WO2015125588A1 - Matériau cible ito pour pulvérisation cathodique et son procédé de production - Google Patents

Matériau cible ito pour pulvérisation cathodique et son procédé de production Download PDF

Info

Publication number
WO2015125588A1
WO2015125588A1 PCT/JP2015/052688 JP2015052688W WO2015125588A1 WO 2015125588 A1 WO2015125588 A1 WO 2015125588A1 JP 2015052688 W JP2015052688 W JP 2015052688W WO 2015125588 A1 WO2015125588 A1 WO 2015125588A1
Authority
WO
WIPO (PCT)
Prior art keywords
ito
sintered body
firing
powder
target material
Prior art date
Application number
PCT/JP2015/052688
Other languages
English (en)
Japanese (ja)
Inventor
享祐 寺村
朋哉 武内
Original Assignee
三井金属鉱業株式会社
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 三井金属鉱業株式会社 filed Critical 三井金属鉱業株式会社
Priority to KR1020157033563A priority Critical patent/KR101583693B1/ko
Priority to CN201580000974.2A priority patent/CN105308002A/zh
Priority to JP2015526439A priority patent/JP5816394B1/ja
Publication of WO2015125588A1 publication Critical patent/WO2015125588A1/fr

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
    • 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
    • C04B35/457—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 based on tin oxides or stannates
    • 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
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising
    • 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
    • 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
    • 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
    • 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
    • C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
    • 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
    • C04B2235/02—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
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5409—Particle size related information expressed by specific surface values
    • 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/604—Pressing at temperatures other than sintering temperatures
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6565—Cooling rate
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
    • C04B2235/6585—Oxygen containing atmosphere, e.g. with changing oxygen pressures at an oxygen percentage above that of air
    • 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
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
    • 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
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
    • C04B2235/85—Intergranular or grain boundary phases

Definitions

  • the present invention relates to an ITO sputtering target material and a manufacturing method thereof.
  • a rotary magnetron cathode sputtering device has a magnetic field generator inside a cylindrical target and performs sputtering while rotating the target while cooling from the inside of the target.
  • the entire surface of the target material becomes eroded and becomes uniform. It is shaved.
  • the use efficiency of the target material is usually 20 to 30% in the flat plate type magnetron sputtering apparatus, whereas the use efficiency of the target material can be increased to 70% or more in the rotary magnetron cathode sputtering apparatus. High usage efficiency can be obtained.
  • rotary magnetron cathode sputtering apparatus by rotating the target, a larger power can be input per unit area than in the conventional flat plate type magnetron sputtering apparatus, so that a high deposition rate can be obtained.
  • Such a rotating cathode sputtering method is widely used for metal target materials that can be easily processed into a cylindrical shape and have high mechanical strength.
  • ceramics are low in strength and brittle, when processed into a cylindrical shape, cracks and deformations are likely to occur during manufacture and when bonded to a substrate. For this reason, it is a fact that ceramic sputtering targets are not sufficiently spread to the rotary cathode sputtering method.
  • An ITO (Indium-Tin-Oxide) film is widely used as a transparent electrode of a flat panel display because it has high permeability and electrical conductivity.
  • the ITO film is generally formed by sputtering an ITO sputtering target.
  • the ITO film is usually formed by using an ITO sputtering target containing about 10% by mass of SnO 2.
  • SnO 2 is formed.
  • An ITO sputtering target containing about 3% by mass is used.
  • ITO material contains less SnO 2, for example, ITO material content of SnO 2 is less than 7 mass% is brittle, it is known that easily broken. In particular, an ITO material having a SnO 2 content of 5% by mass or less is brittle and easily cracked. If such an ITO material with a low SnO 2 content is used in a cylindrical shape for use as a target material for a rotating cathode sputtering system, cracking is more likely to occur. Further, the ITO cylindrical sputtering target material having a small SnO 2 content as described above is likely to be cracked when bonded to a substrate.
  • an ITO cylindrical sputtering target material having a small SnO 2 content requires a more advanced crack prevention technology than a normal ceramic sputtering target material at the time of manufacturing and bonding.
  • Patent Document 1 discloses a technique for suppressing cracking when joining a cylindrical base material with uniform thermal expansion by setting the eccentricity of a ceramic cylindrical target material having a density of 98% or more to 0.2 mm or less. Is disclosed. However, in this technique, as in Example 1, cracks are generated even when the density is 98% or more and the eccentricity of the cylindrical target material is 0.2 mm or less. This is presumably because the coefficient of thermal expansion changes due to the difference in the thickness of the low melting point solder used for bonding and the distance from the heater to be heated.
  • Patent Document 2 describes that when the SnO 2 concentration is less than 10%, the strength decreases due to abnormal grain growth due to firing and cracks occur, and the SnO 2 content is 2.5 to 5.
  • a technique is disclosed in which cracks generated in a fired body are reduced and generation of cracks and nodules is suppressed by setting the density to 7.1 g / cm 3 or more in a 2% by mass ITO sputtering target.
  • this technology cannot prevent cracking for ITO targets with a density of 7.1 g / cm 3 or less, and cracks are generated with a cylindrical ITO target with high use efficiency even with a density of 7.1 g / cm 3 or more. There is a case.
  • the object of the present invention is an ITO sintered body that is less likely to be cracked or deformed in the machining process, even if it has a cylindrical shape that is liable to crack, and an ITO sputtering target material that is less likely to crack or deform in the joining process. And an ITO sputtering target, and a method for producing the ITO sintered body and the ITO sputtering target material.
  • the content of Sn is 2.5 to 10.0 mass% in the amount of SnO 2 terms present in the grain boundaries of the In 2 O 3 matrix and the In 2 O 3 matrix
  • An ITO sintered body having an In 4 Sn 3 O 12 phase The relative density is 98.0% or more, the average particle size of the In 2 O 3 matrix is 17 ⁇ m or less, and the area ratio of the In 4 Sn 3 O 12 phase in the cross section of the ITO sintered body is 0.00. 4% or more.
  • the ITO sintered body of the present invention can be cylindrical.
  • the ITO sputtering target material of the present invention comprises the ITO sintered body.
  • the ITO sputtering target of the present invention is formed by bonding the ITO sputtering target material to a base material with a bonding material.
  • the method for producing the ITO sintered body of the present invention is as follows. Including a firing step of firing the ITO molded body produced from the ITO raw material powder, and a cooling step of cooling the fired product obtained in the firing step, In the cooling step, cooling is performed at a temperature falling rate of 25 ° C./h or less in a temperature range of 1200 to 1350 ° C. and below a firing temperature for firing the ITO molded body.
  • the method for producing another ITO sintered body of the present invention is as follows. Including a firing step of firing the ITO molded body produced from the ITO raw material powder, and a cooling step of cooling the fired product obtained in the firing step, In the cooling step, cooling in a temperature range of 1200 to 1500 ° C. and lower than the firing temperature is performed at a temperature drop rate of 25 ° C./h or less.
  • the ITO molded body and the ITO sintered body can be cylindrical.
  • the manufacturing method of the ITO target material of the present invention manufactures an ITO sintered body by the manufacturing method described above, and processes the obtained ITO sintered body to manufacture a target material.
  • the ITO sintered body of the present invention has a cylindrical shape in which cracks and the like are likely to occur, cracks and deformations are unlikely to occur in the processing process. Even if the ITO sputtering target material of the present invention has a cylindrical shape in which cracking and the like are likely to occur, cracking and deformation are not likely to occur in the bonding process to the base material. For this reason, the ITO sintered compact and ITO sputtering target material of this invention can improve a manufacturing yield.
  • the method for producing an ITO sintered body of the present invention can produce the ITO sintered body efficiently.
  • FIG. 1 is a schematic diagram of the structure of an ITO sintered body and an ITO sputtering target material according to the present invention.
  • the ITO sintered body, the ITO sputtering target material and the ITO sputtering target according to the present invention and the method for producing the ITO sintered body and the ITO sputtering target material will be described in detail.
  • the shapes of the ITO sintered body and the ITO sputtering target material included in the present invention are not particularly limited, such as a flat plate shape and a cylindrical shape, but a great effect can be obtained particularly in a cylindrical shape in which cracking and deformation are likely to occur.
  • ITO sintered body of the present invention the content of Sn is 2.5 to 10.0 mass% in the amount of SnO 2 conversion, present in the grain boundary of the In 2 O 3 matrix and In 2 O 3 matrix
  • the area ratio of the In 4 Sn 3 O 12 phase in the cross section of the body is 0.4% or more.
  • FIG. 1 is a diagram schematically showing a structure image obtained by observing a cross section of an ITO sintered body and an ITO sputtering target material of the present invention with a scanning electron microscope.
  • reference numeral 1 is In 2 O 3 matrix
  • reference numeral 2 is In 4 Sn 3 O 12 phase.
  • the In 4 Sn 3 O 12 phase 2 is present at the grain boundary of the In 2 O 3 matrix 1.
  • the In 2 O 3 matrix in the present invention, In 2 O 3 to SnO 2 refers to a part solute to In 2 O 3 phase formed by.
  • the average particle size of the In 2 O 3 matrix is 17 ⁇ m or less, preferably 3 to 15 ⁇ m, more preferably 5 to 15 ⁇ m.
  • the particle diameter of the In 2 O 3 matrix is obtained as a horizontal ferret diameter on the tissue image.
  • the horizontal ferret diameter is a value obtained by particle analysis in the scanning electron microscope observation.
  • the average particle diameter of the In 2 O 3 matrix was determined by randomly observing 10 fields of view of 100 ⁇ m ⁇ 130 ⁇ m at a magnification of 1000 using a scanning electron microscope, and every In 2 O contained in each field of view.
  • the average horizontal fillet diameter for each visual field is calculated by averaging the values of the horizontal fillet diameters obtained for the three parent phases, and the average horizontal fillet diameters obtained in all visual fields are averaged.
  • the average particle diameter of the In 2 O 3 matrix is 17 ⁇ m or less, the ITO sintered body is difficult to break in the processing step, and the ITO sputtering target material obtained from the ITO sintered body is bonded to the substrate. Cracks and deformation are less likely to occur in the process.
  • the average particle size is small, the grain boundary increases and the resistance may increase, so that the average particle size of the In 2 O 3 matrix is preferably 3 ⁇ m or more.
  • the area ratio of the In 4 Sn 3 O 12 phase in the cross section is 0.4% or more, preferably 0.5 to 5%, more preferably 0.5 to 2. 5%.
  • the area ratio of the In 4 Sn 3 O 12 phase was determined by observing 10 visual fields of 33 ⁇ m ⁇ 43 ⁇ m at random using a scanning electron microscope in a cross section of the ITO sintered body. This is a numerical value obtained by calculating the percentage value of the total area of the In 4 Sn 3 O 12 phase in the visual field area (33 ⁇ 43 ⁇ m 2 ) and averaging the percentage values obtained in all visual fields. .
  • the In 4 Sn 3 O 12 phase is present in a large area at the grain boundary, so that the toughness is increased. Since it becomes higher and more resistant to cracking, the ITO sintered body becomes more difficult to break in the processing process, and the ITO sputtering target material obtained from the ITO sintered body is cracked and deformed in the bonding process to the base material It becomes difficult to do.
  • the area ratio is preferably 5% or less from the viewpoint that the In 4 Sn 3 O 12 phase is less likely to cause arcing and nodules during sputtering.
  • the ITO sintered body of the present invention has a Sn content of 2.5 to 10.0% by mass in terms of SnO 2 content.
  • Sn content When the Sn content is within the above range, it can be effectively used as a sputtering target material, and cracking and deformation are less likely to occur during processing and bonding to a substrate.
  • Sn content when the Sn content is 2.5 to 6.0% by mass in terms of SnO 2, an ITO sputtering target for producing a transparent electrode of a flat panel display or a touch panel from the ITO sintered body of the present invention.
  • the material can be manufactured.
  • the conventional ITO sintered body having a Sn content of 2.5 to 6.0% by mass in terms of SnO 2 is brittle and easy to break, but the ITO sintered body of the present invention is Sn Even if the content of is in the above range, it is difficult to break. Further, when the Sn content is 3.0 to 5.0% by mass in terms of SnO 2 , a useful ITO sputtering target material can be produced, and cracks in processing and bonding to the substrate Deformation can be effectively prevented.
  • the ITO sintered body of the present invention has a relative density of 98.0% or more, preferably 98.5% or more, more preferably 99.0% or more. When the relative density is less than 98.0%, the strength becomes insufficient and the film tends to crack.
  • the ITO sintered body of the present invention is sufficiently suppressed from cracking in the processing step, and further the ITO firing is further suppressed.
  • the ITO sputtering target material obtained from the bonded body is sufficiently suppressed from being cracked or deformed in the bonding step to the base material.
  • the conventional ITO sintered body having a cylindrical shape was likely to be cracked or deformed, but the ITO sintered body of the present invention was cracked or deformed in the processing step even if it was cylindrical. Hateful.
  • a cylindrical ITO product for example, an ITO cylindrical sputtering target material can be suitably manufactured from the cylindrical ITO sintered body.
  • the size of the ITO sintered body of the present invention is not particularly limited.
  • the ITO cylindrical sintered body is processed into a sputtering target material, its size is approximately an outer diameter of 140 to 170 mm, an inner diameter of 110 to 140 mm, and a length of 50 mm or more. The length is appropriately determined according to the application.
  • ⁇ ITO sputtering target material> The ITO sputtering target material of this invention consists of the said ITO sintered compact.
  • the ITO sputtering target material of the present invention is produced by appropriately processing the ITO sintered body, for example, cutting.
  • the ITO sputtering target material of the present invention relates to the Sn content, the relative density, the average particle size of the In 2 O 3 matrix, and the area ratio of the In 4 Sn 3 O 12 phase that the ITO sintered body satisfies. All conditions are met. The description of these conditions in the ITO sputtering target material of the present invention is the same as the description of these conditions described in the ITO sintered body.
  • the ITO sputtering target material of the present invention satisfies the above conditions, it has high strength and is not easily cracked or deformed.
  • the ITO sputtering target material When the ITO sputtering target material is used for sputtering, it is usually joined to a base material made of titanium or the like using solder.
  • this bonding usually involves heating the target material and the cylindrical base material, applying solder to the inner peripheral surface of the target material and the outer peripheral surface of the cylindrical base material, and in the cavity of the target material.
  • a cylindrical base material is inserted into the two, and the two solder layers are combined, and then cooled. During this cooling, stress is generated in the target material due to the difference in thermal expansion coefficient between the target material and the base material.
  • the conventional ITO cylindrical sputtering target material could not resist the stress and was often cracked in the joining process.
  • the ITO sputtering target of the present invention is formed by bonding the ITO sputtering target material to a base material with a bonding material.
  • the substrate usually has a flat plate shape or a cylindrical shape to which a sputtering target material can be bonded.
  • a sputtering target material can be bonded.
  • limiting in particular in the kind of base material It can select from the base material used conventionally and can be used. Examples of the base material include stainless steel and titanium.
  • the type of the bonding material is not particularly limited, and can be appropriately selected from conventionally used bonding materials.
  • Examples of the bonding material include indium solder.
  • a plurality of sputtering target materials may be bonded to one base material.
  • one ITO cylindrical sputtering target material may be bonded to the outside of a single substrate, or two or more may be aligned and bonded on the same axis.
  • the gap between the ITO cylindrical sputtering target materials that is, the length of the divided portion is usually 0.05 to 0.5 mm. As the length of the divided portion is shorter, arcing is less likely to occur during sputtering, but if it is less than 0.05 mm, the target materials may collide with each other due to thermal expansion during the joining process or sputtering.
  • the manufacturing method of the ITO sintered body of the present invention includes a firing step of firing the ITO molded body, and a step of cooling the fired product obtained in the firing step, and the first aspect is the cooling step, Cooling in a temperature range of 1200 to 1500 ° C. and below the temperature at which the ITO molded body is fired is performed at a temperature drop rate of 25 ° C./h or less, and the second aspect is 1200 to 1350 in the cooling step. Cooling is performed at a temperature lowering rate of 25 ° C./h or less in a temperature range of 0 ° C. and below the temperature at which the ITO molded body is fired.
  • the ITO sintered body of the present invention can be efficiently manufactured without generating cracks or deformations, but the manufacturing method of the ITO sintered body of the present invention is as follows.
  • the manufacturing conditions are not limited except for the manufacturing conditions described above, and are not limited to the following manufacturing methods.
  • a preferred embodiment of the method for producing an ITO sintered body according to the present invention includes a step 1 of preparing a granule from a slurry containing a raw material powder and an organic additive, a step 2 of producing a molded body by CIP molding the granule, Step 3 includes degreasing the molded body, Step 4 for firing the degreased molded body, and Step 5 for cooling the fired product obtained in the firing step.
  • Process 1 In step 1, granules are prepared from a slurry containing raw material powder and organic additives.
  • the filling property of the raw materials is improved, and a high-density molded body can be obtained. Further, uneven filling is less likely to occur, and uniform filling is possible. Uneven press is less likely to occur.
  • the raw material powder a mixed powder of In 2 O 3 powder and SnO 2 powder can be used, and the ITO powder may be used alone or mixed with In 2 O 3 powder and SnO 2 powder.
  • the ITO powder when a powder mixture of these raw material powders used for preparing granules and an ITO powder are used alone, the ITO powder is also referred to as an ITO raw material powder.
  • SnO 2 powder and ITO powder each have a specific surface area of usually 1 to 40 m 2 / g measured by BET (Brunauer-Emmett-Teller) method.
  • the mixing ratio of the In 2 O 3 powder, the SnO 2 powder, and the ITO powder is appropriately determined so that the content of the constituent elements in the sintered body is within the aforementioned range.
  • the Sn content in terms of SnO 2 in the finally obtained sintered body is 5.0 mass%
  • the Sn content in terms of SnO 2 in the sintered body is 5.
  • the ratio of each raw material powder contained in ITO raw material powder is determined so that it may become 0 mass%.
  • the content (mass%) of the SnO 2 powder in the ITO raw material powder is finally obtained. It has been confirmed that it can be equated with the Sn content (mass%) in terms of SnO 2 in the body and the target material. Further, when the ITO raw material powder containing the ITO powder, the total content of SnO 2 powder in the ITO raw material powder and (mass%) the content of Sn in the amount of SnO 2 in terms of ITO powder and (mass%) It has been confirmed that it can be equated with the Sn content (mass%) in terms of SnO 2 in the finally obtained sintered body and target material.
  • each powder and zirconia balls can be put in a pot and mixed by ball mill.
  • the organic additive is a substance added to suitably adjust the properties of the slurry and the molded body.
  • examples of the organic additive include a binder, a dispersant, and a plasticizer.
  • the amount of the organic additive is preferably 0.3 to 2.0 mass% with respect to the amount of the ITO raw material powder.
  • the blending amount of the organic additive is more than 2.0% by mass, the strength of the molded body during the removal of the solvent is greatly reduced, and degreasing cracks easily occur. It may be difficult to increase the density.
  • the said compounding quantity of an organic additive is less than 0.3 mass%, sufficient effect of each component may not be acquired.
  • the blending amount of the organic additive is within the above range, an ITO sintered body having a relative density of 98.0% or more can be produced.
  • the binder is added to bind the ITO raw material powder in the molded body and increase the strength of the molded body.
  • the binder normally used when obtaining a molded object in the well-known powder sintering method can be used.
  • Dispersant is added to increase the dispersibility of the raw material powder and binder in the slurry.
  • examples of the dispersant include ammonium polycarboxylate and ammonium polyacrylate.
  • the plasticizer is added to increase the plasticity of the molded body.
  • the plasticizer include polyethylene glycol (PEG) and ethylene glycol (EG).
  • the dispersion medium used when preparing the slurry containing the raw material powder and the organic additive is not particularly limited, and can be appropriately selected from water, alcohol and the like according to the purpose.
  • the method for preparing the slurry containing the raw material powder and the organic additive is not particularly limited, and for example, a method in which the raw material powder, the organic additive, and the dispersion medium are placed in a pot and ball mill mixed can be used.
  • step 2 the granule prepared in step 1 is CIP-molded (Cold Isostatic Pressing) to produce a molded body. If the shape of the molded body is flat, an ITO flat sintered body is obtained, and if it is cylindrical, an ITO cylindrical sintered body is obtained.
  • the pressure during CIP molding is usually 800 kgf / cm 2 or more. The higher the pressure, the denser the granules can be made, and the compact can be densified and strengthened.
  • Process 3 the molded body produced in step 2 is degreased. Degreasing is performed by heating the compact.
  • the degreasing temperature is usually 600 to 800 ° C, preferably 700 to 800 ° C, more preferably 750 to 800 ° C.
  • the higher the degreasing temperature the higher the strength of the molded body. However, when the temperature exceeds 800 ° C, shrinkage of the molded body occurs. (Process 4) In step 4, that is, the firing step, the molded body degreased in step 3 is fired.
  • the firing furnace is not particularly limited, and a firing furnace conventionally used for manufacturing an ITO sintered body can be used.
  • the firing temperature is usually 1450 to 1700 ° C., preferably 1500 to 1650 ° C., more preferably 1500 to 1600 ° C.
  • the firing temperature is too high, the sintered structure of the sintered body becomes enlarged and easily cracked.
  • the firing time is usually 3 to 30 hours, preferably 5 to 20 hours, more preferably 8 to 16 hours. The longer the firing time, the more easily the sintered body is densified. However, when the firing time is too long, the sintered structure of the sintered body is enlarged and easily broken.
  • the heating rate is usually 100 to 500 ° C./h.
  • the firing atmosphere is usually an oxygen atmosphere.
  • Process 5 the fired product obtained in step 4 is cooled.
  • the cooling step the temperature is lowered or kept constant.
  • the cooling rate when cooling the obtained fired product is in a range of 1200 ° C. to 1500 ° C. and not more than the firing temperature.
  • a range hereinafter also referred to as a specific temperature range
  • it is 25 ° C./h or less, preferably 20 ° C./h or less, more preferably 15 ° C./h or less, and further preferably 10 ° C./h or less. That is, when the firing temperature of the molded body is 1500 ° C. or higher, the temperature lowering rate in the temperature range of 1200 ° C. to 1500 ° C. is set to 25 ° C./h or lower.
  • the temperature lowering rate in the temperature range from 1200 ° C. to the firing temperature is set to 25 ° C./h or less.
  • the rate of temperature decrease in the temperature range of 1200 to 1450 ° C. is set to 25 ° C./h or less.
  • the area ratio of the In 4 Sn 3 O 12 phase and the particle size of the In 2 O 3 matrix can be controlled by setting the temperature lowering rate in the specific temperature range to 25 ° C./h or less.
  • the lower the temperature decrease rate in the specific temperature range the larger the area of the In 4 Sn 3 O 12 phase can be increased, and the excessive increase in the particle size of the In 2 O 3 matrix can be suppressed. There is no.
  • the temperature decrease rate in the specific temperature range does not need to be constant, and may vary within a range of 25 ° C./h or less, and there may be time for the temperature decrease rate to be 0 ° C./h in the specific temperature range. .
  • a temperature range other than the specific temperature range that is, when the firing temperature of the molded body is higher than 1500 ° C, a temperature range from the firing temperature to 1500 ° C and a temperature range lower than 1200 ° C, and a firing temperature of the molded body is 1500 ° C or less.
  • the rate of temperature decrease is usually 10 to 100 ° C./h, preferably 20 to 70 ° C./h, more preferably 20 to 50 ° C./h. Cracks due to thermal stress differences are less likely to occur as the rate of temperature drop is smaller, but the thermal stress difference does not normally change even when the temperature is lower than 10 ° C./h.
  • the cooling rate when cooling the obtained fired product is in the range of 1200 ° C. to 1350 ° C. and lower than the firing temperature. In the range, 25 ° C./h or less, preferably 20 ° C./h or less, more preferably 15 ° C./h or less, and further preferably 10 ° C./h or less.
  • the first aspect is more efficiently implemented.
  • the time required for the process can be further shortened, or the cooling rate in the temperature range of 1200 ° C. to 1350 ° C., which is particularly important for tissue formation, can be controlled more precisely to obtain a desired structure. It can be done.
  • the implementation conditions of the second aspect are the same as those of the first aspect except for the temperature range that regulates the temperature drop rate.
  • the cooling atmosphere is usually an oxygen atmosphere.
  • the ITO sintered body is obtained by cooling the fired product.
  • the above-described ITO sintered body of the present invention can be efficiently manufactured by the above-mentioned ITO sintered body manufacturing method.
  • ⁇ Method for producing ITO cylindrical target material> The manufacturing method of the ITO target material of this invention manufactures an ITO sintered compact with the manufacturing method of the above-mentioned ITO sintered compact, processes the obtained ITO sintered compact, and manufactures an ITO target material. Usually, if the shape of the sintered body is flat, an ITO flat target material is manufactured, and if it is cylindrical, an ITO cylindrical target material is manufactured.
  • the processing method of the ITO sintered body is appropriately selected according to the target ITO target material.
  • Examples of the processing method include cutting.
  • the evaluation methods of the ITO sintered body and the ITO sputtering target material obtained in the examples and comparative examples are as follows. 1. Relative density The relative density of the ITO sintered body was measured based on the Archimedes method. Specifically, the air weight of the ITO sintered body is divided by the volume (the weight of the ITO sintered body in water / the specific gravity of water at the measurement temperature), and the theoretical density ⁇ (g / cm 3 ) based on the following formula (X) The percentage value was defined as the relative density (unit:%).
  • C 1 to C i indicate the content (% by weight) of the constituent material of the sintered body
  • ⁇ 1 to ⁇ i are the density (g of each constituent material corresponding to C 1 to C i ). / Cm 3 ).
  • In 2 O 3 Average particle diameter average value of the horizontal Feret's diameter of the average particle diameter of In 2 O 3 matrix of the matrix phase, was determined as follows.
  • the cut surface obtained by cutting the ITO sintered body with a diamond cutter is polished step by step using emery paper # 170, # 320, # 800, # 1500, # 2000, and finally buffed to give a mirror surface. After finishing, the etching solution at 40 ° C.
  • particle analysis software particle analysis version 3.0, manufactured by Sumitomo Metal Technology Co., Ltd.
  • an SEM image of a crystal grain was traced and image recognition was performed with a scanner, and this image was binarized.
  • the conversion value was set so that one pixel was displayed in units of ⁇ m.
  • the area of the In 4 Sn 3 O 12 phase was determined, and the percentage value with respect to the visual field area (33 ⁇ 43 ⁇ m 2 ) was determined as the area ratio.
  • the average value of the area ratio obtained in 10 fields of view was taken as the area ratio of the In 4 Sn 3 O 12 phase in the ITO sintered body.
  • Example 1 And In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 2 It mix
  • the slurry was supplied to a spray drying apparatus, and spray drying was performed under the conditions of an atomizing rotation speed of 14,000 rpm, an inlet temperature of 200 ° C., and an outlet temperature of 80 ° C. to prepare granules.
  • the granules were filled in a 300 mm ⁇ 500 mm mold and molded by a cold press method at a pressure of 200 kgf / cm 2 to produce a flat temporary molded body.
  • the temporary molded body was vacuum-packed and CIP molded at a pressure of 800 kgf / cm 2 to produce a flat molded body.
  • the molded body was heat degreased.
  • the degreasing temperature was 600 ° C.
  • the degreasing time was 10 hours
  • the heating rate was 20 ° C./h in the temperature range up to 400 ° C., and 50 ° C./h in the temperature range higher than 400 ° C.
  • the degreased compact was fired in an oxygen atmosphere under conditions of a firing temperature of 1500 ° C., a firing time of 12 hours, and a heating rate of 300 ° C./h.
  • the fired product obtained was cooled at a temperature lowering rate of 10 ° C./h in a temperature range of 1500 ° C. to 1200 ° C. and a temperature lowering rate outside the temperature range of 50 ° C./h.
  • the relative density of the obtained sintered body was 98.6%
  • the average particle size of the In 2 O 3 mother phase was 7.0 ⁇ m
  • the area ratio of the In 4 Sn 3 O 12 phase was 0.8%.
  • the obtained sintered body was cut to produce 30 ITO flat plate sputtering target materials having a short side of 200 mm, a long side of 350 mm, and a thickness of 9 mm. No cracks occurred in 1 of 30 sheets by the above processing.
  • the nine target materials were joined to a copper backing plate in a row with In solder so that the long sides of the adjacent target materials face each other, thereby producing an ITO target.
  • the interval between the target materials was 0.5 mm.
  • the joining was performed by heating the target material and the backing plate to 150 ° C., applying indium solder to the joining surfaces of the target material and the backing plate, matching the solder layers of both, and then cooling.
  • Example 2 And In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 3 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1500 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1500 ° C. to 1200 ° C. was 20 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 98.8%, the average particle diameter of the In 2 O 3 parent phase and the area ratio of the In 4 Sn 3 O 12 phase were 9.5 ⁇ m and 0.5%, respectively.
  • the obtained sintered body was cut to produce 30 ITO flat plate sputtering target materials having a short side of 200 mm, a long side of 350 mm, and a thickness of 9 mm. No cracks occurred in 1 of 30 sheets by the above processing.
  • Example 3 In 2 O 3 powder, which is the ratio measured specific surface area by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 5 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1500 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1500 ° C. to 1200 ° C. was 15 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 99.2%, the average particle size of the In 2 O 3 matrix and the area ratio of the In 4 Sn 3 O 12 phase were 11.5 ⁇ m and 0.7%, respectively.
  • the obtained sintered body was cut to produce 30 ITO flat plate sputtering target materials having a short side of 200 mm, a long side of 350 mm, and a thickness of 9 mm. No cracks occurred in 1 of 30 sheets by the above processing.
  • Example 4 In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 2 It mix
  • the slurry was supplied to a spray drying apparatus, and spray drying was performed under the conditions of an atomizing rotation speed of 14,000 rpm, an inlet temperature of 200 ° C., and an outlet temperature of 80 ° C. to prepare granules.
  • a cylindrical urethane rubber mold having an inner diameter of 220 mm (thickness 10 mm) having a cylindrical core (mandrel) with an outer diameter of 150 mm and a length of 450 mm is filled while tapping the granules, and after sealing the rubber mold, 800 kgf CIP molding was performed at a pressure of / cm 2 to produce a cylindrical molded body.
  • the molded body was heat degreased.
  • the degreasing temperature was 600 ° C.
  • the degreasing time was 10 hours
  • the heating rate was 20 ° C./h in the temperature range up to 400 ° C., and 50 ° C./h in the temperature range higher than 400 ° C.
  • the degreased molded body was fired in an oxygen atmosphere under conditions of a firing temperature of 1500 ° C., a firing time of 12 hours, and a heating rate of 300 ° C./h.
  • the fired product obtained was cooled at a temperature lowering rate of 10 ° C./h in a temperature range of 1500 ° C. to 1200 ° C. and a temperature lowering rate outside the temperature range of 50 ° C./h.
  • the relative density of the obtained sintered body was 98.8%, the average particle size of the In 2 O 3 mother phase was 6.6 ⁇ m, and the area ratio of the In 4 Sn 3 O 12 phase was 0.9%.
  • the obtained sintered body was cut to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • the cutting was performed by processing the outer diameter using a grindstone, holding the outer diameter with a jig and processing the inner diameter, and then holding the inner diameter with a jig and finishing the outer diameter.
  • 30 ITO cylindrical sputtering target materials were manufactured.
  • Example 5 In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 3 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1470 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1470 ° C. to 1200 ° C. was 10 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 98.1%, the average particle diameter of the In 2 O 3 parent phase and the area ratio of the In 4 Sn 3 O 12 phase were 4.2 ⁇ m and 0.8%, respectively.
  • the obtained sintered body was cut to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. A crack occurred in 1 of 30 pieces by the above processing.
  • the nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • Example 6 And In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 3 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1520 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1500 ° C. to 1200 ° C. was 10 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 98.5%, the average particle diameter of the In 2 O 3 matrix and the area ratio of the In 4 Sn 3 O 12 phase were 10.8 ⁇ m and 0.9%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. None of the 30 cracks occurred by the above processing.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • Example 7 And In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 3 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1500 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1500 ° C. to 1200 ° C. was 20 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 98.4%, the average particle diameter of the In 2 O 3 matrix and the area ratio of the In 4 Sn 3 O 12 phase were 9.2 ⁇ m and 0.4%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. Cracks occurred in 2 out of 30 pieces by the above processing.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • Example 8 And In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 3 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1550 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1500 ° C. to 1200 ° C. was 10 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 99.2%, and the average particle size of the In 2 O 3 mother phase and the area ratio of the In 4 Sn 3 O 12 phase were 13.1 ⁇ m and 1.0%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. None of the 30 cracks occurred by the above processing.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • Example 9 And In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 5 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1470 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1470 ° C. to 1200 ° C. was 10 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 98.2%, the average particle diameter of the In 2 O 3 matrix and the area ratio of the In 4 Sn 3 O 12 phase were 5.3 ⁇ m and 2.2%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. None of the 30 cracks occurred by the above processing.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • Example 10 And In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 5 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1520 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1500 ° C. to 1200 ° C. was 10 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 99.2%, the average particle diameter of the In 2 O 3 mother phase and the area ratio of the In 4 Sn 3 O 12 phase were 11.3 ⁇ m and 1.8%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. None of the 30 cracks occurred by the above processing.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • Example 11 And In 2 O 3 powder, which is the ratio measured specific surface area by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 5 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1500 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1500 ° C. to 1200 ° C. was 15 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 99.0%, the average particle size of the In 2 O 3 parent phase, and the area ratio of the In 4 Sn 3 O 12 phase were 12.1 ⁇ m and 0.5%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. None of the 30 cracks occurred by the above processing.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • Example 12 And In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 5 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1600 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h.
  • the temperature lowering rate from 1500 ° C. to 1200 ° C. was 10 ° C./h, and the temperature lowering rate outside the above temperature range was 50 ° C./h.
  • the density of the obtained fired body was 99.5%, the average particle diameter of the In 2 O 3 matrix and the area ratio of the In 4 Sn 3 O 12 phase were 14.9 ⁇ m and 1.3%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. None of the 30 cracks occurred by the above processing.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1500 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h. The cooling rate was 50 ° C./h in all temperature ranges.
  • the density of the obtained fired body was 98.5%, the average particle size of the In 2 O 3 matrix and the area ratio of the In 4 Sn 3 O 12 phase were 15.1 ⁇ m and 0.1%, respectively.
  • the obtained sintered body was cut to produce 30 ITO flat plate sputtering target materials having a short side of 200 mm, a long side of 350 mm, and a thickness of 9 mm. Nine out of 30 sheets were cracked by the above processing.
  • Example 2 In 2 O 3 powder, which is the ratio specific surface area measured by the BET method was measured by SnO 2 powder and the BET method is 5 m 2 / g surface area of 5 m 2 / g, the content of SnO 2 powder 3 It mix
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1550 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h. The cooling rate was 50 ° C./h in all temperature ranges.
  • the density of the obtained fired body was 98.6%, the average particle diameter of the In 2 O 3 matrix and the area ratio of the In 4 Sn 3 O 12 phase were 17.7 ⁇ m and 0.1%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. Due to the above processing, cracks occurred in 12 out of 30 pieces.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1400 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h. The cooling rate was 50 ° C./h in all temperature ranges.
  • the density of the obtained fired body was 97.6%, the average particle diameter of the In 2 O 3 parent phase and the area ratio of the In 4 Sn 3 O 12 phase were 11.6 ⁇ m and 0.2%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured.
  • cracks occurred in 8 out of 30 pieces.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1400 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h. The temperature lowering rate was 20 ° C./h in all temperature ranges.
  • the density of the obtained fired body was 97.7%, the average particle size of the In 2 O 3 matrix and the area ratio of the In 4 Sn 3 O 12 phase were 6.3 ⁇ m and 0.5%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. Due to the above processing, cracks occurred in 4 out of 30 pieces.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1520 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h. The temperature lowering rate was 30 ° C./h in all temperature ranges.
  • the density of the obtained fired body was 98.6%, the average particle diameter of the In 2 O 3 parent phase and the area ratio of the In 4 Sn 3 O 12 phase were 18.1 ⁇ m and 0.3%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured.
  • cracks occurred in 6 out of 30 pieces.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm, to produce an ITO target.
  • the interval between the target materials was 0.5 mm.
  • the degreased molded body was fired to produce a sintered body. Firing was performed in an oxygen atmosphere at a firing temperature of 1550 ° C., a firing time of 12 hours, and a temperature increase rate of 300 ° C./h. The cooling rate was 50 ° C./h in all temperature ranges.
  • the density of the obtained fired body was 98.6%, the average particle diameter of the In 2 O 3 parent phase and the area ratio of the In 4 Sn 3 O 12 phase were 18.3 ⁇ m and 0.3%, respectively.
  • the obtained sintered body was cut in the same manner as in Example 4 to produce an ITO cylindrical sputtering target material having an outer diameter of 153 mm, an inner diameter of 135 mm, and a length of 300 mm.
  • 30 ITO cylindrical sputtering target materials were manufactured. Nine out of 30 cracks were generated by the above processing.
  • Example 4 In the same manner as in Example 4, nine target materials were joined with In solder to a titanium backing tube having an outer diameter of 133 mm, an inner diameter of 123 mm, and a length of 3200 mm to produce an ITO target.
  • the interval between the target materials was 0.5 mm.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (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)

Abstract

Cette invention concerne : un corps fritté ITO ayant une teneur en Sn de 2,5 à 10,0 % en poids en termes de SnO2, tout en comprenant une matrice In2O3 et une phase In4Sn3O12 qui est présente au joint de grain de la matrice In2O3, ledit corps fritté ayant une densité relative de 98,0 % ou plus, une taille de grain moyenne de matrice In2O3 de 17 µm ou moins, et un rapport de surface de phase In4Sn3O12 dans une coupe transversale du corps fritté ITO de 0,4 % ou plus ; et un matériau de cible ITO pour pulvérisation cathodique constitué dudit corps fritté ITO. Un corps fritté ITO selon l'invention n'est pas sujet à l'apparition de fissures ou à la déformation au cours d'une étape de traitement. Un matériau cible ITO pour pulvérisation cathodique selon l'invention n'est pas sujet à l'apparition de fissures ou à la déformation au cours d'une étape de liaison à une base. Par conséquent, le corps fritté ITO et le matériau de cible ITO pour pulvérisation cathodique selon l'invention sont capables d'améliorer le rendement de production.
PCT/JP2015/052688 2014-02-18 2015-01-30 Matériau cible ito pour pulvérisation cathodique et son procédé de production WO2015125588A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
KR1020157033563A KR101583693B1 (ko) 2014-02-18 2015-01-30 Ito 스퍼터링 타깃재 및 그 제조 방법
CN201580000974.2A CN105308002A (zh) 2014-02-18 2015-01-30 Ito溅射靶材及其制造方法
JP2015526439A JP5816394B1 (ja) 2014-02-18 2015-01-30 Ｉｔｏスパッタリングターゲット材およびその製造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2014028543 2014-02-18
JP2014-028543 2014-02-18

Publications (1)

Publication Number Publication Date
WO2015125588A1 true WO2015125588A1 (fr) 2015-08-27

Family

ID=53878100

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2015/052688 WO2015125588A1 (fr) 2014-02-18 2015-01-30 Matériau cible ito pour pulvérisation cathodique et son procédé de production

Country Status (5)

Country Link
JP (1) JP5816394B1 (fr)
KR (1) KR101583693B1 (fr)
CN (2) CN107253855A (fr)
TW (1) TWI522332B (fr)
WO (1) WO2015125588A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016072441A1 (fr) * 2014-11-07 2016-05-12 Ｊｘ金属株式会社 Cible de pulvérisation d'ito et procédé pour la fabriquer, film électroconducteur transparent d'ito, et procédé de fabrication de film électroconducteur transparent d'ito
JP2017190523A (ja) * 2016-04-12 2017-10-19 三菱マテリアル株式会社 円筒型スパッタリングターゲット

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016174877A1 (fr) * 2015-04-30 2016-11-03 三井金属鉱業株式会社 Matériau d'oxyde d'indium et d'étain (ito) pour cible de pulvérisation cathodique
KR20170113075A (ko) * 2016-03-28 2017-10-12 제이엑스금속주식회사 원통형 스퍼터링 타겟 및 그 제조 방법
JP2018178251A (ja) * 2017-04-07 2018-11-15 三菱マテリアル株式会社 円筒型スパッタリングターゲット及びその製造方法
CN113149614A (zh) * 2021-05-28 2021-07-23 通威太阳能（合肥）有限公司 一种烧结体、靶材及其制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07166341A (ja) * 1993-12-14 1995-06-27 Hitachi Metals Ltd インジウム・スズ酸化物膜用スパッタリング用ターゲットおよびその製造方法
JP2007231381A (ja) * 2006-03-01 2007-09-13 Tosoh Corp Ｉｔｏスパッタリングターゲットおよびその製造方法
WO2009020091A1 (fr) * 2007-08-06 2009-02-12 Mitsui Mining & Smelting Co., Ltd. Corps fritté d'ito et cible de pulvérisation cathodique d'ito
JP2010150611A (ja) * 2008-12-25 2010-07-08 Tosoh Corp 透明導電膜用焼結体及びスパッタリングターゲット並びにその製造方法
JP2011080116A (ja) * 2009-10-07 2011-04-21 Mitsui Mining & Smelting Co Ltd Ｉｔｏスパッタリングターゲットおよびその製造方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4961672B2 (ja) 2004-03-05 2012-06-27 東ソー株式会社 円筒形スパッタリングターゲット並びにセラミックス焼結体及びその製造方法
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
CN102718499B (zh) * 2012-07-10 2014-02-26 国家钽铌特种金属材料工程技术研究中心 一种含In4Sn3O12相ITO溅射靶的制造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07166341A (ja) * 1993-12-14 1995-06-27 Hitachi Metals Ltd インジウム・スズ酸化物膜用スパッタリング用ターゲットおよびその製造方法
JP2007231381A (ja) * 2006-03-01 2007-09-13 Tosoh Corp Ｉｔｏスパッタリングターゲットおよびその製造方法
WO2009020091A1 (fr) * 2007-08-06 2009-02-12 Mitsui Mining & Smelting Co., Ltd. Corps fritté d'ito et cible de pulvérisation cathodique d'ito
JP2010150611A (ja) * 2008-12-25 2010-07-08 Tosoh Corp 透明導電膜用焼結体及びスパッタリングターゲット並びにその製造方法
JP2011080116A (ja) * 2009-10-07 2011-04-21 Mitsui Mining & Smelting Co Ltd Ｉｔｏスパッタリングターゲットおよびその製造方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016072441A1 (fr) * 2014-11-07 2016-05-12 Ｊｘ金属株式会社 Cible de pulvérisation d'ito et procédé pour la fabriquer, film électroconducteur transparent d'ito, et procédé de fabrication de film électroconducteur transparent d'ito
JPWO2016072441A1 (ja) * 2014-11-07 2017-04-27 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
JP2017190523A (ja) * 2016-04-12 2017-10-19 三菱マテリアル株式会社 円筒型スパッタリングターゲット

Also Published As

Publication number Publication date
JP5816394B1 (ja) 2015-11-18
CN107253855A (zh) 2017-10-17
TWI522332B (zh) 2016-02-21
KR20150139623A (ko) 2015-12-11
TW201534572A (zh) 2015-09-16
KR101583693B1 (ko) 2016-01-08
JPWO2015125588A1 (ja) 2017-03-30
CN105308002A (zh) 2016-02-03

Similar Documents

Publication Publication Date Title
JP5816394B1 (ja) Ｉｔｏスパッタリングターゲット材およびその製造方法
JP5750060B2 (ja) セラミックス円筒形スパッタリングターゲット材およびその製造方法
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
JP6264846B2 (ja) 酸化物焼結体、スパッタリングターゲットおよびその製造方法
JPWO2016072441A1 (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
JP2012126937A (ja) Ｉｔｏスパッタリングターゲットとその製造方法
TWI573890B (zh) 濺鍍靶用靶材之製造方法及爪構件
TWI491580B (zh) 蒸鍍用錠及其製造方法
JP5218032B2 (ja) 透明導電膜用焼結体の製造方法
JP6412439B2 (ja) セラミックス製ターゲット材の製造方法および円筒形スパッタリングターゲットの製造方法
JP5784849B2 (ja) セラミックス円筒形スパッタリングターゲット材およびその製造方法
JP2014125422A (ja) 酸化物焼結体、酸化物焼結体スパッタリングターゲットおよびその製造方法
WO2016140021A1 (fr) Matériau cible céramique cylindrique creux, et cible de pulvérisation cathodique cylindrique creux
TWI723974B (zh) 圓筒形靶材之製造方法、圓筒形濺鍍靶及燒製用輔助具
JP2011080116A (ja) Ｉｔｏスパッタリングターゲットおよびその製造方法
TW201734239A (zh) 圓筒形陶瓷系濺射靶材及藉由於背襯管接合一個以上圓筒形陶瓷系濺射靶材而形成之圓筒形陶瓷系濺射靶件
JP2015089966A (ja) スパッタリングターゲット材およびその製造方法
KR20170142169A (ko) Ito 스퍼터링 타깃재
JP2010255022A (ja) Ｉｔｏスパッタリングターゲットとその製造方法
JP7480439B2 (ja) 酸化物焼結体及びその製造方法並びにスパッタリングターゲット材
JP2003055759A (ja) Ｍｇ含有ＩＴＯスパッタリングターゲットの製造方法
JP2016014191A (ja) セラミックス円筒形スパッタリングターゲット材およびその製造方法
TWI755648B (zh) 氧化物燒結體、濺鍍靶及氧化物薄膜之製造方法
TW202325683A (zh) 氧化物燒結體及其製造方法與濺鍍靶材

Legal Events

Date Code Title Description
WWE Wipo information: entry into national phase

Ref document number: 201580000974.2

Country of ref document: CN

ENP Entry into the national phase

Ref document number: 2015526439

Country of ref document: JP

Kind code of ref document: A

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

Ref document number: 15751274

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 20157033563

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: 15751274

Country of ref document: EP

Kind code of ref document: A1