WO2021241687A1 - Cible de pulvérisation et film fonctionnel optique - Google Patents

Cible de pulvérisation et film fonctionnel optique Download PDF

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Publication number
WO2021241687A1
WO2021241687A1 PCT/JP2021/020200 JP2021020200W WO2021241687A1 WO 2021241687 A1 WO2021241687 A1 WO 2021241687A1 JP 2021020200 W JP2021020200 W JP 2021020200W WO 2021241687 A1 WO2021241687 A1 WO 2021241687A1
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Prior art keywords
film
optical functional
less
component
functional film
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PCT/JP2021/020200
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English (en)
Japanese (ja)
Inventor
大亮 金子
啓太 梅本
幸也 杉内
晋 岡野
健志 大友
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三菱マテリアル株式会社
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Priority claimed from JP2021086830A external-priority patent/JP2021188133A/ja
Application filed by 三菱マテリアル株式会社 filed Critical 三菱マテリアル株式会社
Publication of WO2021241687A1 publication Critical patent/WO2021241687A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • 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
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only

Definitions

  • the present invention relates to a sputtering target used for forming an optical functional film that is laminated on a metal thin film or the like to reduce reflection of light from the metal thin film or the like, and an optical functional film.
  • a projection type capacitive touch panel has been adopted as an input means for a mobile terminal device or the like.
  • a sensing electrode is formed for touch position detection.
  • the electrode for sensing is usually formed by patterning, and an X electrode extending in the X direction and a Y electrode extending in the Y direction orthogonal to the X direction are formed on one surface of the transparent substrate. These are provided and arranged in a grid pattern.
  • the pattern of the electrodes is visually recognized from the outside because the metal thin film has a metallic luster. Therefore, it is conceivable to reduce the visibility of the electrode by forming a low-reflectance film having a low reflectance of visible light on the metal thin film.
  • a color filter for color display is adopted.
  • a black member called a black matrix is formed for the purpose of improving contrast and color purity and improving visibility.
  • the above-mentioned low reflectance film can also be used as this black matrix (hereinafter referred to as “BM”).
  • a back electrode of the solar cell when sunlight is incident through a glass substrate or the like, a back electrode of the solar cell is formed on the opposite side thereof.
  • a metal thin film such as molybdenum (Mo) or silver (Ag) is used.
  • Mo molybdenum
  • Ag silver
  • patterning is performed by etching, for example, as described in Patent Documents 1 and 2.
  • patterning is performed using an etching solution containing hydrogen peroxide.
  • the etching property by the etching solution containing hydrogen peroxide is excellent, but the heat resistance is insufficient.
  • the low reflectance film described in Patent Document 2 is a copper oxynitride film (CuNO film) and has excellent heat resistance, but the etching property by an etching solution containing hydrogen peroxide is insufficient. Met.
  • the present invention has been made in view of the above-mentioned circumstances, and is excellent in etching property and heat resistance by an etching solution containing hydrogen peroxide, and can sufficiently suppress reflection of light from a metal thin film or the like. It is an object of the present invention to provide a sputtering target for forming an optical functional film and an optical functional film.
  • the sputtering target according to one aspect of the present invention is a first component composed of one or two kinds of carbides selected from W and Ta, and Si, In, Y, Nb, V and Zn. , Zr, Al, B, Mo, W contains a second component composed of one or more oxides selected from, and the total content of W, Ta in the first component is 10 atomic%. It is characterized in that it is within the range of 35 atomic% or less.
  • the sputtering target having this configuration has a first component and a second component, and the total content of W and Ta in the first component is within the range of 10 atomic% or more and 35 atomic% or less. Therefore, it is possible to form an optical functional film having excellent heat resistance and being able to be satisfactorily etched with an etching solution containing hydrogen peroxide. Further, it is possible to form an optical functional film capable of sufficiently suppressing the reflection of light from a metal thin film or the like.
  • the structure is such that the granular carbides are dispersed in the matrix of the oxide, and the average particle size of the carbides is within the range of 1 ⁇ m or more and 150 ⁇ m or less. It is preferable that In this case, since the average particle size of the carbide is 1 ⁇ m or more, the density of the sputtering target can be increased. Further, since the average particle size of the carbide is 150 ⁇ m or less, it is possible to stably form an optical functional film in which the carbide and the oxide are uniformly mixed by sputtering.
  • the density ratio is preferably 90% or more. In this case, since the density ratio is 90% or more, it is possible to suppress the generation of particles due to abnormal discharge during sputtering, and stable film formation can be achieved.
  • the resistivity is preferably 0.1 ⁇ ⁇ cm or less.
  • the specific resistivity is 0.1 ⁇ ⁇ cm or less, stable film formation can be performed without abnormal discharge by DC sputtering, and an optical functional film can be efficiently formed.
  • the optical functional film according to one aspect of the present invention comprises a first component composed of one or two carbides selected from W and Ta, and Si, In, Y, Nb, V, Zn, Zr, Al, B, It contains a second component composed of one or more oxides selected from Mo and W, and the total content of W and Ta in the first component is in the range of 3 atomic% or more and 11 atomic% or less. It is characterized by being inside.
  • the optical functional film having this configuration has a first component and a second component, and the total content of W and Ta in the first component is in the range of 3 atomic% or more and 11 atomic% or less. Since it is inside, it has excellent heat resistance and can be satisfactorily etched with an etching solution containing hydrogen peroxide. In addition, it is possible to sufficiently suppress the reflection of light from a metal thin film or the like.
  • the visible light reflectance is 20% or less when a film is formed on the surface in contact with the Cu film in a thickness range of 25 nm or more and 75 nm or less. ..
  • the above-mentioned visible light reflectance is suppressed to a low level of 20% or less, it is possible to reliably suppress the reflection of light from the laminated metal thin film or the like.
  • the sheet resistance of a thickness 50nm is 10 6 ⁇ / sq.
  • the sheet resistance of a thickness 50nm is 10 6 ⁇ / sq.
  • Conductivity is ensured as follows, and energization can be performed through this optical functional film.
  • the etching rate with the hydrogen peroxide etching solution is 0.3 mm / sec. Above 5.8 mm / sec. It is preferably within the following range. In this case, the etching rate with the hydrogen peroxide etching solution is 0.3 mm / sec. Above 5.8 mm / sec. Since it is within the following range, when the optical functional film according to one aspect of the present invention is laminated on the metal thin film, it can be satisfactorily etched together with the metal thin film, and patterning can be performed efficiently. It will be possible.
  • the product n ⁇ k ⁇ d of the film thickness d, the refractive index n in the visible light region, and the extinction coefficient k in the visible light region is within the range of 40 or more and 100 or less. It is preferable that In this case, the absorption and interference of visible light makes it possible to more reliably suppress the reflection of visible light.
  • a film is formed on the surface in contact with the Cu film within a thickness range of 25 nm or more and 75 nm or less, and the visible light reflectance after heat treatment held at 400 ° C. for 10 minutes is high. It is preferably 20% or less. In this case, since the visible light reflectance after the heat treatment held at 400 ° C. for 10 minutes is 20% or less, the optical characteristics do not change significantly even if the heat treatment is performed, and the heat resistance is excellent.
  • sputtering for forming an optical functional film which is excellent in etching property and heat resistance by an etching solution containing hydrogen peroxide and can sufficiently suppress reflection of light from a metal thin film or the like.
  • a target and an optical functional film can be provided.
  • the optical functional film 12 is formed so as to be laminated on the metal wiring film 11 formed on the surface of the substrate 1.
  • the metal wiring film 11 is made of aluminum, an aluminum alloy, copper, a copper alloy, or the like, which are metals having excellent conductivity, and in this embodiment, it is made of copper. Since the metal wiring film 11 has a metallic luster, it reflects visible light and is visually recognized from the outside.
  • the optical functional film 12 of the present embodiment is provided to suppress the reflection of visible light in the laminated metal wiring film 11.
  • the optical functional film 12 of the present embodiment has a first component composed of one or two kinds of carbides selected from W and Ta, and Si, In, Y, Nb, V, Zn, Zr, Al, B and Mo.
  • a second component consisting of one or more oxides selected from W, and the total content of W and Ta in the first component is within the range of 3 atomic% or more and 11 atomic% or less. Has been done.
  • the first component composed of one or two kinds of carbides selected from W and Ta has conductivity, and the conductivity of the optical functional film 12 is ensured by this first component. Further, the heat resistance of the optical functional film 12 is improved by this first component.
  • the second component consisting of one or more oxides selected from Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo and W is mixed with the above-mentioned first component. This makes it possible to adjust the optical characteristics of the optical functional film 12. Further, by adopting the above-mentioned composition, it is possible to perform an etching treatment satisfactorily with an etching solution containing hydrogen peroxide.
  • the heat resistance and conductivity of the optical functional film 12 may be insufficient. If the total content of W and Ta in the first component exceeds 11 atomic%, the content of oxides such as Si may be insufficient, and the reflection of light from the metal thin film 11 or the like may not be sufficiently suppressed.
  • the lower limit of the total content of W and Ta in the first component in the optical functional film 12 of the present embodiment is more preferably 5.0 atomic% or more, still more preferably 7.0 atomic% or more.
  • the upper limit of the total content of W and Ta in the first component is more preferably 10.0 atomic% or less, still more preferably 9.0 atomic% or less.
  • the total content of Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo, and W in the second component is preferably in the range of 15 atomic% or more and 50 atomic% or less.
  • the total content of W and Ta in the first component and the total content of Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo and W in the second component are O,
  • the total amount of all elements including C is 100 atomic%.
  • the rest other than the above-mentioned elements whose contents are specified are C, O, and unavoidable impurities.
  • the visible light reflectance when a film is formed on the surface in contact with the Cu film within a thickness range of 25 nm or more and 75 nm or less is the reflectance of the Cu film (about 74). %) Is preferably smaller. Further, it is preferably 30% or less, and further preferably 20% or less.
  • the optical functional film 12 is formed on the Cu film in a thickness range of 25 nm or more and 75 nm or less.
  • the visible light reflectance is 20% or less when a film is formed on the surface in contact with the Cu film within a thickness range of 25 nm or more and 75 nm or less, the reflection of visible light on the metal wiring film 11 can be reliably suppressed.
  • the visible light reflectance is 15% or less when a film is formed on the surface in contact with the Cu film within a thickness range of 25 nm or more and 75 nm or less. It is more preferably present, and further preferably 10% or less.
  • the sheet resistance of a thickness 50nm is 10 6 ⁇ / sq. It is preferably as follows. This makes it possible to conduct conduction between the metal wiring film 11 and the external wiring via the optical functional film 12.
  • the sheet resistance of a thickness of 50nm is 10 6 ⁇ / sq. If it exceeds, the metal wiring and the outside can be electrically connected to each other by forming a hole in the low reflectance film or the substrate.
  • the sheet resistance of the thick 50nm is 10 5 ⁇ / sq. More preferably to less, 10 4 ⁇ / sq. The following is more preferable.
  • the lower limit of the sheet resistance at a thickness of 50 nm is preferably 10 ⁇ / sq. That is all.
  • the etching rate of the hydrogen peroxide etching solution is 0.3 mm or less of the etching rate of the Cu film (5.8 mm ⁇ sec.), And no undissolved residue is generated. / Sec. Above 5.8 mm / sec. It is preferably within the following range. This makes it possible to form a wiring pattern satisfactorily by etching in a state of being laminated with the metal wiring film 11.
  • the hydrogen peroxide etching solution for example, a hydrogen peroxide-based etching solution GHP-3 manufactured by Kanto Chemical Co., Inc. can be used.
  • the lower limit of the etching rate with the hydrogen peroxide etching solution is 0.4 mm / sec.
  • the above is more preferable, and 0.5 mm / sec. The above is more preferable.
  • the upper limit of the etching rate with the hydrogen peroxide etching solution is 3.0 mm / sec. It is more preferably 2.0 mm / sec. The following is more preferable.
  • the product n ⁇ k ⁇ d of the film thickness d, the refractive index n in the visible light region, and the extinction coefficient k in the visible light region is within the range of 40 or more and 100 or less. Is preferable.
  • reflection of the metal wiring film 11 is suppressed by absorption of visible light (extinction coefficient k) and interference (thickness d and refractive index n).
  • the visible light region is a region having a wavelength of 380 to 780 nm.
  • the visible light region is absorbed and interfered with by the visible light region. It is possible to suppress the reflection of light more reliably.
  • the lower limit of d ⁇ n ⁇ k is more preferably 50 or more, and further preferably 60 or more.
  • the upper limit of d ⁇ n ⁇ k is more preferably 90 or less, and further preferably 80 or less.
  • a film is formed on the surface in contact with the Cu film within a thickness range of 25 nm or more and 75 nm or less, and the visible light reflectance after heat treatment held at 400 ° C. for 10 minutes is high. It is preferably 20% or less. As a result, the optical characteristics do not deteriorate even after the heat treatment is performed, and the heat resistance is definitely excellent.
  • the visible light reflectance is more preferably 15% or less after heat treatment in which a film is formed on the surface in contact with the Cu film in a thickness of 25 nm or more and 75 nm or less and held at 400 ° C. for 10 minutes. Is more preferable.
  • the optical functional film 12 is formed on the Cu film in a thickness range of 25 nm or more and 75 nm or less.
  • the sputtering target of this embodiment is used for forming the above-mentioned optical functional film 12.
  • the sputtering target of this embodiment has a first component consisting of one or two carbides selected from W and Ta, and Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo and W. It contains a second component composed of one or more kinds of oxides selected from the above, and the total content of W and Ta in the first component is within the range of 10 atomic% or more and 35 atomic% or less. There is.
  • the first component composed of one or two kinds of carbides selected from W and Ta has conductivity, and the first component ensures the conductivity of the sputtering target of the present embodiment.
  • the second component which consists of one or more oxides selected from Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo, and W, is more sinterable than the first component. Since it is excellent, the density ratio of the sputtering target according to the present embodiment is improved. Further, by adopting the above-mentioned composition, it is possible to form an optical functional film 12 that can be satisfactorily etched with an etching solution containing hydrogen peroxide.
  • the total content of W and Ta in the first component of the sputtering target is 3 atomic% or more and 11
  • the optical functional film of the present embodiment within the range of atomic% or less can be formed.
  • the lower limit of the total content of W and Ta in the first component in the sputtering target of the present embodiment is more preferably 12.0 atomic% or more, still more preferably 14.0 atomic% or more.
  • the upper limit of the total content of W and Ta in the first component is more preferably 32.0 atomic% or less, still more preferably 29.0 atomic% or less.
  • the total content of Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo, and W in the second component is preferably in the range of 7 atomic% or more and 41 atomic% or less.
  • the total content of W and Ta in the first component and the total content of Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo and W in the second component are O,
  • the total amount of all elements including C is 100 atomic%.
  • the rest other than the above-mentioned elements whose contents are specified are C, O, and unavoidable impurities.
  • the structure is such that carbides are dispersed in an island shape in the matrix phase of the above-mentioned oxide, and the average particle size of the carbides is within the range of 1 ⁇ m or more and 150 ⁇ m or less. It is preferable that it is.
  • the average particle size of the carbide is the average number of circle-equivalent diameters.
  • the average particle size of the carbide is 1 ⁇ m or more, the density of the sputtering target can be increased.
  • the average particle size of the carbide is 150 ⁇ m or less, it is possible to stably form an optical functional film in which the carbide and the oxide are uniformly mixed by sputtering.
  • the lower limit of the average particle size of the carbide is more preferably 2 ⁇ m or more, further preferably 8 ⁇ m or more.
  • the upper limit of the average particle size of the carbide is more preferably 120 ⁇ m or less, and further preferably 80 ⁇ m or less.
  • the upper limit of the average particle size of the carbide may be 30 ⁇ m or less, or 15 ⁇ m or less.
  • the density ratio is preferably 90% or more. By setting the density ratio to 90% or more, it is possible to suppress the generation of particles during sputtering.
  • the density ratio is preferably 92% or more, more preferably 93% or more.
  • the upper limit of the density ratio is preferably 100% or less.
  • the resistivity is preferably 0.1 ⁇ ⁇ cm or less.
  • the optical functional film 12 can be stably formed by DC sputtering.
  • the resistivity is preferably 5 ⁇ 10 ⁇ 2 ⁇ ⁇ cm or less, and more preferably 1 ⁇ 10 ⁇ 2 ⁇ ⁇ cm or less.
  • the lower limit of the specific resistivity is preferably 1 ⁇ 10 -6 ⁇ ⁇ cm or more.
  • a first component powder composed of one or two carbides selected from W and Ta, and Si, In, Y, Nb, V, Zn, Zr, A second component powder composed of one or more oxides selected from Al, B, Mo, and W is weighed and mixed to obtain a sintered raw material powder.
  • the mixing method is not particularly limited, but in the present embodiment, a ball mill device is used.
  • the average particle size of the first component powder composed of one or two kinds of carbides selected from W and Ta is preferably in the range of 1 ⁇ m or more and 150 ⁇ m or less.
  • the average particle size of the second component powder consisting of one or more oxides selected from Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo and W is 0.05 ⁇ m or more and 0. It is preferably within the range of .3 ⁇ m or less.
  • the average particle size of the first component powder and the second component powder described above is the volume-based D50 diameter.
  • the above-mentioned sintered raw material powder is sintered by heating while pressurizing to obtain a sintered body.
  • sintering is performed using a hot press device or a hot isotropic pressure pressurizing device (HIP).
  • the sintering temperature is in the range of 650 ° C. or higher and 1000 ° C. or lower
  • the holding time at the sintering temperature is in the range of 0.5 hours or more and 15 hours or less
  • the pressurizing pressure is in the range of 10 MPa or more and 200 MPa or less. Be inside.
  • the first component composed of one or two kinds of carbides selected from W and Ta, and Si, In, Y, Nb, V, Zn. , Zr, Al, B, Mo, W contains a second component consisting of one or more oxides selected from, and the total content of W, Ta in the first component is 10 atomic% or more. Since it is within the range of 35 atomic% or less, it is possible to form an optical functional film 12 which is excellent in heat resistance and can be satisfactorily etched with an etching solution containing hydrogen peroxide. Further, it is possible to form an optical functional film 12 capable of sufficiently suppressing the reflection of light from a metal thin film or the like.
  • the sputtering target of the present embodiment when the structure is such that granular carbides are dispersed in the matrix of the oxide and the average particle size of the carbides is within the range of 1 ⁇ m or more and 150 ⁇ m or less, the sputtering target of this sputtering target. It is possible to increase the density and to stably form an optical functional film 12 in which carbides and oxides are uniformly mixed by sputtering.
  • the sputtering target of the present embodiment when the density ratio is 90% or more, the generation of particles at the time of sputtering can be suppressed, and the optical functional film 12 can be stably formed by sputtering. .. Further, in the sputtering target of the present embodiment, when the specific resistivity is 0.1 ⁇ ⁇ cm or less, stable film formation can be performed by DC sputtering, and the optical functional film 12 can be efficiently formed. can do.
  • the first component composed of one or two kinds of carbides selected from W and Ta, Si, In, Y, Nb, V, Zn, Zr, Al and B , Mo, W contains a second component consisting of one or more oxides selected from, and the total content of W, Ta in the first component is in the range of 3 atomic% or more and 11 atomic% or less. Since it is inside, it has excellent heat resistance and can be satisfactorily etched with an etching solution containing hydrogen peroxide. In addition, it is possible to sufficiently suppress the reflection of light from a metal thin film or the like.
  • the metal wiring film 11 when the visible light reflectance is 20% or less when a film is formed on the surface in contact with the Cu film within a thickness range of 25 nm or more and 75 nm or less, the metal wiring film 11 is used. It is possible to reliably suppress the reflection of light.
  • the sheet resistance of a thickness 50nm is 10 6 ⁇ / sq. In the following cases, conductivity is ensured and energization can be performed through the optical functional film 12.
  • the etching rate with the hydrogen peroxide etching solution is 0.3 mm / sec. Above 5.8 mm / sec. When it is within the following range, when it is laminated on the metal wiring film 11, it can be satisfactorily etched together with the metal wiring film 11, and patterning can be efficiently performed.
  • the product n ⁇ k ⁇ d of the film thickness d, the refractive index n in the visible light region, and the extinction coefficient k in the visible light region is set to be within the range of 40 or more and 100 or less. If so, the absorption and interference of visible light makes it possible to more reliably suppress the reflection of visible light. Further, in the optical functional film 12 of the present embodiment, a film is formed on the surface in contact with the Cu film within a thickness range of 25 nm or more and 75 nm or less, and the visible light reflectance after heat treatment held at 400 ° C. for 10 minutes is 20% or less. In the case of, the optical characteristics do not change significantly even if the heat treatment is performed, and the heat resistance is excellent.
  • the optical functional film 12 of the present embodiment is an optical functional film 12 formed on a metal wiring film 11 containing Al or Cu, or between a substrate and the metal wiring film 11, and W.
  • the first component consisting of one or two carbides selected from Ta and the oxidation of one or more selected from Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo, W. It is characterized in that it contains a second component made of a substance and has a visible light reflectance of 20% or less when a film is formed in a thickness range of 25 nm or more and 75 nm or less.
  • the present invention is not limited to this, and can be appropriately changed without departing from the technical requirements of the invention.
  • the laminated film having the structure shown in FIG. 1 has been described as an example, but the present invention is not limited to this, and the optical functional film 12 of the present embodiment is formed between the substrate and the metal wiring. It may be a laminated film having a structure of a glass substrate / optical functional film / metal wiring formed. In this case, the light from the glass substrate will be reflected. Further, with this structure, the optical functional film does not need to have conductivity.
  • the first component powder consisting of one or two carbides selected from W and Ta, and Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo
  • a second component powder consisting of one or more oxides selected from W was weighed. 1 kg of the weighed raw material powder and 1.3 kg of a ⁇ 5 mm ball were put into a 3 L pot. Next, the raw material powder was mixed with a ball mill device to obtain a raw material powder for sintering. All powders having a purity of 99.9% by mass or more were used.
  • the average particle size of the first component powder and the second component powder was measured as follows. Prepare 100 mL of an aqueous solution having a sodium hexametaphosphate concentration of 0.2 vol%, add 10 mg of each raw material powder to this aqueous solution, and use a laser diffraction / scattering method (measuring device: Microtrac MT3000 manufactured by Nikkiso Co., Ltd.) to distribute the particle size (volume). Reference) was measured. From the obtained particle size distribution (volume basis), the average particle size of the first component powder and the average particle size of the second component powder (D50 diameter) were determined.
  • sintering was performed by hot pressing or HIP to obtain a sintered body.
  • the raw material powder for sintering is filled in a carbon hot press mold ( ⁇ 135 mm), and the hot press is performed at 830 ° C. at the pressures shown in Tables 1 and 2 for 3 hours in a vacuum to bake. A bunch was made.
  • HIP hot pressing
  • a mixed powder raw material powder for sintering
  • CIP cold hydrostatic pressure
  • the molded body was set in the can of SPCC (rolled steel material), and the SPCC was welded. Then, the vacuum was evacuated to 0.001 Pa or less, and then the can was sealed. Sintering was performed at 850 ° C. at the pressures shown in Tables 1 and 2 for 2 hours to prepare a sintered body.
  • SPCC rolled steel material
  • These sintered bodies were machined to a diameter of 125 mm and a thickness of 5 mm, and then attached to a backing plate made of Cu with In solder to prepare a sputtering target. If it is desired to reduce impurity elements, it is preferable to use a raw material powder having a higher purity. Indium oxide powder and zinc oxide powder may be reduced during hot pressing and HIP to precipitate In and Zn, respectively. Therefore, it is preferable to sufficiently apply boron nitride to the carbon mold so that the carbon mold does not come into direct contact with the indium oxide powder and the zinc oxide powder.
  • the obtained sputtering target and the optical functional film formed by using this sputtering target were evaluated for the following items.
  • composition of sputtering target Quantitative analysis of the EPMA device was performed to quantify each metal component and C and O components, and quantification results were obtained. It was confirmed that there was no significant change in the composition at the time of blending the raw materials. For those containing both the carbide of W and the oxide of W, the ratio of the carbide of W and the oxide of W was obtained by performing XPS analysis, and the W in the first component was obtained using the obtained ratio and the quantitative result. And the amount of W in the second component were determined respectively.
  • the volume of the sputtering target was calculated from the dimensions of the obtained processed sputtering target, and the dimensional density of the sputtering target was calculated by dividing the measured weight value by the volume.
  • the ratio of the dimensional density divided by the calculated density is shown in Tables 3 and 4 as the "density ratio".
  • each metal component and C and O components were quantified and quantification results were obtained.
  • the ratio of the carbide of W and the oxide of W was obtained by performing XPS analysis, and the W in the first component was obtained using the obtained ratio and the quantitative result. And the amount of W in the second component were determined respectively. From the obtained results, the ratio of each component was calculated when the total value of the detected metal component and the C and O components was 100 atomic%. Further, in Comparative Example 4, each metal component and the C, O, N components were quantified, and the ratio of each component was calculated when the total value of the metal component and the C, O, N components was 100 atomic%. ..
  • a Cu film having a thickness of 200 nm was formed on a glass substrate.
  • Ar is flowed in the sputtering chamber at 50 sccm so that the above-mentioned optical functional film has an appropriate film thickness d (25 nm or more and 75 nm or less) on the surface in contact with the Cu film, and the total pressure in the chamber is 0.67 Pa.
  • a film was formed with the outputs shown in Tables 5 and 6 at DC with a TS distance of 70 mm to prepare a laminated film.
  • the reflectance of the laminated film formed on the glass substrate as described above was measured.
  • a spectrophotometer U-4100 manufactured by Hitachi, Ltd.
  • the laminated film prepared by measuring the reflectance was heat-treated at 400 ° C. in a nitrogen atmosphere for 10 minutes.
  • the reflectance after the heat treatment was measured in the same manner as immediately after the film formation.
  • Comparative Example 1 the sputtering target, ZnO is WC and the second component is a first component, but contains Y 2 O 3, the content of W are 8.0 atomic%, the deposition The W content in the obtained optical functional film was 2.8 atomic%. In this optical functional film, the reflectance was greatly increased after the heat treatment at 400 ° C., and the heat resistance was insufficient.
  • the sputtering target contained WC as the first component and Y 2 O 3 as the second component, but the W content was 39.0 atomic%, and the film was formed.
  • the W content in the optical functional film was 13.6 atomic%.
  • the reflectance before heat treatment was relatively large at 35%, and the reflection of visible light of the metal thin film could not be sufficiently suppressed.
  • the sputtering target was made of metallic Cu, and oxygen was introduced during sputtering to form an optical functional film made of copper oxide (CuO).
  • the reflectance was greatly increased after the heat treatment at 400 ° C., and the heat resistance was insufficient.
  • the sputtering target was made of metallic Cu, and an optical functional film made of copper oxynitride (CuNO) was formed by introducing nitrogen and oxygen during sputtering.
  • the sheet resistance became very high.
  • it was insoluble in the hydrogen peroxide etching solution and could not be etched.
  • the sputtering target contains the first component and the second component, and the total content of W and Ta in the first component is 10 atomic% or more and 35 atomic% or less. It is within the range, and the total content of W and Ta in the first component in the formed optical functional film is within the range of 3 atomic% or more and 11 atomic% or less.
  • the reflectance of visible light before the heat treatment was low, and the reflection of visible light of the metal thin film could be sufficiently suppressed.
  • the reflectance of visible light did not change significantly even after the heat treatment, and the heat resistance was excellent.
  • the etching treatment could be performed satisfactorily with the hydrogen peroxide etching solution.
  • an optical functional film having excellent etching properties and heat resistance due to an etching solution containing hydrogen peroxide and capable of sufficiently suppressing reflection of light from a metal thin film or the like is formed. It was confirmed that it is possible to provide a sputtering target to be filmed and an optical functional film.
  • the sputtering target of the present embodiment is suitably applied to a step of forming a low reflectance film provided on an electrode (metal film) for sensing in a projected capacitive touch panel and a black matrix in a flat panel display. ..

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Abstract

Une cible de pulvérisation cathodique comprend un premier composant comprenant un carbure d'au moins un élément choisi parmi W et Ta et un second composant d'un oxyde d'au moins un élément choisi parmi Si, In, Y, Nb, V, Zn, Zr, Al, B, Mo et W, la quantité totale contenue de W et de Ta dans le premier composant étant comprise dans une plage de 10-35 % atomiques.
PCT/JP2021/020200 2020-05-28 2021-05-27 Cible de pulvérisation et film fonctionnel optique WO2021241687A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003321771A (ja) * 2002-02-28 2003-11-14 Tosoh Corp スパッタリングターゲットおよびその製造方法
JP2005068507A (ja) * 2003-08-26 2005-03-17 Toshiba Corp 酸化膜形成用スパッタリングターゲットとそれを用いた酸化膜の製造方法
JP2005247664A (ja) * 2004-03-05 2005-09-15 Nippon Sheet Glass Co Ltd 鏡およびその製造方法
WO2013005690A1 (fr) * 2011-07-01 2013-01-10 宇部マテリアルズ株式会社 CIBLE DE MgO POUR PULVÉRISATION CATHODIQUE
WO2019223959A1 (fr) * 2018-05-23 2019-11-28 Hartmetall-Werkzeugfabrik Paul Horn Gmbh Dispositif de pulvérisation cathodique à magnétron
JP2020041217A (ja) * 2018-09-07 2020-03-19 三菱マテリアル株式会社 光学機能膜、スパッタリングターゲット、及び、スパッタリングターゲットの製造方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003321771A (ja) * 2002-02-28 2003-11-14 Tosoh Corp スパッタリングターゲットおよびその製造方法
JP2005068507A (ja) * 2003-08-26 2005-03-17 Toshiba Corp 酸化膜形成用スパッタリングターゲットとそれを用いた酸化膜の製造方法
JP2005247664A (ja) * 2004-03-05 2005-09-15 Nippon Sheet Glass Co Ltd 鏡およびその製造方法
WO2013005690A1 (fr) * 2011-07-01 2013-01-10 宇部マテリアルズ株式会社 CIBLE DE MgO POUR PULVÉRISATION CATHODIQUE
WO2019223959A1 (fr) * 2018-05-23 2019-11-28 Hartmetall-Werkzeugfabrik Paul Horn Gmbh Dispositif de pulvérisation cathodique à magnétron
JP2020041217A (ja) * 2018-09-07 2020-03-19 三菱マテリアル株式会社 光学機能膜、スパッタリングターゲット、及び、スパッタリングターゲットの製造方法

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