepared in Example 1 and the ITO target of Comparative Example 1 were analyzed and the results are shown in Table 1 below.

division Specification of ITO target Example 1 Comparative Example 1 Impurities (ppm) Fe 10 8 7 Cr 10 6 5 Ni 10 5 4 Cu 10 3 5 Si 20 12 10 Al 10 2 One density (%) ≥99.8 99.81 99.85 Bonding rate (%) ≥99.0 99.7 99.8

As shown in Table 1, it was confirmed that the amount of impurities, the density of the recycled ITO target, and the bonding ratio with the backing plate of the recycled ITO target prepared in Example 1 were similar to those of the unused ITO target of Comparative Example 1. [

[ Experimental Example  2]

The thickness of the thin film formed after depositing the recycled ITO target prepared in Example 1 and the ITO target of Comparative Example 1 on a glass substrate was measured using Dektak-6M (Veeco). The results are shown in FIG. 2 .

Referring to FIG. 2, it can be seen that the recycled ITO target prepared in Example 1 exhibited thin film formation at a level equivalent to that of the ITO target of Comparative Example 1.

Claims (7)

(a) debonding an ITO waste target to obtain an ITO target in which a consumed portion exists;
(b) coating the consumable portion of the debonded ITO target with a powder comprising at least one metal using a low temperature spray process; And
(c) processing the surface of the ITO target coated with the consumable part
≪ / RTI > The method according to claim 1,
In step (b), the at least one metal contained in the powder may be at least one selected from the group consisting of Al, Ti, In, Cu, Sn, Zn, Wherein the recycled ITO target is selected from the group consisting of: The method according to claim 1,
In the step (b), the powder contains two kinds of metals, and the amount of one kind of metal is 1 to 90% by weight based on 100% by weight of the powder, and the amount of other one kind of metal is remaining. Way. The method according to claim 1,
Wherein the distance between the ITO target and the injector is 30 to 80 mm in the low-temperature injection step of step (b). The method according to claim 1,
Wherein the gas pressure is in the range of 30 to 40 bar, the gas temperature is in the range of 450 to 550 ° C, and the moving speed of the injector is in the range of 150 to 250 mm / s in the low-temperature injection step of the step (b). The method according to claim 1,
Wherein the step (c) includes processing the ITO target coated with the consumable part to a surface roughness of 0.3 μm or less. A recycled ITO target produced by the method of any one of claims 1 to 6.
KR1020150130444A 2014-10-31 2015-09-15 Preparation method of reuse ito target and the reuse ito target prepared thereby KR20160051585A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR20140150071 2014-10-31
KR1020140150071 2014-10-31

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