WO2016072441A1 - Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜及びｉｔｏ透明導電膜の製造方法 - Google Patents

Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜及びｉｔｏ透明導電膜の製造方法 Download PDF

Info

Publication number
WO2016072441A1
WO2016072441A1 PCT/JP2015/081123 JP2015081123W WO2016072441A1 WO 2016072441 A1 WO2016072441 A1 WO 2016072441A1 JP 2015081123 W JP2015081123 W JP 2015081123W WO 2016072441 A1 WO2016072441 A1 WO 2016072441A1
Authority
WO
WIPO (PCT)
Prior art keywords
sintered body
tin oxide
temperature
rich phase
sputtering target
Prior art date
Application number
PCT/JP2015/081123
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
崇 掛野
Original Assignee
Ｊｘ金属株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ｊｘ金属株式会社 filed Critical Ｊｘ金属株式会社
Priority to KR1020187023361A priority Critical patent/KR20180093140A/ko
Priority to JP2016557791A priority patent/JP6291593B2/ja
Priority to KR1020167031994A priority patent/KR102030892B1/ko
Priority to CN201580023075.4A priority patent/CN106460161B/zh
Publication of WO2016072441A1 publication Critical patent/WO2016072441A1/ja

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Definitions

  • the present invention relates to an ITO sputtering target suitable for forming an ITO film.
  • the present invention relates to an ITO sputtering target that has a small target particle size, high density, high strength, and reduced arcing and nodules, a manufacturing method thereof, an ITO transparent conductive film, and an ITO transparent conductive film manufacturing method.
  • Examples of main applications of the present invention include touch panels, flat panel displays, organic EL, and solar cells.
  • an ITO (indium-tin composite oxide) film is widely used as a transparent electrode (conductive film) in a display device centering on a liquid crystal display.
  • a method for forming the ITO film a method generally called physical vapor deposition such as vacuum vapor deposition or sputtering is used.
  • the magnetron sputtering method is often used because of operability and coating stability.
  • a film is formed by sputtering, in which a cation such as Ar ions is physically collided with a target placed on a cathode, and the material constituting the target is released by the collision energy, so that a substrate on the anode side facing the target is released. This is done by stacking films having the same composition as the target material.
  • the coating method by sputtering has a feature that it can be formed from a thin film of several nm to a thick film of several tens of ⁇ m at a stable film formation speed by adjusting processing time, supply power and the like. .
  • tin oxide is added in an amount of 1.0 to 50.0 wt.
  • Targets with a wide composition range of less than 10% are being developed.
  • Patent Document 1 a mixed powder with indium oxide containing 20 to 50 wt% tin oxide is press-molded, and this molded body is heated in a pure oxygen atmosphere at a temperature of 1500 to 1650 ° C. and a pressure of 0.15 to 1 MPa. It is known to produce an ITO sputtering target by pressure sintering.
  • Patent Document 1 As a typical patent for an ITO sputtering target, there is Patent Document 1 shown below.
  • This patent is “an ITO sputtering target manufactured by powder metallurgy from raw materials mainly composed of indium oxide and tin oxide, having a surface roughness Ra of 0.5 ⁇ m or less and a density D ( g / cm 3 ) and bulk resistance value ⁇ (m ⁇ cm) satisfying the following two expressions at the same time: an ITO sputtering target, a) 6.20 ⁇ D ⁇ 7.23, b ” ⁇ 0.0676D + 0.887 ⁇ ⁇ ⁇ ⁇ 0.0761D + 0.666. It is a technology about 20 years ago.
  • This patent discloses an ITO that hardly generates abnormal discharge or nodule during sputtering and has a minimum amount of gas adsorption so that a high-quality ITO film can be stably obtained under good film forming operations. It can be said that this is an epoch-making invention at that time that a sintered target can be realized.
  • the median diameter obtained from the particle size distribution is in the range of 0.40 (excluding 0.40) to 1.0 ⁇ m, and from the particle size distribution.
  • An ITO target formed using a tin oxide powder having a 90% particle size in the range of 3.0 ⁇ m or less is described.
  • macropores and microcracks are generated inside the sintered body, and the sintered body is processed. Cracks and cracks may occur during storage after storage or after processing. And they may affect the shipment of the product as a target.
  • Patent Document 3 discloses an ITO sintered body in which fine particles composed of In 4 Sn 3 O 12 are present in the In 2 O 3 matrix, which is the main crystal grain, as a technology related to ITO, A technique for providing an ITO sputtering target having a low bulk resistance, characterized in that the fine particles have a three-dimensional star shape in which needle-like protrusions are formed radially from the virtual center of the particle, is disclosed.
  • Patent Document 4 is made of In, Sn, and O, has a sintered density of 7.08 g / cm 3 or more, a bulk resistivity of 80 ⁇ cm to 100 ⁇ cm, and O / (In + Sn + O) of 1.75% or less (weight ratio). ) And an ITO sintered body that is 30% or less of the integrated intensity of the X-ray diffraction peak of the (200) plane of the In 4 Sn 3 O 12 phase, and this sintered body is formed of In, Sn, and O.
  • a technique for switching a sintering atmosphere from an oxidizing atmosphere to a non-oxidizing atmosphere when the sintering temperature becomes 1400 ° C. or higher is disclosed.
  • a low-resistance film with ITO (tin oxide: 10 wt.%) That is generally used, it is necessary to perform heat treatment at 150 ° C. or higher, but there are cases where heat cannot be applied even at 150 ° C. .
  • a transparent conductive film used in a touch panel or the like is a structural problem, and when a heat cannot be applied during film formation or after film formation, a low resistance tin oxide composition that can obtain a low resistance film even at a low temperature can be obtained.
  • ITO is used.
  • the ITO target having a low tin oxide composition changes the probability of existence of a tin-rich phase depending on the sintering temperature.
  • the sintering temperature is controlled, it is difficult to increase the density and it becomes difficult to control the crystal grain size. Also, the density may vary from lot to lot. Further, the dispersibility of the tin-rich phase is deteriorated, and the problem that nodules and arcing are likely to occur easily occurs.
  • Patent Documents 5 to 10 below propose an ITO sputtering target having a low tin oxide composition.
  • the tin oxide content is 1.5% to 3.5% by mass
  • the relative density is 98% or more
  • the crystal phase is a single phase
  • the average crystal grain size is 10 ⁇ m or less
  • the sintered body Is characterized by a bending strength of 70 MPa or more, but the sintering temperature is as high as 1500 ° C., and it takes one effort to produce a molded body by mixing the first granulated powder and the second granulated powder. , Productivity is not so good.
  • Patent Document 6 includes indium oxide, tin oxide, and inevitable impurities.
  • the tin oxide content is 2.5% by mass or more and 5.2% by mass or less, and the average density is 7.1 g / cm 3 or more.
  • the ITO sputtering target has an average crystal grain size of 3 ⁇ m or more and less than 10 ⁇ m, but the holding temperature is as high as 1500 to 1600 ° C., and the strength of the sintered body is not described.
  • Patent Document 7 a tin content of 3 to 12 wt%, solid solution amount of tin that is dissolved in the In 2 O 3 phase is at least 2 wt%, In 2 O 3 phase and In
  • the average crystal grain size of the phase in which tin element is dissolved in the 2 O 3 phase is in the range of 2 to 10 ⁇ m, and the maximum pore diameter present in the sintered body is 3 ⁇ m or less, Indium oxide / tin oxide sintered body characterized in that the maximum agglomerated diameter is 5 ⁇ m or less, the sintering temperature is 1500 ° C. or higher, and the average particle size in Examples and Comparative Examples is as large as 7 ⁇ m or more,
  • the sintered body density is also as low as 6.9 g / cm 3 at the maximum. Further, the strength of the sintered body is not mentioned.
  • Patent Document 8 discloses a sintered body made of indium, tin, and oxygen.
  • the amount of tin is 2 to 4 wt%, the relative density is 90% or more, and the tin oxide phase and the intermediate compound phase other than the indium oxide phase have an area. It has a single-phase structure with a rate of 5% or less and a specific resistance value of 1 ⁇ 10 ⁇ 3 ⁇ ⁇ cm or less, but the sintering temperature is as high as 1500 to 1700 ° C., and the sintered body The specific resistance is also high.
  • Patent Document 9 discloses a sintered body having a large area of 300 mm ⁇ 300 mm or more and a thickness of 6 mm or more, which is substantially composed of indium oxide and tin oxide, and the content of tin oxide is 35% by weight or less. Then, the average density of 7.13 g / cm 3 sintered density is not less than that, the maximum density difference in the plane direction of the sintered body is not more than 0.03 g / cm 3 , and further 2 ⁇ m or less in the central part in the thickness direction.
  • ITO sintered body number hole is equal to or is 500 / mm 2 or less, and held at 1450 ° C. or higher sintering temperature, but is characterized by sintering, sintering temperature 1450 ° C. or higher The sintering method is also finely defined, and it cannot be said that productivity is good.
  • Patent Document 10 includes a sintered body that is substantially composed of indium, tin, and oxygen, has a relative density of 99% or more and has a plate thickness portion of 10 mm or more, and satisfies the following formula (1).
  • Characteristic ITO sputtering target Relative density (%) of central portion in thickness direction of sintered body / density of entire sintered body (%) ⁇ 0.995 The temperature is as high as 1600 ° C., and although not described, it is assumed that the crystal grain size is large.
  • none of the above documents is produced from the viewpoint of increasing the small particle size, increasing the density, and increasing the strength by changing the tin oxide-rich phase by low-temperature sintering.
  • the present invention relates to an ITO sputtering target having a low tin oxide composition capable of obtaining a low-resistance film even at a low temperature.
  • the ITO has a small target particle size, high density, high strength, and reduced arcing and nodules.
  • a sputtering target is provided. Thus, it is an object to improve the quality and reliability of film formation.
  • the average crystal grain size of the sintered body is in the range of 1.0 to 5.0 ⁇ m, and pores having a major axis diameter of 0.1 to 1.0 ⁇ m are 0.5% or less in area ratio
  • the indium oxide phase and the tin oxide rich phase are two phases.
  • the area ratio of the tin oxide rich phase is 0.1 to 1.0% or less, and 95% or more of the tin oxide rich phase is three grain boundaries.
  • Sputtering target characterized by existing in importance.
  • the sputtering target according to 1) above which contains Sn having an atomic ratio of Sn / (In + Sn) of 2.3 to 3.2%. 3)
  • the sintered body density is 7.03 g / cm 3 or more, and the bulk resistivity is 0.10 to 0.15 m ⁇ ⁇ cm, according to any one of the above 1) or 2) Sputtering target.
  • a method for producing a sputtering target comprising In, Sn, O, and inevitable impurities, wherein Sn / (In + Sn) is 1.8% or more in terms of atomic ratio of SnO 2 powder and In 2 O 3 powder. It is characterized in that the ratio is adjusted so as to be 7% (excluding 3.7%) and mixed, and sintering is performed while maintaining the maximum sintering temperature at 1450 ° C. or lower in an oxygen atmosphere.
  • a method of manufacturing an ITO sputtering target A method of manufacturing an ITO sputtering target.
  • the SnO 2 powder and the In 2 O 3 powder are mixed and sintered by adjusting the ratio so that Sn / (In + Sn) is 2.3 to 3.2% by atomic ratio.
  • a transparent conductive film composed of In, Sn, O, and inevitable impurities, and Sn / (In + Sn) is 1.8% or more and 3.7% or less (provided that 3.7%
  • a method for producing a transparent conductive film by sputtering wherein the substrate is kept unheated or kept at 150 ° C. or lower in a mixed gas atmosphere consisting of argon and oxygen and having an oxygen concentration of 4% or less.
  • a mixed gas atmosphere consisting of argon and oxygen and having an oxygen concentration of 4% or less.
  • the present invention relates to an ITO sputtering target having a low tin oxide composition suitable for forming a transparent conductive film and capable of obtaining a low resistance film even at low temperatures.
  • the target has a small particle size, high density, high strength, arcing and nodules. It is possible to provide a sputtering target capable of reducing. As a result, it is possible to improve the quality and reliability of film formation. As a result, there is an excellent effect that the productivity and reliability of the target can be improved.
  • the sputtering target is a sintered body composed of In, Sn, O, and unavoidable impurities, and Sn / (In + Sn) is 1.8% or more and 3.7% or less (inclusive) (Except 3.7%), the average crystal grain size of the sintered body is in the range of 1.0 to 5.0 ⁇ m, and the pores with the major axis diameter of 0.1 to 1.0 ⁇ m are the area
  • the ratio is 0.5% or less, and the indium oxide phase and the tin oxide rich phase are two phases.
  • the area ratio of the tin oxide rich phase is 0.1 to 1.0% or less, and the tin oxide rich phase is 95%. % Or more is present at the grain boundary triple point.
  • the average crystal grain size is less than 1.0 ⁇ m, there is a problem that the density does not increase because the crystal grain size is too small, and when it exceeds 5.0 ⁇ m, the bending strength of the sintered body is less than 100 MPa. Since it occurs, it is not preferable.
  • the area ratio of pores having a major axis diameter of 0.1 to 1.0 ⁇ m is set to 0.5% or less because the presence of pores not only leads to a decrease in density but also the residual pores. Since it may cause arcing due to gas etc., it is better to use as little as possible.
  • the holes having a major axis diameter of less than 0.1 ⁇ m in the sintered body can be ignored because they do not affect the characteristics of the target.
  • pores exceeding 1.0 ⁇ m must be excluded.
  • the structure of the sintered body becomes two phases of an indium oxide phase and a tin oxide rich phase. In the area analysis by EPMA, the area ratio of the tin oxide-rich phase needs to be 0.1 to 1.0% or less. This is a necessary condition for realizing a sintered body having a small average crystal grain size and obtaining the characteristics of the sputtering target of the present invention.
  • the present invention requires that 95% or more of the tin oxide-rich phase is present at the grain boundary triple point.
  • the target is uniformly dispersed, and a tin oxide-rich phase is present as a dispersed state at the grain boundary triple point
  • the “grain boundary triple point” means that the particles in contact with each other are 3 This means that a tin oxide-rich phase is present in the almost central part of the individual assembly.
  • a low temperature 100 ° C. ⁇ 20 ° C. from the sintering holding temperature in the cooling step. It is necessary to hold in.
  • the ITO sputtering target can further increase the conductivity by setting the sintered body density to a high density of 7.03 g / cm 3 or more and the bulk resistivity to 0.10 to 0.15 m ⁇ ⁇ cm.
  • the maximum size of the tin oxide-rich phase is desirably 1 ⁇ m, and a target that suppresses the coarsening of the tin oxide-rich phase is preferable.
  • Indium oxide of the present invention in the production of sintered bodies ITO sputtering target made of tin oxide and unavoidable impurities, the SnO 2 powder and In 2 O 3 powder, with Sn / (In + Sn) atomic ratio, 1.8% The ratio is adjusted so as to be 3.7% or less (excluding 3.7%) and mixed, and sintering is performed in an oxygen atmosphere while maintaining the maximum sintering temperature at 1450 ° C. or less. .
  • the indium oxide-tin oxide based oxide (ITO) sintered body target of the present invention can be produced by a process of mixing, pulverizing, molding and sintering each raw material powder.
  • the raw material powder it is desirable to use indium oxide powder and tin oxide powder having a specific surface area of about 5 m 2 / g.
  • the indium oxide powder has a bulk density of 0.3 to 0.8 g / cm 3 , a median diameter (D 50 ) of 0.5 to 2.5 ⁇ m, and a specific surface area of 3.0 to 6.0 m 2.
  • tin oxide powder bulk density: 0.2 to 0.6 g / cm 3
  • specific surface area 3.0 to 6.0 m 2 / g use.
  • Each raw material powder is weighed so as to have a desired composition ratio, and then mixed and ground.
  • pulverization methods depending on the desired particle size and the material to be pulverized, but a wet medium stirring mill such as a bead mill is suitable.
  • a slurry in which powder is dispersed in water is forcibly stirred together with a grinding medium such as zirconia or alumina, which is a material with high hardness, and a pulverized powder can be obtained with high efficiency.
  • the pulverizing medium is also worn at this time, the pulverizing medium itself is mixed as an impurity in the pulverized powder.
  • the pulverization amount is defined by the difference in specific surface area before and after pulverization, the pulverization amount is almost proportional to the input energy to the powder in the wet medium stirring mill. Therefore, when performing pulverization, it is important that the wet medium stirring mill manages the integrated power.
  • the difference in specific surface area before and after pulverization ( ⁇ BET) is 0.5 to 5.0 m 2 / g, and the median diameter (D 50 ) after pulverization is 2.5 ⁇ m or less.
  • the finely pulverized slurry is granulated. This is because by improving the fluidity of the powder by granulation, the powder is uniformly filled in the mold at the time of press molding in the next step, and a homogeneous molded body is obtained.
  • granulation There are various types of granulation, and one method for obtaining granulated powder suitable for press molding is a method using a spray-type drying device (spray dryer). This is a method in which powder is dispersed as slurry in hot air and dried instantaneously, and spherical granulated powder of 10 to 500 ⁇ m can be continuously obtained.
  • strength can be improved by adding binders, such as polyvinyl alcohol (PVA), in a slurry, and making it contain in granulated powder.
  • PVA polyvinyl alcohol
  • the amount of PVA added was PVA 4 to 10 wt. % Of the aqueous solution containing 50 to 250 cc / kg of the raw material powder.
  • the crushing strength of the granulated powder during press molding can be adjusted by adding a plasticizer suitable for the binder.
  • a method for improving the strength of the molded body by adding a small amount of water to the obtained granulated powder to wet it. In drying with a spray dryer, it is important to control the inlet temperature and outlet temperature of hot air.
  • the temperature difference between the inlet and outlet is large, the amount of drying per unit time will increase and the productivity will improve, but if the inlet temperature is too high, the powder and added binder will change in quality due to heat, and the desired characteristics May not be obtained. In addition, when the outlet temperature is too low, the granulated powder may not be sufficiently dried.
  • press molding is performed.
  • the granulated powder is filled into a mold and molded by holding a pressure of 400 to 1000 kgf / cm 2 for 1 to 3 minutes.
  • a pressure of 400 to 1000 kgf / cm 2 When the pressure is less than 400 kgf / cm 2 , a molded body having sufficient strength and density cannot be obtained.
  • the pressure When the pressure is 1000 kgf / cm 2 or more, the molded body itself is out of pressure when taken out from the mold. It may break due to deformation due to being released, which is not preferable in production.
  • the molded body is sintered in an oxygen atmosphere to obtain a sintered body.
  • Sintering is performed at a sintering temperature of 1450 ° C. or lower.
  • the sintering temperature exceeds 1450 ° C., the structure of the sintered body becomes a single phase and the crystal grain size becomes coarse, so the upper limit is preferably set to 1450 ° C.
  • a binder removal step or the like may be introduced as needed during the temperature rise to the sintering temperature.
  • the holding time at the sintering temperature is shorter than 2 hours, the sintering does not proceed sufficiently, and the density of the sintered body does not increase sufficiently, or the sintered body warps. Even if the holding time exceeds 100 hours, unnecessary energy and time is wasted, which is not preferable for production. Preferably, it is 5 to 20 hours.
  • the atmosphere during cooling when the temperature is lowered is an air atmosphere or an oxygen atmosphere, and is maintained at a temperature lower than the maximum holding temperature of 100 ° C. ⁇ 20 ° C. for about 1 hour, so that 95% or more of the tin oxide rich phase exists at the grain boundary triple point can do. This is because solid solution of Sn precipitates during cooling, and by maintaining at a low temperature of 100 ° C.
  • the holding time may be 1 hour or longer, but no significant change is observed. This holding time can be appropriately adjusted in consideration of the holding temperature and the like, and is not particularly limited as long as a desired structure is obtained.
  • the bulk resistivity can be measured using, for example, NP-5, model: ⁇ -5 +.
  • NP-5 model: ⁇ -5 +.
  • a volume resistivity can be calculated by multiplying the obtained resistance by a sample thickness and a correction coefficient RCF (Resistency Correction Factor).
  • the sintered body sintered under these conditions has a sintered body density of 7.03 g / cm 3 or higher, a bulk resistivity of 0.10 to 0.15 m ⁇ ⁇ cm, It is possible to improve conductivity. Further, the maximum size of the tin oxide rich phase can be set to 1 ⁇ m, and the target can be prevented from being coarsened. Moreover, the strength of the target can be increased by setting the bending strength of the sintered body of the ITO sputtering target to 100 MPa or more.
  • the surface of the sintered body thus obtained is ground, and the side is further cut into a size of 127 mm ⁇ 508 mm with a diamond cutter.
  • an oxygen-free copper backing plate is placed on a hot plate set at 200 ° C., and indium is used as a brazing material, and the thickness is applied to be about 0.2 mm.
  • An ITO sintered body is bonded onto the backing plate and allowed to cool to room temperature.
  • This target was attached to a SYNCHRON magnetron sputtering system (BSC-7011), the input power was 2.3 W / cm 2 with a DC power source, the gas pressure was 0.6 Pa, and the sputtering gas was argon (Ar) and oxygen (O 2 ). Film formation is performed with a total gas flow rate of 300 sccm and an oxygen concentration of 0 to 4%.
  • the substrate is not heated or maintained at 150 ° C. or less in a mixed gas atmosphere composed of argon and oxygen and having an oxygen concentration of 4% or less, and the ITO sputtering of the present invention is performed. It is preferable to form a film on a substrate using a target.
  • the substrate may be not only a glass substrate but also a film substrate such as PET.
  • the transparent conductive film thus prepared is a transparent conductive film made of In, Sn, O, and inevitable impurities, and Sn / (In + Sn) is 1.8% or more and 3.7% or less (by atomic ratio). However, it contains Sn that is not 3.7%), the resistivity of the film in non-heated film formation is 3.0 m ⁇ ⁇ cm or less, and the transmittance at a wavelength of 550 nm is 80% or more.
  • a transparent conductive film can be obtained.
  • a transparent conductive film containing Sn having an atomic ratio of Sn / (In + Sn) of 2.3 to 3.2% and including In, Sn, O, and unavoidable impurities may be used.
  • the produced transparent conductive film can be made into crystallization temperature 120 degrees C or less.
  • the observed part of the target is divided into four equal parts, the central part of the four equally divided sintered bodies is two visual fields, and the total eight visual fields are the observed parts.
  • a specific example of the observation location is indicated by ⁇ in FIG.
  • the upper left figure in FIG. 4 shows a round sintered body, the right figure in FIG. 4 shows a square sintered body, and the lower left figure in FIG. 4 shows a cylindrical type.
  • the code method was used as a method for measuring the average crystal grain size.
  • a straight line is drawn from a grain boundary to a grain boundary in an arbitrary direction on an SEM image of x2,000 times, and the average of the length of the line crossing one particle is defined as an average crystal grain size.
  • An arbitrary straight line (from the grain boundary to the grain boundary) is drawn on the SEM image (photograph), the number of intersections with the grain boundary is counted, and the following (Formula 1) is calculated.
  • the sample was etched with aqua regia after mirror polishing.
  • the SEM images were taken with FE-EPMA (JXA-8500F type FE electron probe microanalyzer manufactured by JEOL Ltd.).
  • the vacancies were observed using a SEM image of x2,000 times.
  • the holes have a substantially circular shape (including a perfect circle), an elliptical shape, and a distorted circular shape, and each of the largest diameter portion and the major axis diameter (including the diameter) were measured.
  • the pore area ratio was determined from the histogram using the SEM image of 8 fields of x2,000 magnification, after grayscale / binarization processing in Adobe Photoshop Elements 7.0, from the histogram (average area of 8 fields of view) Ratio) was calculated.
  • the sample was etched with aqua regia after mirror polishing.
  • the SEM images were taken with FE-EPMA (JXA-8500F type FE electron probe microanalyzer manufactured by JEOL Ltd.).
  • FIG. 1 is based on FE-EPMA (JXA-8500F type FE electron probe microanalyzer manufactured by JEOL Ltd.) of an ITO sintered body containing Sn with an atomic ratio of Sn / (In + Sn) of 3.8%. Although it is a surface analysis result of Sn x2000 times, a tin oxide rich phase refers to a phase (white part in an image) whose Sn intensity is stronger than other phases.
  • FE-EPMA JXA-8500F type FE electron probe microanalyzer manufactured by JEOL Ltd.
  • FIG. 1 is a diagram (image) showing the analysis result of the Sn plane of an ITO sintered body containing Sn with an atomic ratio of Sn / (In + Sn) of 3.8%, and the right side is an SEM image.
  • FIG. The maximum size of the tin oxide-rich phase refers to the maximum major axis diameter in the image 8 field of view.
  • Indium oxide phase A phase other than the tin oxide rich phase in the Sn plane analysis result of FIG. 1 is defined as an indium oxide phase.
  • Grain boundary triple point A in FIG. 2 is an SEM image of an ITO sintered body containing 2.8% Sn / (In + Sn) in atomic ratio, and a line is drawn along the grain boundary in FIG. And it becomes like B of FIG.
  • the grain boundary triple point refers to the intersection of the grain boundaries of three grains, as indicated by the ⁇ portion in B of FIG.
  • a circled portion B in FIG. 2 indicates a portion that is not a grain boundary triple point.
  • C in FIG. 2 is an Sn surface analysis result in the same field of view as A in FIG. 2, and a portion surrounded by a round dotted line is a tin oxide rich phase.
  • 2C is overlapped with A in FIG. 2 to confirm whether the tin oxide rich phase is located at the grain boundary triple point, and the number of tin oxide rich phases and the tin oxide rich phase located at the grain boundary triple point. Confirm that the ratio of the number is 95% or more in all 8 fields of view.
  • 2D is an SEM image obtained by superimposing A in FIG. 2 and C in FIG.
  • arcing detection sensitivity The number of arcing (micro arc) occurrences (times) was measured with a micro arc monitor (MAM Genesis) manufactured by Landmark Technology.
  • the arcing criteria were as follows: arcing with a detection voltage of 100 V or more and emission energy (sputtering voltage when sputtering occurred ⁇ sputtering current ⁇ generation time) of 20 mJ or less was counted.
  • FIG. 3 is a photograph of a target after 35 hours of continuous sputtering. A white dotted line frame is photographed with a digital camera, and after gray scale / binarization processing (see FIG. 3) at Adobe Photoshop Elements 7.0, nodules are obtained from the histogram. The area ratio was calculated, and the average of the three locations was defined as the nodule coverage.
  • Example 1 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.8% in terms of atomic ratio.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 5 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.070 g / cm 3 , a bending strength of 115 MPa, a bulk resistivity of 0.110 m ⁇ ⁇ cm, an average crystal grain size of 3.43 ⁇ m, and an area ratio of a tin oxide-rich phase of 0.7.
  • the tin oxide rich phase triple point existence probability was 98%, and the hole area ratio was 0.08%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 28 times / 24 hr, and the nodule coverage was as good as 1%.
  • the results are shown in Table 1.
  • Example 2 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.8% in terms of atomic ratio.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.100 g / cm 3 , a bending strength of 120 MPa, a bulk resistivity of 0.116 m ⁇ ⁇ cm, an average crystal grain size of 3.54 ⁇ m, and a tin oxide-rich phase area ratio of 0.1.
  • the tin oxide rich phase triple point existence probability was 99%, and the hole area ratio was 0.07%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of arcing occurrences was 23/24 hr, and the nodule coverage was as good as 0.8%.
  • Example 2 the same DC power density and gas pressure were used, and argon was used as the sputtering gas, the oxygen content was 0, 1, 2, 4%, and the glass substrate (EagleXG) was formed without heating at a gas flow rate of 300 sccm.
  • a 40 nm ITO film was prepared. This membrane is heated to 50 to 200 ° C. in an air atmosphere for 60 minutes using an inert oven furnace (model number: INL-45-S), and the film before and after heating is XRD (apparatus model: Rigaku_Fully Automatic Horizontal Model) Multi-purpose X-ray diffractometer (SmartLab) measurement confirmed the presence or absence of crystallization.
  • the crystallization temperature was a temperature at which the peak of the (222) plane of In 2 O 3 was observed by XRD measurement.
  • the film resistivity When the oxygen concentration was 0%, the film resistivity was 2.70 m ⁇ ⁇ cm, the transmittance at a wavelength of 500 nm was 80.5%, and the crystallization temperature was 100 ° C.
  • the film resistivity When the oxygen concentration was 1%, the film resistivity was 1.01 m ⁇ ⁇ cm, the transmittance at a wavelength of 500 nm was 84.0%, and the crystallization temperature was 100 ° C.
  • the oxygen concentration was 2%, the film resistivity was 0.59 m ⁇ ⁇ cm, the transmittance at a wavelength of 500 nm was 88.1%, and the crystallization temperature was 100 ° C.
  • Example 3 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.8% in terms of atomic ratio.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 15 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.105 g / cm 3 , a bending strength of 121 MPa, a bulk resistivity of 0.124 m ⁇ ⁇ cm, an average crystal grain size of 3.66 ⁇ m, and a tin oxide-rich phase area ratio of 0.1.
  • tin oxide rich phase triple point existence probability 99%, pore area ratio was 0.05%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 20 times / 24 hr, and the nodule coverage was as good as 0.3%.
  • Example 4 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.8% in terms of atomic ratio.
  • the maximum sintering temperature was 1430 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.082 g / cm 3 , a bending strength of 116 MPa, a bulk resistivity of 0.118 m ⁇ ⁇ cm, an average crystal grain size of 3.26 ⁇ m, and an area ratio of a tin oxide-rich phase of 0.
  • the tin oxide rich phase triple point existence probability was 99%, and the hole area ratio was 0.10%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 25/24 hr, and the nodule coverage was as good as 0.7%.
  • Example 5 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.8% in terms of atomic ratio.
  • the maximum sintering temperature was 1400 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.058 g / cm 3 , a bending strength of 113 MPa, a bulk resistivity of 0.121 m ⁇ ⁇ cm, an average crystal grain size of 3.20 ⁇ m, and an area ratio of a tin oxide-rich phase of 0.
  • tin oxide rich phase triple point existence probability was 98%
  • pore area ratio was 0.15%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 31 times / 24 hr, and the nodule coverage was good at 1.2%.
  • Example 6 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 1.8% in terms of atomic ratio.
  • the maximum sintering temperature was 1350 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.036 g / cm 3 , a bending strength of 110 MPa, a bulk resistivity of 0.129 m ⁇ ⁇ cm, an average crystal grain size of 3.01 ⁇ m, and a tin oxide-rich phase area ratio of 0.001.
  • the tin oxide rich phase triple point existence probability was 97%, and the hole area ratio was 0.23%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 40 times / 24 hr, and the nodule coverage was as good as 1.5%.
  • Example 7 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 1.8% in terms of atomic ratio.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.074 g / cm 3 , a bending strength of 111 MPa, a bulk resistivity of 0.131 m ⁇ ⁇ cm, an average crystal grain size of 3.96 ⁇ m, and a tin oxide-rich phase area ratio of 0.8.
  • tin oxide-rich phase triple point existence probability was 99%, and the hole area ratio was 0.08%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 31 times / 24 hr, and the nodule coverage was as good as 0.9%.
  • Example 7 argon was used as the sputtering gas with the same DC power density and gas pressure, the oxygen content was 0, 1, 2, and 4%, and the glass substrate (EagleXG) was formed without heating at a gas flow rate of 300 sccm.
  • a 40 nm ITO film was prepared. This membrane is heated to 50 to 200 ° C. in an air atmosphere for 60 minutes using an inert oven furnace (model number: INL-45-S), and the film before and after heating is XRD (apparatus model: Rigaku_Fully Automatic Horizontal Model) Multi-purpose X-ray diffractometer (SmartLab) measurement confirmed the presence or absence of crystallization.
  • the crystallization temperature was a temperature at which the peak of the (222) plane of In 2 O 3 was observed by XRD measurement.
  • the film resistivity was 2.93 m ⁇ ⁇ cm
  • the transmittance at a wavelength of 500 nm was 81.1%
  • the crystallization temperature was 80 ° C.
  • the film resistivity was 1.33 m ⁇ ⁇ cm
  • the transmittance at a wavelength of 500 nm was 83.2%
  • the crystallization temperature was 80 ° C.
  • the film resistivity was 0.65 m ⁇ ⁇ cm
  • the transmittance at a wavelength of 500 nm was 88.7%
  • the crystallization temperature was 80 ° C.
  • Example 8 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 1.8% in terms of atomic ratio.
  • the maximum sintering temperature was 1400 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.045 g / cm 3 , a bending strength of 107 MPa, a bulk resistivity of 0.125 m ⁇ ⁇ cm, an average crystal grain size of 3.46 ⁇ m, and an area ratio of a tin oxide-rich phase of 0.
  • the tin oxide rich phase triple point existence probability was 99%, and the hole area ratio was 0.11%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 33 times / 24 hr, and the nodule coverage was good at 1.2%.
  • Example 9 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.1% in terms of atomic ratio.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained, the sintered body density 7.079g / cm 3, flexural strength 113MPa, bulk resistivity 0.125m ⁇ ⁇ cm, an average crystal grain size 3.55Myuemu, the area ratio of the tin oxide-rich phase 0.
  • tin oxide-rich phase triple point existence probability was 99%, and the hole area ratio was 0.12%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 30 times / 24 hr, and the nodule coverage was as good as 1.3%.
  • Example 10 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.1% in terms of atomic ratio.
  • the maximum sintering temperature was 1400 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.050 g / cm 3 , a bending strength of 110 MPa, a bulk resistivity of 0.122 m ⁇ ⁇ cm, an average crystal grain size of 2.75 ⁇ m, and a tin oxide-rich phase area ratio of 0.7.
  • the tin oxide rich phase triple point existence probability was 99%, and the hole area ratio was 0.13%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of arcing occurrences was 31 times / 24 hr, and the nodule coverage was as good as 1.6%.
  • Example 11 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.6% in terms of atomic ratio.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.088 g / cm 3 , a bending strength of 119 MPa, a bulk resistivity of 0.123 m ⁇ ⁇ cm, an average crystal grain size of 2.97 ⁇ m, and an area ratio of a tin oxide-rich phase of 0.
  • tin oxide rich phase triple point existence probability was 98%
  • hole area ratio was 0.10%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 25 times / 24 hr, and the nodule coverage was as good as 1%.
  • Example 12 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 2.6% in terms of atomic ratio.
  • the maximum sintering temperature was 1400 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.071 g / cm 3 , a bending strength of 115 MPa, a bulk resistivity of 0.119 m ⁇ ⁇ cm, an average crystal grain size of 2.83 ⁇ m, and a tin oxide-rich phase area ratio of 0.001.
  • the tin oxide rich phase triple point existence probability was 98%, and the hole area ratio was 0.10%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 28 times / 24 hr, and the nodule coverage was as good as 1.1%.
  • Example 13 Sintering was carried out using SnO 2 powder and In 2 O 3 powder, the ratio of which was adjusted so that Sn / (In + Sn) was 3.0% in terms of atomic ratio, in an oxygen atmosphere as a sintering raw material.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.103 g / cm 3 , a bending strength of 126 MPa, a bulk resistivity of 0.117 m ⁇ ⁇ cm, an average crystal grain size of 3.67 ⁇ m, and a tin oxide-rich phase area ratio of 0.1.
  • the tin oxide rich phase triple point existence probability was 41%, and the pore area ratio was 0.08%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 21 times / 24 hr, and the nodule coverage was as good as 0.9%.
  • Example 14 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 3.0% in terms of atomic ratio.
  • the maximum sintering temperature was 1400 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.091 g / cm 3 , a bending strength of 121 MPa, a bulk resistivity of 0.115 m ⁇ ⁇ cm, an average crystal grain size of 3.49 ⁇ m, and a tin oxide-rich phase area ratio of 0.001.
  • tin oxide rich phase triple point existence probability was 98%
  • pore area ratio was 0.09%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 24 times / 24 hr, and the nodule coverage was as good as 0.9%.
  • Example 15 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 3.2% in terms of atomic ratio.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.109 g / cm 3 , a bending strength of 127 MPa, a bulk resistivity of 0.110 m ⁇ ⁇ cm, an average crystal grain size of 3.82 ⁇ m, and a tin oxide-rich phase area ratio of 0.1.
  • the tin oxide rich phase triple point existence probability was 98%, and the hole area ratio was 0.07%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of arcing occurrences was 18 times / 24 hr, and the nodule coverage was as good as 0.7%.
  • Example 15 the same DC power density and gas pressure, argon as the sputtering gas, oxygen content of 0, 1, 2, and 4%, gas flow rate of 300 sccm, and heating to the glass substrate (Eagle XG) without heating.
  • a 40 nm ITO film was prepared.
  • This membrane is heated to 50 to 200 ° C. in an air atmosphere for 60 minutes using an inert oven furnace (model number: INL-45-S), and the film before and after heating is XRD (apparatus model: Rigaku_Fully Automatic Horizontal Model) Multi-purpose X-ray diffractometer (SmartLab) measurement confirmed the presence or absence of crystallization. Crystallization temperature and a temperature peak is observed in the In 2 of O 3 (222) plane by XRD measurement.
  • the film resistivity When the oxygen concentration was 0%, the film resistivity was 2.65 m ⁇ ⁇ cm, the transmittance at a wavelength of 500 nm was 80.1%, and the crystallization temperature was 110 ° C. When the oxygen concentration was 1%, the film resistivity was 0.97 m ⁇ ⁇ cm, the transmittance at a wavelength of 500 nm was 83.6%, and the crystallization temperature was 110 ° C. When the oxygen concentration was 2%, the film resistivity was 0.60 m ⁇ ⁇ cm, the transmittance at a wavelength of 500 nm was 89.2%, and the crystallization temperature was 110 ° C.
  • Example 16 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 3.2% in terms of atomic ratio.
  • the maximum sintering temperature was 1400 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained has a sintered body density of 7.100 g / cm 3 , a bending strength of 123 MPa, a bulk resistivity of 0.104 m ⁇ ⁇ cm, an average crystal grain size of 3.77 ⁇ m, and a tin oxide-rich phase area ratio of 0.1.
  • tin oxide-rich phase triple point existence probability was 98%
  • hole area ratio was 0.06%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of arcing occurrences was 18 times / 24 hr, and the nodule coverage was as good as 0.6%.
  • Example 17 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 3.5% in terms of atomic ratio.
  • the maximum sintering temperature was 1450 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it hold
  • the sintered body thus obtained had a sintered body density of 7.112 g / cm 3 , a bending strength of 130 MPa, a bulk resistivity of 0.111 m ⁇ ⁇ cm, an average crystal grain size of 4.02 ⁇ m, and a tin oxide-rich phase area ratio of 0.001.
  • a target was prepared by using this sintered body, DC power density 2.3 W / cm 2, the gas pressure is 0.6 Pa, the sputtering gas is argon (Ar), was subjected to a continuous 35 hours sputtering at a gas flow rate 300sccm However, the number of occurrences of arcing was 15 times / 24 hr, and the nodule coverage was as good as 0.6%.
  • Example 18 Sintering was carried out in an oxygen atmosphere using SnO 2 powder and In 2 O 3 powder whose ratios were adjusted so that Sn / (In + Sn) was 3.5% in terms of atomic ratio.
  • the maximum sintering temperature was 1400 ° C., and the holding time at the maximum sintering temperature was 10 hours. Then, it kept at 1300 degreeC for 1 hour at the time of temperature-fall cooling.
  • the sintered body thus obtained has a sintered body density of 7.102 g / cm 3 , a bending strength of 128 MPa, a bulk resistivity of 0.106 m ⁇ ⁇ cm, an average crystal grain size of 3.89 ⁇ m, a tin oxide-rich phase area ratio of 0.1.
  • tin oxide-rich phase triple point existence probability was 97%
  • the pore area ratio was 0.05%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 14 times / 24 hr, and the nodule coverage was good at 0.5%.
  • tin oxide-rich phase triple point existence probability was 0%, and the hole area ratio was 0.52%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 120 times / 24 hr, and the nodule coverage was 2.5%, which was not satisfactory because the conditions of the present invention were not satisfied.
  • tin oxide-rich phase triple point existence probability was 99%, and the hole area ratio was 0.68%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 148 times / 24 hr, and the nodule coverage was 3.1%, which did not satisfy the conditions of the present invention, and was unsatisfactory.
  • tin oxide-rich phase triple point existence probability was 94%
  • hole area ratio was 0.20%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 334 times / 24 hr, and the nodule coverage was 4.8%.
  • tin oxide-rich phase triple point existence probability was 0%, and the pore area ratio was 0.55%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 100 times / 24 hr, and the nodule coverage was 2.6%, which did not satisfy the conditions of the present invention and was defective.
  • tin oxide-rich phase triple point existence probability was 0%, and the hole area ratio was 0.63%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 114 times / 24 hr, and the nodule coverage was 2.9%, which was not satisfactory because the conditions of the present invention were not satisfied.
  • tin oxide-rich phase triple point existence probability was 0%, and the hole area ratio was 0.62%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 128 times / 24 hr, and the nodule coverage was 2.9%, which did not satisfy the conditions of the present invention and was defective.
  • tin oxide-rich phase triple point existence probability was 99%, and the hole area ratio was 0.66%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 145 times / 24 hr, and the nodule coverage was 3.3%, which did not satisfy the conditions of the present invention and was defective.
  • tin oxide-rich phase triple point existence probability was 0%, and the pore area ratio was 0.78%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 138 times / 24 hr, and the nodule coverage was 3.2%, which did not satisfy the conditions of the present invention, and was unsatisfactory.
  • the sputtering gas was argon
  • the oxygen content was 0, 1, 2, 4%
  • the gas flow rate was 300 sccm
  • the glass substrate was not heated.
  • a 40 nm ITO film was prepared. This membrane is heated to 50-200 ° C in an air atmosphere for 60 minutes using an inert gas oven furnace (model number: INL-45-S), and the film before and after heating is XRD (apparatus model number: manufactured by Rigaku_fully automatic horizontal type)
  • the presence or absence of crystallization was confirmed by multipurpose X-ray diffractometer SmartLab) measurement.
  • the crystallization temperature was a temperature at which the peak of the (222) plane of In 2 O 3 was observed by XRD measurement.
  • the film resistivity When the oxygen concentration was 0%, the film resistivity was 6.21 m ⁇ ⁇ cm, the transmittance at a wavelength of 500 nm was 72.9%, and the crystallization temperature was 50 ° C.
  • the oxygen concentration was 1%
  • the film resistivity was 4.60 m ⁇ ⁇ cm
  • the transmittance at a wavelength of 500 nm was 76.3%
  • the crystallization temperature was 50 ° C.
  • the oxygen concentration was 2%
  • the film resistivity When the oxygen concentration was 2%, the film resistivity was 3.01 m ⁇ ⁇ cm, the transmittance at a wavelength of 500 nm was 78.7%, and the crystallization temperature was 50 ° C.
  • tin oxide-rich phase triple point existence probability was 0%, and the hole area ratio was 0.85%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 162 times / 24 hr, and the nodule coverage was 3.5%, which did not satisfy the conditions of the present invention and was defective.
  • tin oxide-rich phase triple point existence probability was 0%, and the hole area ratio was 0.88%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 173 times / 24 hr, and the nodule coverage was 3.8%, which did not satisfy the conditions of the present invention and was defective.
  • tin oxide-rich phase triple point existence probability was 0%, and the hole area ratio was 1.02%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 199 times / 24 hr, and the nodule coverage was 1.3%.
  • the tin oxide rich phase triple point existence probability was 92% and the pore area ratio was 0.22%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 60 times / 24 hr, and the nodule coverage was 1.3%, which did not satisfy the conditions of the present invention, and was defective.
  • the same DC power density and gas pressure were used, and the sputtering gas was argon, the oxygen content was 0, 1, 2, 4%, and the glass substrate (EagleXG) was heated without heating at a gas flow rate of 300 sccm.
  • a 40 nm ITO film was prepared. This film was heated to 50 to 200 ° C. in an air atmosphere for 60 minutes using an inert gas oven furnace (model number: INL-45-S), and the film before and after heating was XRD (apparatus model: Rigaku_Fully Automatic Horizontal Model) The presence or absence of crystallization was confirmed by multipurpose X-ray diffractometer SmartLab) measurement. The crystallization temperature was a temperature at which the peak of the (222) plane of In 2 O 3 was observed by XRD measurement.
  • the film resistivity was 2.74 m ⁇ ⁇ cm
  • the transmittance at a wavelength of 500 nm was 77.1%
  • the crystallization temperature was 130 ° C.
  • the film resistivity was 0.99 m ⁇ ⁇ cm
  • the transmittance at a wavelength of 500 nm was 84.6%
  • the crystallization temperature was 130 ° C.
  • the film resistivity was 0.61 m ⁇ ⁇ cm
  • the transmittance at a wavelength of 500 nm was 86.8%
  • the crystallization temperature was 130 ° C.
  • the tin oxide rich phase triple point existence probability was 91% and the pore area ratio was 0.07%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 156 times / 24 hr, and the nodule coverage was 2.0%, which was not satisfactory because the conditions of the present invention were not satisfied.
  • the tin oxide rich phase triple point existence probability was 92%, and the hole area ratio was 0.06%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 140 times / 24 hr, and the nodule coverage was 2.2%, which did not satisfy the conditions of the present invention and was defective.
  • tin oxide-rich phase triple point existence probability 90%, pore area ratio was 0.07%.
  • a target was prepared using this sintered body, and sputtering was performed continuously at a DC power density of 2.3 W / cm 2 , a gas pressure of 0.6 Pa, a sputtering gas of argon (Ar), and a gas flow rate of 300 sccm for 35 hours.
  • the number of occurrences of arcing was 230 times / 24 hr, and the nodule coverage was 2.6%, which did not satisfy the conditions of the present invention and was defective.
  • Example 8 and Comparative Example 12 were described and other examples and comparative examples were omitted, this is for the purpose of avoiding complexity, and it is added that similar results are obtained.
  • the present invention relates to an ITO sputtering target having a low tin oxide composition suitable for forming a transparent conductive film and capable of obtaining a low resistance film even at a low temperature, and has a small target particle size, high density, and high strength.
  • An ITO sputtering target capable of reducing arcing and nodules can be provided.
  • it is possible to reduce the change in film characteristics accompanying the progress of sputtering and to improve the quality of film formation. As a result, there is an excellent effect that the productivity and reliability of the ITO target can be improved.
  • the ITO sputtering target of the present invention is particularly useful for forming an ITO film and is optimal for applications such as a touch panel, a flat panel display, an organic EL, and a solar cell.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Non-Insulated Conductors (AREA)
  • Manufacturing Of Electric Cables (AREA)
PCT/JP2015/081123 2014-11-07 2015-11-05 Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜及びｉｔｏ透明導電膜の製造方法 WO2016072441A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
KR1020187023361A KR20180093140A (ko) 2014-11-07 2015-11-05 Ito 스퍼터링 타겟 및 그 제조 방법 그리고 ito 투명 도전막 및 ito 투명 도전막의 제조 방법
JP2016557791A JP6291593B2 (ja) 2014-11-07 2015-11-05 Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜の製造方法
KR1020167031994A KR102030892B1 (ko) 2014-11-07 2015-11-05 Ito 스퍼터링 타겟 및 그 제조 방법 그리고 ito 투명 도전막 및 ito 투명 도전막의 제조 방법
CN201580023075.4A CN106460161B (zh) 2014-11-07 2015-11-05 Ito溅射靶及其制造方法和ito透明导电膜及ito透明导电膜的制造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2014226601 2014-11-07
JP2014-226601 2014-11-07

Publications (1)

Publication Number Publication Date
WO2016072441A1 true WO2016072441A1 (ja) 2016-05-12

Family

ID=55909165

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2015/081123 WO2016072441A1 (ja) 2014-11-07 2015-11-05 Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜及びｉｔｏ透明導電膜の製造方法

Country Status (5)

Country Link
JP (1) JP6291593B2 (ko)
KR (2) KR102030892B1 (ko)
CN (1) CN106460161B (ko)
TW (1) TWI594970B (ko)
WO (1) WO2016072441A1 (ko)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020143359A (ja) * 2019-03-08 2020-09-10 Ｊｘ金属株式会社 スパッタリングターゲット部材の製造方法及びスパッタリングターゲット部材
JP2020164930A (ja) * 2019-03-29 2020-10-08 Ｊｘ金属株式会社 Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜及びｉｔｏ透明導電膜の製造方法
JP2022017241A (ja) * 2020-02-03 2022-01-25 日東電工株式会社 積層体、タッチセンサ、調光素子、光電変換素子、熱線制御部材、アンテナ、電磁波シールド部材および画像表示装置
JP2022019756A (ja) * 2020-03-19 2022-01-27 日東電工株式会社 透明導電層および透明導電性シート
CN114574824A (zh) * 2018-03-30 2022-06-03 Ｊｘ金属株式会社 溅射靶部件及其制造方法
WO2024105854A1 (ja) * 2022-11-17 2024-05-23 日本電信電話株式会社 リチウム二次電池、及び、リチウム二次電池の製造方法
JP7492916B2 (ja) 2019-06-27 2024-05-30 日東電工株式会社 透明導電性フィルム

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11908596B2 (en) 2020-02-03 2024-02-20 Nitto Denko Corporation Transparent conductive layer, transparent conductive sheet, touch sensor, light control element, photoelectric conversion element, heat ray control member, antenna, electromagnetic wave shield member, and image display device
CN113735565B (zh) * 2021-08-30 2022-11-15 深圳市众诚达应用材料科技有限公司 低锡含量ito溅射靶材、制备方法及薄膜太阳能电池

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09125236A (ja) * 1995-10-30 1997-05-13 Hitachi Metals Ltd インジウム酸化物系焼結体およびその製造方法ならびにインジウム酸化物系ターゲット
JP2000113732A (ja) * 1998-06-25 2000-04-21 Asahi Glass Co Ltd 透明導電膜とその製造方法、透明導電膜付き基板およびタッチパネル
WO2003014409A1 (fr) * 2001-08-02 2003-02-20 Idemitsu Kosan Co., Ltd. Cible de pulverisation, film conducteur transparent et leur procede de fabrication
JP2004323877A (ja) * 2003-04-22 2004-11-18 Sumitomo Metal Mining Co Ltd Ｉｔｏ薄膜作製用ターゲットとその製造方法
JP2005126766A (ja) * 2003-10-23 2005-05-19 Sumitomo Metal Mining Co Ltd 酸化インジウム系ターゲットおよびその製造方法
JP2011065937A (ja) * 2009-09-18 2011-03-31 Toppan Printing Co Ltd 透明導電性薄膜及びその製造方法
WO2013172055A1 (ja) * 2012-05-17 2013-11-21 株式会社カネカ 透明電極付き基板およびその製造方法、ならびにタッチパネル
WO2014156234A1 (ja) * 2013-03-29 2014-10-02 Jx日鉱日石金属株式会社 Ｉｔｏスパッタリングターゲット及びその製造方法
WO2015125588A1 (ja) * 2014-02-18 2015-08-27 三井金属鉱業株式会社 Ｉｔｏスパッタリングターゲット材およびその製造方法

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4934926A (ko) 1972-08-05 1974-03-30
JPS503759A (ko) 1973-05-15 1975-01-16
JPS526983A (en) 1975-07-08 1977-01-19 Tokyo Shibaura Electric Co Locking device for key
JP2750483B2 (ja) 1991-11-26 1998-05-13 株式会社 ジャパンエナジー Ｉｔｏスパッタリングターゲット
JPH10147862A (ja) 1996-11-15 1998-06-02 Sumitomo Metal Mining Co Ltd 酸化インジウム・酸化錫焼結体
JP2000233969A (ja) 1998-12-08 2000-08-29 Tosoh Corp Ｉｔｏスパッタリングターゲットおよび透明導電膜の製造方法
JP3721080B2 (ja) * 1999-05-10 2005-11-30 株式会社日鉱マテリアルズ スパッタリングターゲット及びその製造方法
KR100663617B1 (ko) 2001-03-12 2007-01-05 닛코킨조쿠 가부시키가이샤 아이티오 스퍼터링 타겟트용 산화 주석 분말 및 아이티오막형성용 소결체 스퍼터링 타겟트
JP3988411B2 (ja) 2001-06-22 2007-10-10 住友金属鉱山株式会社 Ｉｔｏ焼結体とその製造方法、及びそれを用いたｉｔｏスパッタリングターゲット
JP2009040621A (ja) 2007-08-06 2009-02-26 Mitsui Mining & Smelting Co Ltd Ｉｔｏ焼結体およびｉｔｏスパッタリングターゲット
KR101580321B1 (ko) * 2009-04-29 2015-12-23 삼성전기주식회사 티탄산바륨의 제조방법 및 그 방법에 의하여 제조된 티탄산바륨
JP2012126937A (ja) 2010-12-13 2012-07-05 Sumitomo Metal Mining Co Ltd Ｉｔｏスパッタリングターゲットとその製造方法

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09125236A (ja) * 1995-10-30 1997-05-13 Hitachi Metals Ltd インジウム酸化物系焼結体およびその製造方法ならびにインジウム酸化物系ターゲット
JP2000113732A (ja) * 1998-06-25 2000-04-21 Asahi Glass Co Ltd 透明導電膜とその製造方法、透明導電膜付き基板およびタッチパネル
WO2003014409A1 (fr) * 2001-08-02 2003-02-20 Idemitsu Kosan Co., Ltd. Cible de pulverisation, film conducteur transparent et leur procede de fabrication
JP2004323877A (ja) * 2003-04-22 2004-11-18 Sumitomo Metal Mining Co Ltd Ｉｔｏ薄膜作製用ターゲットとその製造方法
JP2005126766A (ja) * 2003-10-23 2005-05-19 Sumitomo Metal Mining Co Ltd 酸化インジウム系ターゲットおよびその製造方法
JP2011065937A (ja) * 2009-09-18 2011-03-31 Toppan Printing Co Ltd 透明導電性薄膜及びその製造方法
WO2013172055A1 (ja) * 2012-05-17 2013-11-21 株式会社カネカ 透明電極付き基板およびその製造方法、ならびにタッチパネル
WO2014156234A1 (ja) * 2013-03-29 2014-10-02 Jx日鉱日石金属株式会社 Ｉｔｏスパッタリングターゲット及びその製造方法
WO2015125588A1 (ja) * 2014-02-18 2015-08-27 三井金属鉱業株式会社 Ｉｔｏスパッタリングターゲット材およびその製造方法

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114574824A (zh) * 2018-03-30 2022-06-03 Ｊｘ金属株式会社 溅射靶部件及其制造方法
JP2020143359A (ja) * 2019-03-08 2020-09-10 Ｊｘ金属株式会社 スパッタリングターゲット部材の製造方法及びスパッタリングターゲット部材
JP2020164930A (ja) * 2019-03-29 2020-10-08 Ｊｘ金属株式会社 Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜及びｉｔｏ透明導電膜の製造方法
JP7158102B2 (ja) 2019-03-29 2022-10-21 Ｊｘ金属株式会社 Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜及びｉｔｏ透明導電膜の製造方法
JP7492916B2 (ja) 2019-06-27 2024-05-30 日東電工株式会社 透明導電性フィルム
JP2022017241A (ja) * 2020-02-03 2022-01-25 日東電工株式会社 積層体、タッチセンサ、調光素子、光電変換素子、熱線制御部材、アンテナ、電磁波シールド部材および画像表示装置
JP7186271B2 (ja) 2020-02-03 2022-12-08 日東電工株式会社 積層体、タッチセンサ、調光素子、光電変換素子、熱線制御部材、アンテナ、電磁波シールド部材および画像表示装置
JP2022019756A (ja) * 2020-03-19 2022-01-27 日東電工株式会社 透明導電層および透明導電性シート
JP7273930B2 (ja) 2020-03-19 2023-05-15 日東電工株式会社 透明導電性シート
WO2024105854A1 (ja) * 2022-11-17 2024-05-23 日本電信電話株式会社 リチウム二次電池、及び、リチウム二次電池の製造方法

Also Published As

Publication number Publication date
JPWO2016072441A1 (ja) 2017-04-27
TW201630849A (zh) 2016-09-01
KR20160148593A (ko) 2016-12-26
CN106460161A (zh) 2017-02-22
KR102030892B1 (ko) 2019-10-10
TWI594970B (zh) 2017-08-11
JP6291593B2 (ja) 2018-03-14
KR20180093140A (ko) 2018-08-20
CN106460161B (zh) 2018-12-04

Similar Documents

Publication Publication Date Title
JP6291593B2 (ja) Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜の製造方法
TWI645059B (zh) 氧化銦－氧化鋅系（ｉｚｏ）濺鍍鈀及其製造方法
JP5887819B2 (ja) 酸化亜鉛焼結体、それから成るスパッタリングターゲットおよび酸化亜鉛薄膜
JP5764828B2 (ja) 酸化物焼結体およびそれを加工したタブレット
CN103717779A (zh) Zn-Sn-O系氧化物烧结体及其制造方法
WO2013042423A1 (ja) Ｚｎ－Ｓｉ－Ｏ系酸化物焼結体とその製造方法および透明導電膜
JP6078189B1 (ja) Ｉｚｏ焼結体スパッタリングターゲット及びその製造方法
EP2428500A1 (en) Indium oxide sintered body, indium oxide transparent conductive film, and method for manufacturing the transparent conductive film
JP5987105B2 (ja) Ｉｔｏスパッタリングターゲット及びその製造方法
JP6159867B1 (ja) 透明導電膜形成用ターゲット、透明導電膜形成用ターゲットの製造方法及び透明導電膜の製造方法
JP7158102B2 (ja) Ｉｔｏスパッタリングターゲット及びその製造方法並びにｉｔｏ透明導電膜及びｉｔｏ透明導電膜の製造方法
TWI778100B (zh) 氧化物燒結體及濺鍍靶
JP6885038B2 (ja) 酸化物焼結体、その製造方法及びスパッタリングターゲット
WO2012073879A1 (ja) スパッタリングターゲット
JP6343695B2 (ja) 酸化インジウム−酸化亜鉛系（ｉｚｏ）スパッタリングターゲット及びその製造方法
JP7178707B2 (ja) ＭｇＯ－ＴｉＯ系スパッタリングターゲットの製造方法
JP6800405B2 (ja) 酸化物焼結体、その製造方法及びスパッタリングターゲット
JP2010084177A (ja) 酸化亜鉛系焼結ターゲットおよびその製造方法
WO2013042747A1 (ja) 酸化物焼結体およびその製造方法並びに酸化物透明導電膜
JP5890671B2 (ja) Ｉｔｏスパッタリングターゲットの製造方法
JP5740992B2 (ja) 酸化物焼結体、それから成るターゲットおよび透明導電膜

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 15856447

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2016557791

Country of ref document: JP

Kind code of ref document: A

DPE1 Request for preliminary examination filed after expiration of 19th month from priority date (pct application filed from 20040101)
ENP Entry into the national phase

Ref document number: 20167031994

Country of ref document: KR

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 15856447

Country of ref document: EP

Kind code of ref document: A1