CN111902561B - Shield layer, method for producing shield layer, and oxide sputtering target - Google Patents

Shield layer, method for producing shield layer, and oxide sputtering target Download PDF

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CN111902561B
CN111902561B CN201980019072.1A CN201980019072A CN111902561B CN 111902561 B CN111902561 B CN 111902561B CN 201980019072 A CN201980019072 A CN 201980019072A CN 111902561 B CN111902561 B CN 111902561B
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shield layer
atomic
transmittance
less
range
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CN111902561A (en
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森理惠
山口刚
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Mitsubishi Materials Corp
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Mitsubishi Materials Corp
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    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
    • G02F1/133509—Filters, e.g. light shielding masks
    • G02F1/133512—Light shielding layers, e.g. black matrix
    • 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
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • 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
    • 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
    • G02B1/16—Optical coatings produced by application to, or surface treatment of, optical elements having an anti-static effect, e.g. electrically conducting coatings
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0083—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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    • 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
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    • 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
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
    • G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
    • G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices

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Abstract

A shield layer (20) is provided on a liquid crystal display panel (10), and the shield layer (20) is characterized by being composed of the following oxides: the total of the metal components is 100 atomic%, In is contained In a range of 60 atomic% to 80 atomic%, and the balance is Si and inevitable impurity metal elements, and Zr may be contained In a range of 1 atomic% to 32 atomic% with the total of the metal components being 100 atomic%.

Description

Shield layer, method for producing shield layer, and oxide sputtering target
Technical Field
The present invention relates to a shield layer provided for preventing static electricity in a display panel, a method for producing the shield layer, and an oxide sputtering target used for the method for producing the shield layer.
The present application claims priority based on patent application No. 2018-.
Background
In display panels such as liquid crystal displays, organic EL displays, and touch panels, shielding layers are provided to prevent malfunctions of liquid crystal elements, organic EL elements, and the like due to static electricity. In particular, in the embedded touch panel, the following actions are also required for the shielding layer: a touch signal is allowed to reach a sensor portion inside a panel while eliminating interference from the outside.
In addition, the shielding layer is required to have high transmittance of visible light in order to ensure visibility of the display panel.
Here, for example, in patent document 1, the shielding layer may be an ITO film or an IZO film.
In patent document 1, the following structure is adopted: a polarizing film is disposed on a surface of a glass substrate disposed on the liquid crystal cell, and the shielding layer is laminated on the polarizing film.
Further, patent document 2 proposes a transparent conductive film containing 7.2 to 11.2 atomic% of silicon (Si) in Indium Tin Oxide (ITO).
Patent document 1: US2013/0329171A1
Patent document 2: japanese patent laid-open publication No. 2013-142194
Therefore, as described in patent document 1, when an ITO film or an IZO film is used as the shielding layer, the film looks yellowish due to low transmittance in visible light, and thus the visibility may be deteriorated.
In addition, the transparent conductive film described in patent document 2 has a high resistance value and excellent light transmittance, but has insufficient environmental resistance, and may have a deteriorated resistance value and transmittance in a use environment.
In addition, the shield layer is required to have excellent environmental resistance (heat resistance and moisture resistance) so that the resistance value and the transmittance do not change even when the shield layer is used in a high-temperature and high-humidity environment, depending on the state of use of the display panel.
Here, since the ITO film and IZO film are easily crystalline, when used in a high-temperature and high-humidity environment, corrosive substances such as moisture are likely to enter the film, and the resistance value and transmittance may change.
Disclosure of Invention
The present invention has been made in view of the above circumstances, and an object thereof is to provide a shield layer having high transmittance of visible light, sufficiently high resistance value, and excellent environmental resistance (heat resistance and moisture resistance), a method for producing the shield layer, and an oxide sputtering target.
In order to solve the above problems, a shield layer according to the present invention is provided on a display panel, the shield layer comprising: the total of the metal components is 100 atomic%, In is contained In a range of 60 atomic% or more and 80 atomic% or less, and the balance is Si and inevitable impurity metal elements.
The shielding layer according to the present invention is composed of the following oxides: the total of the metal components is 100 atomic%, In is contained In a range of 60 atomic% to 80 atomic%, and the remainder is Si and inevitable impurity metal elements, and therefore, the visible light transmittance is excellent and the resistance value is sufficiently high.
Further, since the barrier layer of the present invention is easily amorphous, corrosive substances such as moisture are less likely to enter the inside of the film, and the resistance value and the transmittance do not change significantly even when used under a high-temperature and high-humidity environment, and the barrier layer has excellent environmental resistance (heat resistance and moisture resistance).
Further, since the shield layer of the present invention has resistance to water and alcohol, the transmittance and the resistance value do not change significantly even when the shield layer is washed with water, alcohol, or the like.
In the shield layer of the present invention, Zr may be contained in a range of 1 at% to 32 at% where the total of the metal components is 100 at%.
In this case, the total metal component is 100 atomic%, and the Zr content is 1 atomic% or more, so that the durability of the shield layer is further improved. Further, the hardness becomes high, and scratch resistance and the like are enhanced.
On the other hand, since the content of Zr is limited to 32 atomic% or less, it is possible to suppress an increase in refractive index, and to suppress occurrence of unnecessary reflection, thereby suppressing a decrease in visible light transmittance.
In the shield layer of the present invention, the thickness is preferably set in the range of 7nm to 25 nm.
In this case, the thickness of the shield layer is set to 7nm or more, and therefore, the durability can be sufficiently improved.
On the other hand, since the thickness of the shielding layer is set to 25nm or less, the transmittance and the resistance value can be sufficiently ensured.
In the shielding layer of the present invention, the transmittance at a wavelength of 550nm is preferably 95% or more.
In this case, since the transmittance at a wavelength of 550nm is 95% or more, the transmittance of visible light is excellent. Therefore, a display panel with excellent visibility can be configured.
In the shield layer of the present invention, the sheet resistance is preferably in the range of 1E + 7. omega./□ or more and 5E + 10. omega./□ or less.
In this case, the sheet resistance is set in the range of 1E +7 Ω/□ or more and 5E +10 Ω/□ or less, and therefore, static electricity and interference can be effectively removed, and the touch sensor inside the display can accurately detect the touch signal.
Further, as for the value of the sheet resistance (unit: Ω/□ (Ω/sq.)), the value A × 10 was calculated in accordance with JIS X0210-BIs expressed as AE + B (when B is a positive number).
The method for producing a shield layer according to the present invention is a method for producing the shield layer, wherein oxygen is introduced into a sputtering apparatus using an oxide sputtering target composed of an oxide containing In a range of 60 at% or more and 80 at% or less with the total metal components being 100 at%, and the remainder being Si and inevitable impurity metal elements, and wherein the flow ratio of oxygen/argon with respect to the amount of oxygen introduced is 0.03 or less, and oxygen is deposited by sputtering.
According to the method for producing the shield layer having such a structure, since oxygen is introduced into the sputtering apparatus using the oxide sputtering target composed of the oxide containing In a range of 60 at% or more and 80 at% or less and the balance being Si and inevitable impurity metal elements, the shield layer having a high visible light transmittance and a sufficiently high resistance value can be formed.
Further, since the flow rate ratio of oxygen/argon is 0.03 or less with respect to the amount of oxygen introduced, the resistance value of the formed shield layer can be suppressed from becoming excessively high.
In the method for producing a barrier layer according to the present invention, the oxide sputtering target may contain Zr in a range of 1 at% to 32 at% where the total of the metal components is 100 at%.
In this case, since the oxide sputtering target further contains Zr in a range of 1 at% or more and 32 at% or less, it is possible to form a hard-hardness shielding layer having excellent durability while ensuring the transmittance of visible light.
In the method for manufacturing a shield layer according to the present invention, the sheet resistance of the shield layer is preferably set to be in a range of 1E +7 Ω/□ or more and 5E +10 Ω/□ or less.
In this case, by setting the sheet resistance of the shielding layer to be in a range of 1E +7 Ω/□ or more and 5E +10 Ω/□ or less, it is possible to manufacture a shielding layer that can effectively remove static electricity and interference and allow the touch sensor inside the display to accurately detect a touch signal.
The oxide sputtering target of the present invention is a method for producing the above shield layer.
According to the oxide sputtering target having this structure, the barrier layer can be formed by performing sputtering deposition by introducing oxygen into a sputtering apparatus with an oxygen/argon flow ratio of 0.03 or less.
According to the present invention, it is possible to provide a shield layer having high visible light transmittance, sufficiently high resistance value, and excellent environmental resistance (heat resistance and moisture resistance), a method for producing the shield layer, and an oxide sputtering target.
Drawings
Fig. 1 is an explanatory view showing an example of a liquid crystal display panel including a shield layer according to an embodiment of the present invention.
Detailed Description
Hereinafter, a shield layer and a method for manufacturing the shield layer according to an embodiment of the present invention will be described with reference to the drawings.
The shielding layer of the present embodiment is disposed in a display panel such as a liquid crystal display panel, an organic EL display panel, or a touch panel for preventing static electricity. In this embodiment, a description will be given of a shield layer provided in a liquid crystal display panel.
First, a liquid crystal display panel 10 including the shield layer 20 of the present embodiment will be described with reference to fig. 1.
As shown in fig. 1, the liquid crystal display panel 10 includes a first glass substrate 11, a second glass substrate 12, and a liquid crystal layer 13 disposed between the first glass substrate 11 and the second glass substrate 12. In the present embodiment, the first glass substrate 11 and the second glass substrate 12 are alkali-free glasses and do not contain Na.
Further, by forming the first glass substrate 11 and the second glass substrate 12 from alkali-free glass, it is possible to suppress mixing of alkali components into the liquid crystal layer and the TFT (thin film field effect transistor), and to avoid deterioration of display performance.
The shield layer 20 of the present embodiment is disposed on the second glass substrate 12.
A polarizing film 15 is disposed on the shielding layer 20, and a protective film 16 is formed on the polarizing film 15.
In this case, after the formation of the shield layer 20, if the surface of the shield layer 20 is contaminated for some reason before proceeding to the next step, the surface of the shield layer 20 may be cleaned with water, alcohol, or the like. Therefore, the shielding layer 20 is also required to have resistance to water and alcohol.
Here, the shield layer 20 of the present embodiment is composed of the following oxides: the total of the metal components is 100 atomic%, In is contained In a range of 60 atomic% or more and 80 atomic% or less, and the balance is Si and inevitable impurity metal elements.
In the shield layer 20 of the present embodiment, the total of the metal components is 100 atomic%, and Zr may be contained In a range of 1 atomic% or more and 32 atomic% or less In addition to In.
In the shield layer 20 of the present embodiment, the thickness t is set to be in the range of 7nm to 25 nm.
In the shield layer 20 of the present embodiment, the transmittance at a wavelength of 550nm is 95% or more.
In the shield layer 20 of the present embodiment, the resistance value is set to be in the range of 1E +7 Ω/□ or more and 5E +10 Ω/□ or less.
Here, the reason why the composition, thickness, characteristics, and the like of the shield layer 20 are limited as described above will be described.
(In)
In the shield layer 20 made of an oxide of In and Si, when the total of the metal components is 100 atomic%, and the In content is less than 60 atomic%, there is a possibility that the conductivity required as the shield layer 20 cannot be secured. On the other hand, when the In content exceeds 80 atomic%, the transmittance at short wavelengths is lowered, and the visibility may be lowered.
As described above, In the present embodiment, the total of the metal components is set to 100 atomic%, and the In content is set to be In the range of 60 atomic% or more and 80 atomic% or less.
In order to further secure the conductivity of the shield layer 20, the total amount of the metal components is preferably 100 atomic%, and the In content is preferably 62 atomic% or more, and more preferably 64 atomic% or more.
On the other hand, In order to reliably suppress the decrease In the visible light transmittance, the In content is preferably 78 atomic% or less.
(Zr)
In the shield layer 20 of the present embodiment, Zr may be contained as a metal component In addition to In and Si.
Here, by setting the total of the metal components to 100 atomic% and the Zr content to 1 atomic% or more, the durability of the shield layer 20 can be improved, and the hardness becomes hard and the scratch resistance becomes strong. On the other hand, by setting the Zr content to 32 atomic% or less, the increase in refractive index can be suppressed, and the occurrence of unnecessary reflection can be suppressed, so that the decrease in visible light transmittance can be suppressed.
As described above, when Zr is contained in the present embodiment, the total of the metal components is preferably 100 atomic%, and the content of Zr is preferably in a range of 1 atomic% or more and 32 atomic% or less. In addition, in the case where Zr is contained as an inevitable impurity metal element, the content thereof may be less than 1 atomic%.
In order to further improve the durability of the shield layer 20, the total amount of the metal components is set to 100 atomic%, and the content of Zr is preferably set to 2 atomic% or more, and more preferably 3 atomic% or more.
On the other hand, in order to suppress an increase in refractive index and further suppress a decrease in transmittance, the Zr content is preferably 28 at% or less, and more preferably 25 at% or less.
(thickness)
In the shield layer 20 of the present embodiment, when the thickness t is 7nm or more, the durability of the shield layer 20 can be sufficiently ensured. On the other hand, when the thickness t of the shielding layer 20 is 25nm or less, the transmittance and the resistance value of visible light can be sufficiently ensured.
As described above, in the present embodiment, the thickness t of the shield layer 20 is preferably set to be in the range of 7nm to 25 nm.
In order to further improve the durability of the shield layer 20, the thickness t of the shield layer 20 is preferably 8nm or more, and more preferably 10nm or more.
On the other hand, in order to further secure the transmittance and the resistance value of visible light, the thickness t of the shielding layer 20 is preferably 20nm or less, and more preferably 18nm or less.
(transmittance)
In the shield layer 20 of the present embodiment, when the transmittance at a wavelength of 550nm is 95% or more, a sufficient transmittance can be secured, and the liquid crystal display panel 10 having excellent visibility can be configured.
As described above, in the shielding layer 20 of the present embodiment, the transmittance at a wavelength of 550nm is preferably set to 95% or more.
In order to form the liquid crystal display panel 10 having further excellent visibility, the transmittance of the shielding layer 20 of the present embodiment at a wavelength of 550nm is preferably 97% or more, and more preferably 98% or more.
(resistance value)
In the shield layer 20 of the present embodiment, when the resistance value is 1E +7 Ω/□ or more and 5E +10 Ω/□ or less, static electricity and interference can be effectively removed without preventing the touch sensor inside the display from detecting a touch signal.
As described above, in the present embodiment, the resistance value of the shield layer 20 is preferably set to be in the range of 1E +7 Ω/□ or more and 5E +10 Ω/□ or less.
In order to more reliably remove static electricity and interference and allow a touch signal to reach a sensor portion inside the panel, the resistance value of the shield layer 20 is preferably 3E +7 Ω/□ or more, and more preferably 5E +7 Ω/□ or more. The resistance value is preferably 9E + 9. omega./□ or less, and more preferably 5E + 9. omega./□ or less.
Next, a method for manufacturing the shield layer 20 of the present embodiment will be described.
In the method for manufacturing the shield layer according to the present embodiment, an oxide sputtering target having a composition corresponding to the shield layer 20 is used.
The oxide sputtering target is composed of a sintered body of an oxide In which In is contained In a range of 60 at% to 80 at%, with the total metal component taken as 100 at%, and the remainder is Si and unavoidable impurity metal elements. Further, Zr may be contained in a range of 1 at% or more and 32 at% or less, with the total of the metal components being 100 at%. In addition, in the case where Zr is contained as an inevitable impurity metal element, the content thereof may be less than 1 atomic%.
Here, the oxide sputtering target can be manufactured in the following manner.
First, In was prepared as a raw material powder2O3Powder, SiO2Powder and optionally ZrO2And (3) powder.
In2O3The powder preferably has a purity of 99.9 mass% or more and an average particle diameter of 0.1 to 10 μm.
SiO2The powder preferably has a purity of 99.8% by mass or more and an average particle diameter of 0.2 to 20 μm.
ZrO2The powder preferably has a purity of 99.9 mass% or more and an average particle diameter of 0.2 to 20 μm. In addition, in the present embodiment, with respect to ZrO2Purity of the powder by measuring Fe2O3、SiO2、TiO2、Na2O content with the remainder being ZrO2The calculated purity was measured. ZrO in the present embodiment2The powder may contain HfO in an amount of at most 2.5 mass%2。
These oxide powders were weighed so as to have a predetermined composition ratio, and mixed by using a pulverization mixing device to prepare a mixed raw material powder. Here, the specific surface area (BET specific surface area) of the mixed raw material powder is preferably set to 11.5m2More than g and 13.5m2Within a range of,/g or less.
The obtained mixed raw material powder is filled into a molding die and pressurized to obtain a molded body having a predetermined shape.
The molded article was charged into an electric furnace, heated and sintered. In this case, the holding temperature is preferably set in the range of 1300 ℃ to 1600 ℃ and the holding time is preferably set in the range of 2 hours to 10 hours. Further, oxygen is preferably introduced into the electric furnace.
Then, the sintered body was cooled to 600 ℃ in an electric furnace at a cooling rate of 200 ℃/hr or less, and then cooled to room temperature in a furnace, and the sintered body was taken out from the electric furnace.
The obtained sintered body is machined to produce an oxide sputtering target having a predetermined size.
Next, using this oxide sputtering target, the shield layer 20 is formed on the surface of the second glass substrate 12.
The oxide sputtering target was joined to a base material and mounted in a sputtering apparatus, and after the inside of the sputtering apparatus was set to a vacuum atmosphere, a sputtering gas pressure was adjusted by introducing Ar gas and oxygen gas, thereby performing sputtering film formation.
In this case, the oxygen amount introduced into the sputtering apparatus is preferably set to a flow ratio of oxygen/argon of 0.03 or less, and more preferably 0.02 or less. The lower limit of the oxygen/argon flow rate ratio is not particularly limited, but is preferably 0.002 or more. By introducing oxygen in this range, a barrier layer having a more preferable resistance value can be formed.
The shield layer 20 of the present embodiment having the above-described structure is composed of the following oxides: the total of the metal components is 100 atomic%, In is contained In a range of 60 atomic% to 80 atomic%, and the remainder is Si and inevitable impurity metal elements, and therefore, the liquid crystal display panel 10 has excellent visible light transmittance and a sufficiently high resistance value, and sufficiently functions as the shielding layer 20 In the liquid crystal display panel 10.
Further, since the shield layer 20 of the present embodiment is easily amorphous, corrosive substances such as moisture are less likely to enter the inside of the film, and the resistance value and the transmittance do not change significantly even when used under a high-temperature and high-humidity environment, and the shield layer has excellent environmental resistance (heat resistance and moisture resistance).
Further, since the transmittance and the resistance value do not change greatly even when the shield layer 20 is in contact with water or alcohol, the shield layer 20 is not deteriorated even if the shield layer 20 is washed with water or alcohol after the formation of the shield layer 20 and the surface of the shield layer 20 is contaminated for some reason before the next step.
In the shield layer 20 of the present embodiment, when Zr is contained in a range of 1 at% to 32 at%, the total metal components being 100 at%, the durability of the shield layer 20 can be further improved. Further, the shield layer 20 has high hardness and is enhanced in scratch resistance and the like. Further, since the increase in refractive index can be suppressed and the occurrence of unnecessary reflection can be suppressed, the decrease in visible light transmittance can be suppressed.
In addition, as described above, in the present embodiment, ZrO2The powder sometimes contains up to 2.5 mass% of HfO2Therefore, the barrier layer 20 may contain Hf in an atomic ratio of at most 1.7% relative to Zr in terms of metal component.
In the present embodiment, when the thickness of the shield layer 20 is 7nm or more, the durability of the shield layer 20 can be sufficiently improved.
On the other hand, when the thickness of the shielding layer 20 is 25nm or less, the transmittance and the resistance value of the shielding layer 20 for visible light can be sufficiently ensured. Thus, the liquid crystal display panel is particularly suitable for the shielding layer 20 in the liquid crystal display panel 10.
In the shield layer 20 of the present embodiment, when the transmittance at a wavelength of 550nm is 95% or more, the transmittance of visible light is excellent, and the visibility of the liquid crystal display panel 10 can be ensured.
In the shield layer 20 of the present embodiment, when the resistance value is set to 1E +7 Ω/□ or more and 5E +10 Ω/□ or less, static electricity and interference can be effectively removed without preventing the touch sensor inside the display from detecting a touch signal.
According to the method for manufacturing the shield layer 20 of the present embodiment, since the oxide sputtering target made of the oxide containing In the range of 60 atomic% or more and 80 atomic% or less is used, oxygen is introduced into the sputtering apparatus and the sputtering film is formed, the shield layer 20 having high visible light transmittance and sufficiently high resistance value can be stably formed.
Further, since the flow rate ratio of oxygen/argon is 0.03 or less with respect to the amount of oxygen introduced, the resistance value of the formed shield layer 20 can be suppressed from becoming excessively high.
In the method for producing the shielding layer 20 according to the present embodiment, when Zr is contained in the oxide sputtering target in a range of 1 at% or more and 32 at% or less with the total metal components being 100 at%, the shielding layer 20 having hard hardness and excellent durability can be formed while ensuring the visible light transmittance.
The embodiments of the present invention have been described above, but the present invention is not limited to these embodiments, and can be modified as appropriate within a range not departing from the technical spirit of the present invention.
For example, although the shielding layer 20 provided on the liquid crystal display panel 10 shown in fig. 1 has been described as an example in the present embodiment, the present invention is not limited to this, and may be provided on a liquid crystal display panel having another structure, or may be provided on another display panel such as an organic EL display or a touch panel.
In the present embodiment, the structure in which the oxide sputtering target produced as described above is used to form a film has been described, but the present invention is not limited to this, and a sputtering target produced by another production method may be used to form a film.
Examples
The following describes the results of a confirmation experiment performed to confirm the effectiveness of the present invention.
< oxide sputtering target >
Indium oxide powder (In) was prepared as a raw material powder2O3Powder: purity of 99.9% by mass or more and average particle diameter of 1 μm), and silicon oxide powder (SiO)2Powder: purity of 99.8% by mass or more and average particle diameter of 2 μm) and, if necessary, zirconia powder (ZrO)2Powder: purity of 99.9 mass% or more and average particle diameter of 2 μm). Then, they were weighed so as to have the mixing ratios shown in table 1.
In addition, for zirconia powder (ZrO)2Powder) by measuring Fe2O3、SiO2、TiO2、Na2O content with the remainder being ZrO2The purity calculated may contain at most 2.5% by mass HfO2。
The weighed raw material powders were put into a bead mill together with zirconia balls having a diameter of 0.5mm as a grinding medium and a solvent (Solmix a-11 manufactured by Japan Alcohol tracing co., ltd.) and ground/mixed. The pulverization/mixing time was set to 1 hour.
After the pulverization/mixing, the zirconia balls were separated and recovered, and a slurry containing the raw material powder and the solvent was obtained. The obtained slurry was heated to remove the solvent to obtain a mixed powder.
Next, the obtained mixed powder was filled in a mold having an inner diameter of 200mm at 150kg/cm2The press was performed under the pressure of (2) to thereby prepare a disk-shaped molded article having a diameter of 200mm and a thickness of 10 mm.
The obtained molded article was charged into an electric furnace (furnace internal volume 27000 cm)3) In the above step (2), the resultant was sintered by keeping the temperature at 1400 ℃ for 7 hours while introducing oxygen at a flow rate of 4L/min, thereby producing a sintered body.
After firing, the resultant was cooled to 600 ℃ in an electric furnace at a cooling rate of 130 ℃/hr while continuing to introduce oxygen. Then, the introduction of oxygen was stopped, the temperature was cooled to room temperature in the furnace, and the sintered body was taken out from the electric furnace.
The obtained sintered body was machined to produce a disk-shaped oxide sputtering target having a diameter of 152.4mm and a thickness of 6 mm.
< formation of a Shielding layer (oxide film) >
An oxide sputtering target was welded to an oxygen-free copper backing plate and mounted in a magnetron sputtering apparatus (SHOWA SHINKU co., ltd., SPH-2307).
Then, the inside of the sputtering apparatus was evacuated to 7X 10 by a vacuum evacuation apparatus-4After Pa or less, Ar gas and oxygen gas were introduced so as to obtain the flow ratio of oxygen/argon described in the column of "oxygen amount at sputtering" in table 1, the sputtering pressure was adjusted to 0.67Pa, and pre-sputtering was performed for 1 hour, thereby removing the processed layer on the target surface. The flow rate of oxygen at this time was set to the conditions shown in Table 1,the power is set to DC 615W. The flow rate ratio of oxygen/argon is defined as a ratio of an oxygen flow rate (sccm) to an argon flow rate (sccm).
Then, the inside of the sputtering apparatus was evacuated to 7X 10 by a vacuum evacuation apparatus-4Pa or less, and then sputtering was performed under the same conditions as the above-described pre-sputtering to form a film, and a shield layer (oxide film) having a thickness shown in table 1 was formed on a 50mm square alkali-free glass substrate. The distance between the substrate and the target at this time was set to 60 mm.
The composition, transmittance, resistance value, refractive index, hardness, transmittance after constant temperature and humidity test, and resistance value of the obtained shielding layer (oxide film) were evaluated in the following manners. The crystallinity of the oxide film was confirmed.
(composition of oxide film)
The solution obtained by dissolving the above oxide film with an acid was analyzed using an inductively coupled plasma emission spectroscopy (ICP-OES) apparatus (Agilent5100) manufactured by Agilent Technologies, inc., and the In concentration, Zr concentration, and Si concentration of each oxide film were measured. Table 1 shows the composition of the film in which the total of the metal components is 100 atomic%.
(transmittance)
The transmittance of light having a wavelength of 550nm was measured as the transmittance of a representative wavelength of visible light using a spectrophotometer (V-550 manufactured by JASCO Corporation).
(transmittance at short wavelength)
The transmittance of light having a wavelength of 350nm was measured as the transmittance in the short wavelength region of visible light using a spectrophotometer (V-550 manufactured by JASCO Corporation), and the relative value of the transmittance at the wavelength of 350nm to the transmittance at the wavelength of 550nm was calculated as the transmittance at 350 nm/the transmittance at 550 nm.
The relative value of the transmittance at a wavelength of 350nm to the transmittance at a wavelength of 550nm is 0.85 or more, and the case of less than 0.85 is indicated by ". times".
(resistance value)
The measurement was performed by a low voltage application/leakage current measurement method. As the measuring apparatus, Hiresta manufactured by Mitsubishi Chemical Analytech co.
(refractive index)
The refractive index of the oxide film was measured using an ellipsometer under conditions that the incident angle was 75 ° and the measurement wavelength was 550 nm.
(hardness)
Under the above sputtering conditions, an oxide film having a film thickness of 500nm was formed on a glass substrate (EAGLE-XG manufactured by Corning Incorporated co., ltd.). The oxide film was measured using an ultra fine indentation hardness tester (ENT-1100 a manufactured by ELIONIX inc.) with a press load of 25 mgf. The formed glass substrate was set in an apparatus at 27 ℃ and after 1 hour had elapsed, hardness measurement was performed. The average value of 10 point measurements for hardness is shown in table 2.
(constant temperature and humidity test)
A constant temperature and humidity test 1 in which the sample was kept at a constant temperature and humidity of 60 ℃ and a relative humidity of 90% for 240 hours and a constant temperature and humidity test 2 in which the sample was kept at a constant temperature and humidity of 85 ℃ and a relative humidity of 85% for 240 hours were carried out. After the constant temperature and humidity test 1 and after the constant temperature and humidity test 2, the transmittance and the resistance value at a wavelength of 550nm were measured as described above.
(crystallinity of film)
XRD analysis was performed on the oxide film formed to have a film thickness of 30nm under the conditions of inventive example 11 and conventional example 1, and the crystallinity of the oxide film was confirmed. As a result, in conventional example 1, it was confirmed that the oxide film was crystalline. In contrast, in inventive example 11, the oxide film was amorphous.
[ Table 1]
Figure GDA0003354474360000111
In addition, the method is as follows: the content of the metal element when the total of the metal components is 100 atomic%
In addition, 2: flow ratio of oxygen/argon
※3：ITO SnO2: 10% by mass In2O3: the remaining part
In addition, 4: IZO ZnO: 10% by mass In2O3: the remaining part
※5：ITO-Si SnO2:In2O31:9 (mass ratio), SiO2: 15% by mass
In addition, 6: ITO-Si Sn: 3.0 atomic%, In: 36.1 atomic%, Si: 11.0 atomic%, O: the remaining part
[ Table 2]
Figure GDA0003354474360000121
In addition, the method is as follows: the constant temperature and humidity test conditions are that the temperature is 60 ℃, the relative humidity is 90 percent, and the test time is 240 hours
In addition, 6: the constant temperature and humidity test conditions are that the temperature is 85 ℃, the relative humidity is 85 percent, and the test time is 240 hours
In conventional example 1 in which an ITO film was formed as a shielding layer, the transmittance at the initial wavelength of 550nm, the relative values of the transmittance at the wavelength of 350nm with respect to the transmittance at the wavelength of 550nm, and the resistance value were insufficient. After the constant temperature and humidity test 1 and the constant temperature and humidity test 2, a change in the resistance value was observed, and the environmental resistance was insufficient.
In conventional example 2 in which an IZO film was formed as a shielding layer, the transmittance at the initial wavelength of 550nm, the relative values of the transmittance at the wavelength of 350nm with respect to the transmittance at the wavelength of 550nm, and the resistance value were insufficient. After the constant temperature and humidity test 1 and the constant temperature and humidity test 2, a change in the resistance value was observed, and the environmental resistance was insufficient.
In conventional example 3 in which an ITO — Si film was formed as a shield layer, variations in transmittance and resistance were observed after the constant temperature and humidity test 2, and environmental resistance was insufficient.
In comparative example 1 In which the In content of the shield layer (oxide film) is less than the range of the present invention, the resistance value becomes too high, and the conductivity required as the shield layer cannot be secured.
In comparative example 2 In which the In content of the shield layer (oxide film) was more than the range of the present invention, the transmittance at short wavelengths was decreased. Further, after the constant temperature and humidity test 1 and the constant temperature and humidity test 2, a variation in transmittance was observed, and the environmental resistance was insufficient.
In comparative example 3 in which the Zr content of the barrier layer (oxide film) is more than the range of the present invention, the refractive index becomes large.
On the other hand, In the shield layer (oxide film) In which the In and Zr contents are set within the range of the present invention, it was confirmed that: the transmittance is sufficiently high and the resistance value is set within a suitable range, and is particularly suitable for use as a shielding layer. Further, even after the constant temperature and humidity test 1 and the constant temperature and humidity test 2, the transmittance and the resistance value do not greatly change.
Further, in invention examples 1 to 4 and 6 to 17 containing Zr, the hardness of the film was confirmed to be improved as compared with the Zr-free invention example 5.
In inventive examples 1 to 10 and 12 to 17, in which the thickness was 20nm or less, it was confirmed that: the transmittance at a wavelength of 350nm is 0.85 or more relative to the transmittance at a wavelength of 550nm, and the optical film has a high transmittance even at a short wavelength.
From the above, it is confirmed that: according to the present invention, it is possible to provide a shield layer having high transmittance of visible light, sufficiently high resistance value, and excellent environmental resistance (heat resistance and moisture resistance).
Industrial applicability
According to the present invention, it is possible to provide a shield layer having high visible light transmittance, sufficiently high resistance value, and excellent environmental resistance (heat resistance and moisture resistance), a method for producing the shield layer, and an oxide sputtering target.
Description of the symbols
10-liquid crystal display panel, 11-first glass substrate, 12-second glass substrate, 13-liquid crystal layer, 15-polarizing film, 16-protective film, 20-shielding layer.

Claims (3)

1. A shielding layer disposed on a display panel, the shielding layer characterized in that,
is composed of the following oxides: the total of the metal components is 100 atomic%, In is contained In the range of 60 atomic% or more and 80 atomic% or less, and the rest is Si and inevitable impurity metal elements,
the sheet resistance of the shielding layer is in the range of 1E +7 omega/□ or more and 5E +10 omega/□ or less,
the thickness of the shielding layer is in the range of 7nm to 25nm,
the total of the metal components is 100 atomic%, and Zr is contained in a range of 1 atomic% or more and 32 atomic% or less.
2. The shielding layer of claim 1,
the transmittance of the shielding layer at a wavelength of 550nm is 95% or more.
3. A method for manufacturing a shield layer, characterized by manufacturing the shield layer according to claim 1 or 2,
the method for producing a shield layer comprises introducing oxygen into a sputtering apparatus using an oxide sputtering target composed of an oxide, and performing sputtering deposition,
wherein the oxide contains 60 to 80 atomic% of In, with the total of the metal components being 100 atomic%, and the balance being Si and unavoidable impurity metal elements,
the flow rate ratio of oxygen/argon with respect to the amount of oxygen introduced is 0.03 or less,
the sheet resistance of the shielding layer is in the range of 1E +7 omega/□ or more and 5E +10 omega/□ or less,
the oxide sputtering target further contains Zr in a range of 1 at% to 32 at% with the total metal component being 100 at%.
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