WO2015182657A1 - 酸化アルミニウム又はアルミニウム基板用の密着被膜形成剤 - Google Patents
酸化アルミニウム又はアルミニウム基板用の密着被膜形成剤 Download PDFInfo
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- WO2015182657A1 WO2015182657A1 PCT/JP2015/065251 JP2015065251W WO2015182657A1 WO 2015182657 A1 WO2015182657 A1 WO 2015182657A1 JP 2015065251 W JP2015065251 W JP 2015065251W WO 2015182657 A1 WO2015182657 A1 WO 2015182657A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- 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
Definitions
- the present invention relates to an adhesive film forming agent for aluminum oxide such as sapphire glass or an aluminum substrate.
- Sapphire glass is a single crystal aluminum oxide and has excellent properties of being extremely hard and transparent, resistant to heat and insoluble in chemicals. Due to its high hardness and resistance to scratches, sapphire glass is used for watch cover glass (windshield), camera lens cover glass, and touch panel substrates for smartphones and tablets. Also known is a technology for applying antifouling agents such as fluorine compounds and silicon compounds to the surface of members such as glass in order to increase the scratch resistance, which is the resistance to scratching when other substances are rubbed against the substrate. It has been. By applying an antifouling agent, the slipperiness of the surface is improved, and even if an impact is applied, the impact can be softened by the slipperiness and excellent scratch resistance can be obtained. In addition, the application of the antifouling agent also provides an effect that water repellency, oil repellency, and fingerprints are difficult to stick.
- antifouling agents such as fluorine compounds and silicon compounds
- Patent Document 2 Film formation by a dry coating method such as sputtering, PVD (Physical Vapor Deposition), or CVD (Chemical Vapor Deposition) is performed in a vacuum vessel, which requires an expensive and large-scale apparatus. There is also a problem that the size and shape of the base material on which the film can be formed are limited.
- film formation by wet coating methods such as flexographic printing, spin coating, ink jetting, slit coating, bar coating, and spraying is inexpensive and can form a film at high speed.
- wet-coating method that sufficiently adheres to aluminum oxide, and in order to apply an antifouling agent, it was necessary to perform film formation by a high-cost dry coating method.
- the purpose of the present invention is to provide a functional film such as an antifouling agent on aluminum oxide such as sapphire glass or an aluminum substrate.
- An object of the present invention is to provide an adhesive film forming agent for aluminum oxide or aluminum substrate that can be formed into a film.
- An adhesive film-forming agent for an aluminum oxide or aluminum substrate comprising a hydrolyzed / condensed product of alkoxysilane and an aluminum salt.
- the hydrolysis / condensation product of alkoxysilane is a hydrolysis / condensation product of an alkoxysilane component containing at least one selected from alkoxysilanes represented by the following formulas (I) and (II): Film forming agent.
- R 1 and R 3 each independently represents an alkyl group having 1 to 5 carbon atoms
- R 2 represents a halogen atom, a vinyl group, a methacryloxy group, an acryloxy group
- a hydrocarbon group having 1 to 20 carbon atoms which may be substituted with at least one selected from the group consisting of a styryl group, a phenyl group, and a cyclohexyl group, and may have a hetero atom, a hydrogen atom, a halogen atom Atom, vinyl group, methacryloxy group, acryloxy group, styryl group, phenyl group, cyclohexyl group, amino group, glycidoxy group, mercapto group, isocyanate group or ureido group are represented.
- m represents
- the aluminum salt is at least one selected from the group consisting of aluminum chloride, aluminum nitrate, aluminum sulfate, aluminum acetate, aluminum oxalate, aluminum sulfamate, aluminum sulfonate, aluminum acetoacetate, aluminum acetylacetonate, and basic salts thereof.
- the adhesive film forming agent according to any one of the above items. 6). 1 to 5 above containing at least one selected from the group consisting of N-methyl-pyrrolidone, ethylene glycol, dimethylformamide, dimethylacetamide, diethylene glycol, propylene glycol, hexylene glycol and derivatives thereof as a precipitation inhibitor.
- the adhesive film forming agent according to any one of the above items.
- the adhesive film forming agent of the present invention is applied to an aluminum oxide or aluminum substrate such as sapphire glass by coating or the like to form a film, and a functional film such as an antifouling agent is formed thereon, Properties such as excellent scratch resistance can be imparted.
- a cover glass for a touch panel having excellent antifouling properties and scratch resistance can be obtained. Since the surface of metal aluminum is oxidized in the air to form an aluminum oxide film, the adhesive film forming agent of the present invention can also be used for a metal aluminum substrate.
- the adhesive film forming agent of the present invention contains a hydrolyzed / condensed product of alkoxysilane as component (A) and an aluminum salt as component (B).
- the hydrolysis / condensation product of the alkoxysilane that is the component (A) is a hydrolysis / condensation product of an alkoxysilane component that includes at least one selected from alkoxysilanes represented by the following formulas (I) and (II). is there.
- R 1 represents an alkyl group having 1 to 5 carbon atoms. From the viewpoint of reactivity, the OR 1 group is preferably a methoxy group, an ethoxy group, or a propoxy group.
- alkoxysilane represented by a formula (I) is not limited to these.
- the alkoxysilane represented by the formula (I) is preferably 40 mol% or more because sufficient hardness may not be obtained at 40 mol% or less in all alkoxysilanes. More preferably, it is 50 mol% or more. More preferably, it is 80 mol% or more.
- R 2 m Si (OR 3 ) 4-m (II)
- R 2 may be substituted with at least one selected from the group consisting of a halogen atom, a vinyl group, a methacryloxy group, an acryloxy group, a styryl group, a phenyl group, and a cyclohexyl group, and has a heteroatom.
- R ⁇ 1 >, R ⁇ 2 > and R ⁇ 3 > represent the said definition each independently.
- R 3 represents an alkyl group having 1 to 5 carbon atoms, and m represents an integer of 1 to 3. In the case where R 3 is more, R 3 are each independently, represent a defined above. From the viewpoint of reactivity, the OR 3 group is preferably a methoxy group or an ethoxy group.
- alkoxysilane represented by Formula (II) is not limited to these.
- the alkoxysilane hydrolyzate / condensate contained in the adhesive film-forming agent of the present invention is preferably a pentamer or less from the viewpoint of storage stability and hardness during low-temperature firing. A monomer is more preferable.
- This alkoxysilane hydrolyzed / condensed product can be condensed in the presence of a base and water.
- the amount of the base present is preferably 0.01 to 2 moles, more preferably 0.05 to 1 moles with respect to the alkoxysilane.
- the amount of water present is preferably 0.5 times to 10 times moles, more preferably 1 time to 5 times moles relative to the alkoxysilane.
- Examples of the aluminum salt contained in the adhesive film forming agent of the present invention include aluminum chloride, aluminum nitrate, aluminum sulfate, aluminum acetate, aluminum oxalate, aluminum sulfamate, aluminum sulfonate, aluminum acetoacetate, aluminum acetylacetonate, and the like.
- a hydrate, a hydrated salt, or a basic salt is mentioned.
- an aluminum nitrate salt is particularly preferable from the viewpoint of availability and storage stability of the film forming agent.
- the adhesion film forming agent of the present invention preferably contains a precipitation inhibitor from the viewpoint of storage stability.
- the precipitation inhibitor is used to prevent the aluminum salt from being precipitated in the coating film when the coating film is formed from the adhesive film forming agent of the present invention.
- the precipitation preventing agent include N-methyl-pyrrolidone, ethylene glycol, dimethylformamide, dimethylacetamide, diethylene glycol, propylene glycol, hexylene glycol, and derivatives thereof. These may be used alone or in combination. can do.
- the adhesive film forming agent of the present invention usually contains an organic solvent that dissolves or disperses the components (A) and (B). It is preferable that this organic solvent forms a coating film of the adhesive film forming agent, dissipates when the coating film is heated to obtain an adhesive film, and does not remain in the formed adhesive film. Therefore, as such an organic solvent, those having the above components (A) and (B) dissolved or dispersed satisfactorily and having a boiling point of preferably 60 to 250 ° C., more preferably 75 to 200 ° C. are suitable. .
- organic solvent examples include alcohols such as methanol, ethanol, propanol and butanol, esters such as ethyl acetate, glycols such as ethylene glycol and ether derivatives thereof, ester derivatives, ethers such as diethyl ether, acetone, Examples thereof include ketones such as methyl ethyl ketone and cyclohexanone, and aromatic hydrocarbons such as benzene and toluene. Of these, ethanol, propanol, or propylene glycol monomethyl ether is preferred from the viewpoints of solvent persistence and coatability.
- the adhesive film forming agent of the present invention is a component other than those described above, for example, inorganic fine particles, metalloxane monomers, metalloxane oligomers, metalloxane polymers, crosslinking agents, organic polymers, leveling agents, Components such as a surfactant may be included.
- the adhesive film forming agent of the present invention is at least one selected from the alkoxysilanes represented by the formulas (I) and (II), which is the component (A), and an aluminum salt that is the component (B). It is produced by mixing in an organic solvent containing water.
- the alkoxysilane represented by the formulas (I) and (II) is hydrolyzed / condensed by contact with water to be converted into a hydrolyzed / condensed product.
- the adhesive film forming agent of the present invention is obtained in the form of a composition containing a hydrolyzed / condensed alkoxysilane and an aluminum salt dissolved or dispersed in an organic solvent.
- the organic solvent used here can be the same as the above-mentioned organic solvent contained in the adhesive film forming agent of the present invention, including preferable characteristics.
- (A) the alkoxysilane hydrolysis / condensation product and (B) component aluminum salt are both solid metal oxides.
- it is preferably 0.1 to 20% by mass, more preferably 0.5 to 6% by mass.
- the content exceeds 20% by mass, the storage stability of the composition is deteriorated and it is difficult to control the thickness of the protective film to be formed.
- the content is 0.1% by mass or less, the thickness of the protective film to be obtained becomes thin, and it is necessary to form a coating film many times in order to obtain a predetermined film thickness. .
- the amount of water used for the hydrolysis of the alkoxysilane as the component (A) is preferably 0.5 or more in molar ratio (amount of water (mol)) / total mole of alkoxysilane used). ⁇ 5 is more preferred.
- this molar ratio is 0.5 or more, the above-described alkoxysilane is sufficiently hydrolyzed to improve the film formability and increase the strength of the resulting adhesive coating.
- the moisture content is involved in the reaction, so the moisture content of the metal salt relative to the amount of water used for the hydrolysis. Must be included.
- the temperature during the hydrolysis of the alkoxysilane is preferably in the range of 20 to 100 ° C. Among them, the range of 25 to 80 ° C. is more preferable from the viewpoint of obtaining a condensate having an appropriate molecular weight.
- the hydrolysis time is preferably 30 minutes to 48 hours, more preferably 30 minutes to 24 hours, from the viewpoint of obtaining a condensate having an appropriate molecular weight.
- the precipitation inhibitor may be added when the alkoxysilane undergoes hydrolysis / condensation reaction in the presence of an aluminum salt, or may be added after completion of the hydrolysis / condensation reaction.
- the precipitation inhibitor preferably has a weight ratio of (precipitation inhibitor / aluminum oxide) of 1 or more, more preferably 2 to 20, when the aluminum of the aluminum salt is converted to aluminum oxide. When this ratio is less than 1, the effect of preventing precipitation of the metal salt during coating film formation is reduced.
- the content ratio of the hydrolysis / condensation product of the alkoxysilane as the component (A) and the aluminum salt as the component (B) contained in the adhesion film forming agent of the present invention is the total number of moles of silicon atoms (Si).
- the molar ratio (Al / (Si + Al)) of aluminum atoms to the total number of moles of aluminum atoms (Al) is preferably 0.1 to 0.5, and more preferably 0.2 to 0.4. When this molar ratio is 0.1 or more, or 0.5 or less, the desired adhesion characteristics can be improved.
- the adhesion film-forming agent of the present invention is applied to a substrate whose surface is covered with aluminum oxide, such as aluminum oxide or an aluminum substrate, and baked to obtain an adhesion film on the substrate surface.
- aluminum oxide such as aluminum oxide or an aluminum substrate
- various coating methods can be applied. For example, a dip coating method, a spin coating method, a spray coating method, a brush coating method, a roll transfer method, a screen printing method, an ink jet method, a flexographic printing method, and the like can be used.
- the coating film formed on the substrate surface is then heated at a temperature of, for example, 50 to 100 ° C., preferably 60 to 80 ° C. to dry the coating film, and then 100 ° C. or more, preferably 100 to 600 ° C.
- An adhesive film having a dense film structure can be obtained by baking at a temperature of preferably 300 to 600 ° C. for 10 minutes or longer, preferably 0.5 to 2 hours. These heat treatments can be performed using an apparatus such as an oven furnace or a hot plate. In addition, it is also possible to abbreviate
- a film is formed on the aluminum oxide substrate from the adhesion film forming agent of the present invention.
- This adhesion film can function as an adhesion auxiliary layer for forming a coating agent for forming various characteristic films on the surface.
- an antifouling agent is used as the coating agent, an aluminum oxide substrate having an excellent scratch-resistant film on the surface can be obtained.
- the adhesive film forming agent of the present invention is used to form an adhesive film on the surface of aluminum oxide or an aluminum substrate. That is, an adhesion film is formed on the surface of the aluminum oxide substrate, and then a functional film obtained from a specific coating agent is formed on the surface of the adhesion film.
- the adhesion film is directly formed on the surface of the aluminum oxide substrate from the above-described adhesion film forming agent of the present invention.
- the functional film is an antifouling layer.
- the antifouling layer can be formed by applying an antifouling agent and baking it. Excellent scratch resistance is obtained by using sapphire glass as the substrate, forming a film obtained from the adhesive film forming agent of the present invention on the substrate, and subsequently forming a film 2 obtained from the antifouling agent.
- the thickness of the adhesion coating or the functional film is preferably 5 to 1000 nm, more preferably 10 to 400 nm.
- the adhesive film forming agent of the present invention is also effective for aluminum oxide having various crystal structures.
- sapphire glass which is single crystal aluminum oxide, it can also be used for polycrystalline or amorphous aluminum oxide.
- the adhesive film forming agent of the present invention can be used for a structure composed of a metal aluminum substrate.
- the functional film provided on the adhesion coating is not particularly limited. Specific examples include coatings obtained from antifouling agents, paints, adhesives, antireflective agents, water repellents, hydrophilic agents, oil repellents, lipophilic agents, hard coat agents, antiskid materials, and the like.
- FIG. 1 is a schematic cross-sectional view of a cover glass for a touch panel.
- the cover glass 1 for a touch panel has a functional film 2 through an adhesion coating 3 on the surface of the sapphire glass 4.
- the adhesion film 3 is a film directly formed on the surface of the sapphire glass using the adhesion film forming agent of the present invention.
- An example of the functional film 2 is an antifouling layer.
- the antifouling layer can be formed by applying an antifouling agent and baking it.
- the antifouling agent is maintained on the sapphire glass even when the finger or substance is rubbed. be able to. As a result, it is possible to prevent problems such as deterioration of scratch resistance, water repellency and oil repellency, and fingerprint adhesion when using the touch panel.
- TEOS Tetraethoxysilane
- AN Aluminum nitrate nonahydrate
- EtOH Ethanol
- PGME Propylene glycol monomethyl ether
- HG Hexylene glycol
- PB Propylene glycol monobutyl ether
- BCS Ethylene glycol monobutyl ether
- Antifouling agent manufactured by FT-Net, P-5425-0.2
- Example 1 Into a four-necked reaction flask, EtOH (22.49 g), water (7.42 g), and AN (12.88 g) were added and stirred. Next, EtOH (28.60 g) and TEOS (28.60 g) were added, and the mixture was stirred at 20 ° C. for 1 hour to prepare a solution. This solution (30 g) was mixed with HG (14 g), PB (10.5 g), BCS (10.5 g), and PGME (35 g) to obtain an adhesive film forming agent.
- Example 2 ⁇ Example 2> EtOH (22.93 g), water (6.6 g), and AN (19.62 g) were added to a four-neck reaction flask and stirred. Next, EtOH (25.43 g) and TEOS (25.43 g) were added and stirred in a water bath for 1 hour to prepare a solution. This solution (30 g) was mixed with HG (14 g), PB (10.5 g), BCS (10.5 g), and PGME (35 g) to obtain an adhesive film forming agent.
- an antifouling agent which is an agent as a coating for forming a functional film
- a substrate with an adhesion coating obtained from Examples and Comparative Examples using a spin coater. Then, it was dried at 80 ° C. for 3 minutes on a hot plate, and then heated at 170 ° C. for 20 minutes in a clean oven to produce a sapphire glass having an antifouling film on the surface.
- Comparative Example 2 a substrate in which the antifouling agent film was directly formed on the sapphire glass substrate was prepared without coating the adhesion film forming agents of Examples and Comparative Examples.
- the sapphire-coated sapphire glass substrates of Examples 1 and 2 had a water contact angle of 90 ° or more and a change from the initial of 20 ° even when 800 round-trip steel wool friction was performed. It was confirmed that good scratch resistance was obtained.
- the sapphire glass substrate with antifouling agent of Comparative Examples 1 and 2 had a water contact angle of less than 90 ° and decreased by 20 ° or more due to 800 reciprocating steel wool friction.
- An aluminum oxide substrate having an antifouling film as a functional film formed through a film obtained from the adhesive film forming agent of the present invention has excellent scratch resistance, a watch cover glass (windshield), and a camera lens cover. It can be used as a touch panel substrate such as glass, smartphone or tablet.
Abstract
Description
基材に他の物質を擦りつけた際の傷の付きにくさである耐擦傷性を上げるため、ガラスなどの部材表面にフッ素系化合物やシリコン系化合物などの防汚剤を塗布する技術も知られている。防汚剤を塗布することで表面の滑り性が良くなり、衝撃が加わっても、滑り性によってその衝撃をやわらげることができ、優れた耐擦傷性を得ることができる。また、防汚剤の塗布により、撥水、撥油、及び指紋が付きにくいという効果も得られる。
1.アルコキシシランの加水分解・縮合体と、アルミニウム塩とを含有することを特徴とする酸化アルミニウム又はアルミニウム基板用の密着被膜形成剤。
2.アルコキシシランの加水分解・縮合体が、下記式(I)及び(II)で示されるアルコキシシランから選ばれる少なくとも1種を含むアルコキシシラン成分の加水分解・縮合体である、上記1に記載の密着被膜形成剤。
(化1)
Si(OR1)4 (I)
(化2)
R2 mSi(OR3)4-m (II)
上記式(I)及び(II)において、R1及びR3は、それぞれ独立して、炭素数1~5のアルキル基を表し、R2は、ハロゲン原子、ビニル基、メタクリロキシ基、アクリロキシ基、スチリル基、フェニル基、及びシクロヘキシル基からなる群から選ばれる少なくとも1種で置換されていてもよく、かつヘテロ原子を有していてもよい炭素数1~20の炭化水素基、水素原子、ハロゲン原子、ビニル基、メタクリロキシ基、アクリロキシ基、スチリル基、フェニル基、シクロヘキシル基、アミノ基、グリシドキシ基、メルカプト基、イソシアネート基又はウレイド基を表す。mは1~3の整数を表す。
4.上記アルミニウム塩が硝酸アルミニウム塩である、上記1~3のいずれか1項に記載の密着被膜形成剤。
5.珪素原子の全モル数(Si)とアルミニウム原子のモル数(Al)を合計に対するアルミニウム原子のモル比(Al/(Si+Al))が、0.1~0.5である、上記1~4のいずれか1項に記載の密着被膜形成剤。
6.析出防止剤として、N-メチル-ピロリドン、エチレングリコール、ジメチルホルムアミド、ジメチルアセトアミド、ジエチレングリコール、プロピレングリコール、ヘキシレングリコール及びこれらの誘導体からなる群より選ばれる少なくとも1つを含有する、上記1~5のいずれか1項に記載の密着被膜形成剤。
8.上記7に記載の密着被膜を有する酸化アルミニウム又はアルミニウム基板。
9.上記7に記載の密着被膜を有するタッチパネル。
10.上記1~6のいずれか1項に記載の密着被膜形成剤を、酸化アルミニウム基板又はアルミニウム基板に塗布した塗膜を100~600℃で焼成する酸化アルミニウム又はアルミニウム基板用の密着被膜の形成方法。
(A)成分であるアルコキシシシランの加水分解・縮合体は、下記式(I)及び(II)で表されるアルコキシシランから選ばれる少なくとも1種を含むアルコキシシラン成分の加水分解・縮合体である。
Si(OR1)4 (I)
R1は、炭素数1~5のアルキル基を表す。反応性の観点から、OR1基としては、メトキシ基、エトキシ基又はプロポキシ基が好ましい。
式(I)で表されるアルコキシシランは、全アルコキシシラン中、40モル%以下では充分な硬度が得られない場合があるため、40モル%以上が好ましい。より好ましくは50モル%以上である。更に好ましくは80モル%以上である。
R2 mSi(OR3)4-m (II)
R2は、ハロゲン原子、ビニル基、メタクリロキシ基、アクリロキシ基、スチリル基、フェニル基、及びシクロヘキシル基からなる群から選ばれる少なくとも1種で置換されていてもよく、かつヘテロ原子を有していてもよい炭素数1~20の炭化水素基、水素原子、ハロゲン原子、ビニル基、メタクリロキシ基、アクリロキシ基、スチリル基、フェニル基、シクロヘキシル基、アミノ基、グリシドキシ基、メルカプト基、イソシアネート基又はウレイド基を表す。なお、R1、R2及びR3が複数となる場合、R1、R2及びR3は、それぞれ独立して、上記定義を表す。
このアルコキシシランの加水分解・縮合体は、塩基及び水の存在下に縮合させることが可能である。塩基の存在量はアルコキシシランに対して0.01倍モルから2倍モルが好ましく、0.05倍モルから1倍モルがより好ましい。水の存在量はアルコキシシランに対して0.5倍モルから10倍モルが好ましく、1倍モルから5倍モルがより好ましい。
本発明の密着被膜形成剤に含有されるアルミニウム塩としては、塩化アルミニウム、硝酸アルミニウム、硫酸アルミニウム、酢酸アルミニウム、蓚酸アルミニウム、スルファミン酸アルミニウム、スルホン酸アルミニウム、アセト酢酸アルミニウム、アルミニウムアセチルアセトナート、これらの水和物、含水塩、又は塩基性塩が挙げられる。
その中でも、入手の容易性と、被膜形成剤の貯蔵安定性の点から、特に、硝酸アルミニウム塩が好ましい。
本発明の密着被膜形成剤には、保存安定性の観点から、析出防止剤が含まれることが好ましい。析出防止剤は、本発明の密着被膜形成剤から被膜を形成した際、被膜中にアルミニウム塩が析出するのを防止するために用いられる。
析出防止剤としては、N-メチル-ピロリドン、エチレングリコール、ジメチルホルムアミド、ジメチルアセトアミド、ジエチレングリコール、プロピレングリコール、ヘキシレングリコール、これらの誘導体等が挙げられ、これらを1種又は2種以上混合して使用することができる。
本発明の密着被膜形成剤は、通常、上記の(A)成分及び(B)成分を溶解又は分散させる有機溶媒を含有する。この有機溶媒は、密着被膜形成剤の塗膜を形成し、この塗膜を加熱処理して密着被膜を得る際に逸散し、形成された密着被膜中には残存しないのが好ましい。このため、かかる有機溶媒としては、上記の(A)成分及び(B)成分を良好に溶解又は分散させ、沸点が好ましくは60~250℃、より好ましくは75~200℃のものが好適である。
有機溶媒の例としては、メタノール、エタノール、プロパノール、ブタノールなどのアルコール類、酢酸エチルエステルなどのエステル類、エチレングリコールなどのグリコール類及びそのエーテル誘導体、エステル誘導体、ジエチルエーテルなどのエーテル類、アセトン、メチルエチルケトン、シクロヘキサノンなどのケトン類、ベンゼン、トルエンなどの芳香族炭化水素類などが挙げられる。なかでも、溶媒の残存性及び塗布性の観点から、エタノール、プロパノール、又はプロピレングリコールモノメチルエーテルが好ましい。
本発明の密着被膜形成剤は、本発明の効果を損なわない限りにおいて、上記以外の成分、例えば、無機微粒子、メタロキサンモノマー、メタロキサンオリゴマー、メタロキサンポリマー、架橋剤、有機ポリマー、レベリング剤、界面活性剤等の成分が含まれていてもよい。
本発明の密着被膜形成剤は、上記の(A)成分である、式(I)及び(II)で表されるアルコキシシランから選ばれる少なくとも1種と、(B)成分であるアルミニウム塩と、水を含有する有機溶媒中で混合することにより製造される。式(I)及び(II)で表されるアルコキシシランは、水との接触により加水分解・縮合して加水分解・縮合体に転化する。これにより、本発明の密着被膜形成剤は、アルコキシシランの加水分解・縮合体と、アルミニウム塩とが有機溶媒中に溶解又は分散して含有する組成物の形態で得られる。
ここで使用される有機溶媒は、好ましい特性も含めて、本発明の密着被膜形成剤中に含有される上記した有機溶媒と同じものが使用できる。
なお、上記加水分解において、(B)成分であるアルミニウム塩の含水塩が共存する場合には、その含水分が反応に関与するため、加水分解に用いる水の量に対して金属塩の含水分を算入する必要がある。
析出防止剤は、アルミニウム塩のアルミニウムを酸化アルミニウムに換算して、(析出防止剤/酸化アルミニウム)の重量比率が1以上であるのが好ましく、2~20がより好ましい。この比率が1未満であると、塗膜形成時における金属塩の析出防止効果が小さくなる。
本発明の密着被膜形成剤を、酸化アルミニウム又はアルミニウム基板のように、表面が酸化アルミニウムで覆われている基板に塗布し、焼成することにより基板表面に密着被膜が得られる。
本発明の密着被膜形成剤を用い、基板表面にその塗膜を形成する方法としては、様々な塗布法を適用して行うことができる。例えば、ディップコート法、スピンコート法、スプレーコート法、刷毛塗り法、ロール転写法、スクリーン印刷法、インクジェット法、フレキソ印刷法等を用いることができる。
上記のようにして、酸化アルミニウム基板上で、本発明の密着被膜形成剤から被膜が形成される。この密着被膜は、その表面に、様々な特性被膜を形成するーティング剤を形成するための密着補助層として機能することができる。例えば、コーティング剤として防汚剤を用いた場合は、優れた耐擦傷特性被膜を表面に有する酸化アルミニウム基板が得られる。
本発明の密着被膜形成剤は、酸化アルミニウム又はアルミニウム基板の表面に密着被膜を形成するのに使用される。すなわち、酸化アルミニウム基板の表面に密着被膜を形成し、次いで、密着被膜の表面には、特定のコーティング剤から得られる機能性膜を形成する。密着被膜は、上述した本発明の密着被膜形成剤から、酸化アルミニウム基板の表面に直接に形成される。
密着被膜や機能性膜の厚さは、いずれも、5~1000nmが好ましく、より好ましくは10~400nmである。
また、金属アルミニウムの表面は、空気中で酸化し、酸化アルミニウム被膜が形成されるため、本発明の密着被膜形成剤は、金属アルミニウム基板から成る構造体に対しても使用することができる。
本発明において、密着被膜上に設けられる機能性膜は特に限定されない。具体的な例としては、防汚剤、塗料、接着剤、反射防止剤、撥水剤、親水剤、撥油剤、親油剤、ハードコート剤、防滑材などから得られる被膜を挙げることができる。
発明の密着被膜形成剤を使用して得られる酸化アルミニウム基板の代表例として、図1に示されるタッチパネル用カバーガラスが挙げられる。図1は、タッチパネル用カバーガラスの模式的な断面図である。タッチパネル用カバーガラス1は、サファイアガラス4の表面上に、機能性膜2を密着被膜3を介して有する。密着被膜3は、本発明の密着被膜形成剤を用いてサファイアガラスの表面に直接形成された被膜である。機能性膜2の一例としては、防汚層が挙げられる。防汚層は防汚剤を塗布し、焼成することで形成できる。
サファイアガラス上に本発明の被膜形成剤から得られる密着被膜を形成し、続いて防汚剤の膜を形成することで、指や物質をこすり付けても防汚剤をサファイアガラス上に維持することができる。これにより、タッチパネルを使用する際の耐擦傷性、撥水性、撥油性の劣化及び指紋などが付着する問題を防ぐことができる。
[化合物とその略称]
TEOS:テトラエトキシシラン AN:硝酸アルミニウム・九水和物
EtOH:エタノール PGME:プロピレングリコールモノメチルエーテル
HG:ヘキシレングリコール PB:プロピレングリコールモノブチルエーテル
BCS:エチレングリコールモノブチルエーテル
防汚剤: FT-Net社製、P-5425-0.2
4つ口反応フラスコに、EtOH(22.49g)、水(7.42g)、及びAN(12.88g)を投入し、攪拌した。次いで、EtOH(28.60g)、及びTEOS(28.60g)を投入し、20℃で1時間攪拌して、溶液を調製した。
この溶液(30g)をHG(14g)、PB(10.5g)、BCS(10.5g)、及びPGME(35g)と混合することで密着被膜形成剤を得た。
4つ口反応フラスコに、EtOH(22.93g)、水(6.6g)、及びAN(19.62g)を投入し、攪拌した。次いで、EtOH(25.43g)、及びTEOS(25.43g)を投入し、1時間水浴中で攪拌して、溶液を調製した。
この溶液(30g)をHG(14g)、PB(10.5g)、BCS(10.5g)、及びPGME(35g)と混合することで密着被膜形成剤を得た。
還流管を備えつけた4つ口反応フラスコに、EtOH(33.87g)、アルコキシシランとしてTEOS(34.72g)を投入し、攪拌した。次いで、EtOH(16.94g)、水(13.6g)、及び硝酸60重量%含有水溶液(0.88g)を、30分間滴下しながら投入し、攪拌した。次いで、3時間還流し、室温まで放冷して、溶液を調製した。
この溶液(30g)をHG(14g)、PB(10.5g)、BCS(10.5g)、及びPGME(35g)と混合することで密着被膜形成剤を得た。
スピンコーターを用い、上述した実施例1、2及び比較例1の密着被膜形成剤を、それぞれ、厚さ0.7mmのサファイアガラス(単結晶サファイアガラス、表面粗さ:1Å以下)に塗布し、ホットプレート上で80℃で3分間の乾燥を行った。続いて、クリーンオーブン中で、150℃又は300℃で、30分間加熱することで、厚さ50~100nmの実施例及び比較例の密着被膜を得た。
次に、機能性膜を形成するコーティングとして剤である防汚剤を、スピンコーターを用いて、実施例及び比較例から得られる密着被膜付基板に塗布した。その後、ホットプレート上で80℃で、3分間乾燥させ、次いで、クリーンオーブン中、170℃で、20分間加熱させることで、表面に防汚剤膜を有するサファイアガラスを製造した。
比較例2では、実施例及び比較例の密着被膜形成剤を塗膜せず、サファイアガラス基板に直接、防汚剤膜を形成した基板も作製した。
往復式耐擦傷性試験機(大栄科学精器製作所社製)の台上に保持された、上記実施例及び比較例で作製したサファイアガラス基板の表面上に、#0000の等級のスチールウール(日本スチールウール社製、登録商標:ボンスター)を、面積2cm2の四角形パッドを接触するように載せ、かかるパッドを印加荷重1,000g、毎分25往復の速度で、0往復から1000往復まで摩擦した。摩擦200往復ごとに、接触角計(協和界面科学社製、DM-701)を用いて、液量3μLでの水の接触角測定を行った。測定結果を、まとめて表1に示す。
一方、比較例1、2の防汚剤付サファイアガラス基板は、800往復のスチールウール摩擦により、水接触角が90°未満となり、20°以上低下した。
3 密着被膜層 4 サファイアガラス基板
Claims (10)
- アルコキシシランの加水分解・縮合体と、アルミニウム塩とを含有することを特徴とする酸化アルミニウム又はアルミニウム基板用の密着被膜形成剤。
- アルコキシシランの加水分解・縮合体が、下記式(I)及び(II)で示されるアルコキシシランからなる群から選ばれる少なくとも1種を含むアルコキシシランの加水分解・縮合体である、請求項1に記載の密着被膜形成剤。
(化1)
Si(OR1)4 (I)
(化2)
R2 mSi(OR3)4-m (II)
上記式(I)及び(II)中、R1及びR3は、それぞれ独立して、炭素数1~5のアルキル基を表し、R2は、ハロゲン原子、ビニル基、メタクリロキシ基、アクリロキシ基、スチリル基、フェニル基、及びシクロヘキシル基からなる群から選ばれる少なくとも1種で置換されていてもよく、かつヘテロ原子を有していてもよい炭素数1~20の炭化水素基、水素原子、ハロゲン原子、ビニル基、メタクリロキシ基、アクリロキシ基、スチリル基、フェニル基、シクロヘキシル基、アミノ基、グリシドキシ基、メルカプト基、イソシアネート基又はウレイド基を表す。mは1~3の整数を表す。 - 上記アルミニウム塩が、塩化アルミニウム、硝酸アルミニウム、硫酸アルミニウム、酢酸アルミニウム、蓚酸アルミニウム、スルファミン酸アルミニウム、スルホン酸アルミニウム、アセト酢酸アルミニウム、アルミニウムアセチルアセトナート及びこれらの塩基性塩からなる群から選ばれる少なくとも1種である、請求項1又は2に記載の密着被膜形成剤。
- 上記アルミニウム塩が硝酸アルミニウム塩である、請求項1~3のいずれか1項に記載の密着被膜形成剤。
- 珪素原子の全モル数(Si)とアルミニウム原子のモル数(Al)を合計に対するアルミニウム原子のモル比(Al/(Si+Al))が、0.1~0.5である、請求項1~4のいずれか1項に記載の密着被膜形成剤。
- 析出防止剤として、N-メチル-ピロリドン、エチレングリコール、ジメチルホルムアミド、ジメチルアセトアミド、ジエチレングリコール、プロピレングリコール、ヘキシレングリコール及びこれらの誘導体からなる群より選ばれる少なくとも1つを、更に含有する、請求項1~5のいずれか1項に記載の密着被膜形成剤。
- 請求項1~6のいずれか1項に記載の密着被膜形成剤を用いて得られる被膜。
- 請求項7に記載の被膜を有する酸化アルミニウム基板又はアルミニウム基板。
- 請求項7に記載の被膜を有するタッチパネル。
- 請求項1~6のいずれかに1項に記載の密着被膜形成剤を、酸化アルミニウム基板又はアルミニウム基板に塗布した塗膜を100~600℃で焼成する酸化アルミニウム又はアルミニウム基板用の密着被膜の形成方法。
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