WO2011030716A1 - ガラス/樹脂積層体、及びそれを用いた電子デバイス - Google Patents
ガラス/樹脂積層体、及びそれを用いた電子デバイス Download PDFInfo
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- WO2011030716A1 WO2011030716A1 PCT/JP2010/065067 JP2010065067W WO2011030716A1 WO 2011030716 A1 WO2011030716 A1 WO 2011030716A1 JP 2010065067 W JP2010065067 W JP 2010065067W WO 2011030716 A1 WO2011030716 A1 WO 2011030716A1
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- glass
- resin
- glass substrate
- resin layer
- layer
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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
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
-
- 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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
-
- 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
- B32B2315/00—Other materials containing non-metallic inorganic compounds not provided for in groups B32B2311/00 - B32B2313/04
- B32B2315/08—Glass
-
- 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
- B32B2379/00—Other polymers having nitrogen, with or without oxygen or carbon only, in the main chain
- B32B2379/08—Polyimides
-
- 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
- B32B2457/00—Electrical equipment
-
- 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
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/206—Organic displays, e.g. OLED
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
- Y10T156/11—Methods of delaminating, per se; i.e., separating at bonding face
- Y10T156/1168—Gripping and pulling work apart during delaminating
- Y10T156/1195—Delaminating from release surface
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/266—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension of base or substrate
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
- Y10T428/31623—Next to polyamide or polyimide
Definitions
- the present invention relates to a glass / resin laminate having a glass substrate and a resin layer, and an electronic device using the same.
- the glass / resin laminate described in Patent Document 2 is applied to a printed wiring board, and since the resin layers are laminated on both sides of the glass substrate, the surface flatness is not sufficient. For this reason, it is difficult to accurately form a member for an electronic device (for example, an organic EL element) on the surface of the glass / resin laminate.
- an electronic device for example, an organic EL element
- This invention is made
- the present invention provides a glass / resin laminate having a glass substrate and a resin layer.
- the resin layer includes a polyimide obtained by polycondensing an aromatic diamine having a benzoxazole structure and an aromatic tetracarboxylic acid anhydride,
- the difference in average linear expansion coefficient between the glass substrate and the resin layer at 25 to 300 ° C. is ⁇ 100 ⁇ 10 ⁇ 7 to + 100 ⁇ 10 ⁇ 7 / ° C.
- the present invention relates to a glass / resin laminate in which at least one outermost layer of the laminate is the glass substrate.
- the present invention also provides: The glass / resin laminate of the present invention, the support plate, and a peelable resin layer having a peelable surface, The glass / resin laminate so that the outermost surface of the other outermost layer of the glass / resin laminate is in close contact with the peelable surface of the peelable resin layer fixed to the surface (first main surface) of the support plate. It is related with the glass substrate laminated body by which the resin laminated body and the said support plate were laminated
- this invention relates to an electronic device provided with the glass / resin laminated body of this invention, and its manufacturing method.
- the present invention it is possible to provide a glass / resin laminate that is excellent in surface flatness and heat resistance and can suppress warpage and peeling during heating and cooling.
- a glass / resin laminate that is excellent in surface flatness and heat resistance and can suppress warpage and peeling during heating and cooling.
- the handling property of the glass / resin laminate is improved, and a conventional general single wafer sheet It becomes possible to input to the electronic device manufacturing process.
- FIG. 1 is a side view showing an embodiment of a glass / resin laminate according to the present invention.
- FIG. 2 is a side view showing another embodiment of the glass / resin laminate according to the present invention.
- FIG. 3 is a side view showing an embodiment of the glass substrate laminate according to the present invention.
- FIG. 4 is a process diagram showing an embodiment of a method for producing a glass substrate laminate according to the present invention.
- FIG. 5 is a process diagram showing an embodiment of a method for manufacturing an electronic device according to the present invention.
- FIG. 1 is a side view showing an embodiment of a glass / resin laminate according to the present invention.
- a glass substrate 12 and a resin layer 14 are laminated, and one outermost layer of the laminate is the glass substrate 12.
- the surface flatness of the glass / resin laminated body 10 can be improved.
- the glass substrate 12 and the resin layer 14 are in direct contact.
- the glass substrate 12 will be described.
- the glass substrate 12 can be obtained by melting a glass raw material and molding the molten glass into a plate shape.
- the molding method may be a general one, and for example, a float method, a fusion method, a slot down draw method, a redraw method, a pulling method, or the like is used.
- the glass substrate 12 may be, for example, a conventionally known alkali glass substrate containing an alkali metal oxide, or may be a non-alkali glass substrate, and is based on an applied electronic device and its manufacturing process. Although it selects suitably, it is preferable that it is a non-alkali glass substrate from the small heat shrinkage rate.
- the thermal shrinkage rate of the glass substrate 12 When the thermal shrinkage rate of the glass substrate 12 is large, the positional deviation at the time of cooling the component (for example, organic EL element) of the electronic device formed on the heated glass substrate 12 becomes excessive.
- a linear expansion coefficient defined in JIS R 3102-1995 is used as an index of the heat shrinkage rate.
- the average linear expansion coefficient at 25 to 300 ° C. of the glass substrate 12 (hereinafter simply referred to as “average linear expansion coefficient”) is preferably 0 to 200 ⁇ 10 ⁇ 7 / ° C., more preferably 0 to 100 ⁇ 10 ⁇ . 7 / ° C., more preferably 0 to 50 ⁇ 10 ⁇ 7 / ° C.
- the thickness of the glass substrate 12 is not particularly limited, but is preferably 0.3 mm or less, more preferably 0.2 mm or less, and still more preferably 0.15 mm or less from the viewpoint of weight reduction and thinning. . In the case of 0.3 mm or less, it is possible to give good flexibility to the glass substrate 12. In the case of 0.15 mm or less, the glass substrate 12 can be wound into a roll. Further, the thickness of the glass substrate 12 is preferably 0.02 mm or more for reasons such as easy manufacture of the glass substrate 12 and easy handling of the glass substrate 12.
- the shape of the glass substrate 12 is not particularly limited, but may be a rectangular shape or a belt shape. In any case, it is preferable that the width direction dimension (short direction dimension) of the glass substrate 12 is 2000 mm or less. When it exceeds 2000 mm, it becomes difficult to manufacture the resin layer 14 laminated on the glass substrate 12.
- the resin layer 14 includes a polyimide formed by condensation polymerization of aromatic diamines having a benzoxazole structure and aromatic tetracarboxylic acid anhydrides.
- the resin layer 14 consists only of the said polyimide.
- condensation polymerization for example, first, a diamine and a tetracarboxylic acid anhydride are subjected to a ring-opening polyaddition reaction in a solvent to obtain a polyamic acid solution, and then the polyamic acid solution is made necessary from this polyamic acid solution. Accordingly, it is performed by forming a green film or the like and then performing dehydration condensation (imidization).
- each isomer of amino (aminophenyl) benzoxazole for example, The compounds represented by the following formulas (1) to (4) are preferred.
- each isomer is each isomer determined according to the coordination position of two amino groups of amino (aminophenyl) benzoxazole.
- one or two or more diamines having no benzoxazole structure exemplified below may be used in combination as long as the total diamine is less than 30 mol%.
- diamines include 4,4′-bis (3-aminophenoxy) biphenyl, bis [4- (3-aminophenoxy) phenyl] ketone, and bis [4- (3-aminophenoxy) phenyl].
- some or all of the hydrogen atoms on the aromatic ring in the aromatic diamine are substituted with halogen atoms, alkyl groups having 1 to 3 carbon atoms or alkoxyl groups, cyano groups, and some or all of the hydrogen atoms with halogen atoms.
- the tetracarboxylic anhydrides used in this embodiment are aromatic tetracarboxylic dianhydrides.
- Specific examples of the aromatic tetracarboxylic dianhydrides include the following.
- tetracarboxylic dianhydrides may be used alone or in combination of two or more.
- one or two or more non-aromatic tetracarboxylic dianhydrides exemplified below may be used in combination as long as the total tetracarboxylic dianhydride is less than 30 mol%. Absent.
- Such tetracarboxylic dianhydrides include, for example, butane-1,2,3,4-tetracarboxylic dianhydride, pentane-1,2,4,5-tetracarboxylic dianhydride, cyclobutanetetra Carboxylic dianhydride, cyclopentane-1,2,3,4-tetracarboxylic dianhydride, cyclohexane-1,2,4,5-tetracarboxylic dianhydride, cyclohex-1-ene-2,3 , 5,6-tetracarboxylic dianhydride, 3-ethylcyclohex-1-ene-3- (1,2), 5,6-tetracarboxylic dianhydride, 1-methyl-3-ethylcyclohexane- 3- (1,2), 5,6-tetracarboxylic dianhydride, 1-methyl-3-ethylcyclohexane- 3- (1,2), 5,6-tetracarboxylic
- the solvent used when polymerizing diamines and tetracarboxylic acid anhydrides to obtain polyamic acid is not particularly limited as long as it dissolves both the raw material monomer and the polyamic acid to be produced.
- Solvents are preferred, for example, N-methyl-2-pyrrolidone, N-acetyl-2-pyrrolidone, N, N-dimethylformamide, N, N-diethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, hexamethylphosphoric Amides, ethyl cellosolve acetate, diethylene glycol dimethyl ether, sulfolane, halogenated phenols and the like can be mentioned.
- the amount of the solvent used may be an amount sufficient to dissolve the monomer as a raw material.
- the specific amount used is that the total mass of monomers in the solution in which the monomer is dissolved is usually 5 to 40 mass. %, Preferably 10 to 30% by mass.
- the conditions for the polymerization reaction (hereinafter also simply referred to as “polymerization reaction”) for obtaining the polyamic acid may be conventionally known conditions.
- the polymerization reaction is carried out in an organic solvent at a temperature range of 0 to 80 ° C. Stirring and / or mixing continuously for min to 30 hours. If necessary, the polymerization reaction may be divided or the temperature may be increased or decreased.
- the order of adding the two types of monomers is not particularly limited, but it is preferable to add aromatic tetracarboxylic anhydrides to the solution of aromatic diamines.
- the weight of the polyamic acid in the polyamic acid solution obtained by the polymerization reaction is preferably 5 to 50% by mass, more preferably 10 to 30% by mass, and the viscosity of the solution is measured with a Brookfield viscometer (25 ° C.). From the viewpoint of liquid feeding stability, it is preferably 10 to 2000 Pa ⁇ s, and more preferably 100 to 1000 Pa ⁇ s.
- Vacuum degassing during the polymerization reaction is effective for producing a good quality polyamic acid organic solvent solution.
- polymerization by adding a small amount of terminal blockers to aromatic diamines before a polymerization reaction.
- the terminal blocking agent include compounds having a carbon-carbon double bond such as maleic anhydride.
- the amount of maleic anhydride used is preferably 0.001 to 1.0 mole per mole of aromatic diamine.
- a green film is obtained by applying the polyamic acid solution on a support and drying, and then subjecting the green film to a heat treatment.
- a method of imidization reaction may be mentioned.
- the support on which the polyamic acid solution is applied should have a smoothness and rigidity sufficient to form the polyamic acid solution into a film, and a drum or belt whose surface is made of metal, plastic, glass, porcelain, etc. And the like.
- the surface of the support is preferably a metal, more preferably stainless steel that is resistant to rust and has excellent corrosion resistance.
- the surface of the support may be plated with metal such as Cr, Ni, or Sn.
- the surface of the support can be mirror-finished or processed into a satin finish as required.
- Application of the polyamic acid solution to the support includes, but is not limited to, casting from a slit base, extrusion through an extruder, squeegee coating, reverse coating, die coating, applicator coating, wire bar coating, etc.
- Conventionally known solution coating means can be appropriately used.
- the conditions for obtaining the green film by drying the polyamic acid solution coated on the support are not particularly limited, and the temperature is exemplified by 60 to 150 ° C., preferably 80 to 120 ° C., and the drying time is 5 ⁇ 180 minutes is exemplified, preferably 10 to 120 minutes, more preferably 30 to 90 minutes.
- a conventionally known drying apparatus that satisfies such conditions can be applied, and examples thereof include hot air, hot nitrogen, far infrared rays, and high frequency induction heating.
- an imidization reaction is performed. In general, the imidization reaction proceeds by treatment at a temperature higher than that of the drying, and a polyimide film can be obtained.
- the polyamic acid solution may contain a ring-closing catalyst and a dehydrating agent, and the imidization reaction may be promoted by the action of the ring-closing catalyst and the dehydrating agent.
- the imidization reaction is partially advanced to form a film having self-supporting property, and then imidization can be performed completely by heating.
- the timing for adding the ring closure catalyst to the polyamic acid solution is not particularly limited, and may be added in advance before the polymerization reaction for obtaining the polyamic acid.
- Specific examples of the ring-closing catalyst include aliphatic tertiary amines such as trimethylamine and triethylamine, and heterocyclic tertiary amines such as isoquinoline, pyridine, and betapicoline. Among them, heterocyclic tertiary amines are mentioned. At least one amine selected from is preferred.
- the amount of the ring-closing catalyst used per mole of polyamic acid is not particularly limited, but is preferably 0.5 to 8 moles.
- the timing of adding the dehydrating agent to the polyamic acid solution is not particularly limited, and may be added in advance before the polymerization reaction for obtaining the polyamic acid.
- Specific examples of the dehydrating agent include aliphatic carboxylic acid anhydrides such as acetic anhydride, propionic anhydride, butyric anhydride, and aromatic carboxylic acid anhydrides such as benzoic anhydride. Among them, acetic anhydride, benzoic anhydride, etc. Acids or mixtures thereof are preferred.
- the amount of dehydrating agent used per mole of polyamic acid is not particularly limited, but is preferably 0.1 to 4 moles. When a dehydrating agent is used, a gelation retarder such as acetylacetone may be used in combination.
- the polyimide film precursor (green film) formed on the support may be peeled off from the support before complete imidization, or may be peeled off after imidization.
- the coating amount when the polyamic acid solution is applied to the support and the concentration of the polyamic acid solution can be appropriately adjusted.
- Such a resin layer 14 containing polyimide obtained by polycondensation of aromatic diamines having a benzoxazole structure and aromatic tetracarboxylic acid anhydride is compared with a resin layer made of general polyimide, High heat resistance and low average linear expansion coefficient.
- the average linear expansion coefficient of the resin layer 14 is preferably 0 to 100 ⁇ 10 ⁇ 7 / ° C., more preferably 0 to 50 ⁇ 10 ⁇ 7 / ° C., and further preferably 0 to 30 ⁇ 10 ⁇ 7 / ° C. ° C. If it is in the said range, the difference of the average linear expansion coefficient of the glass substrate 12 and the resin layer 14 will not become excessive.
- the difference in average linear expansion coefficient between the glass substrate 12 and the resin layer 14 is preferably ⁇ 100 ⁇ 10 ⁇ 7 to + 100 ⁇ 10 ⁇ 7 / ° C. or less, more preferably ⁇ 50 ⁇ 10 ⁇ 7 to + 50 ⁇ 10. It is ⁇ 7 / ° C. or lower, more preferably ⁇ 30 ⁇ 10 ⁇ 7 to + 30 ⁇ 10 ⁇ 7 / ° C. or lower. If it is in the said range, the stress which generate
- the method for measuring the average linear expansion coefficient of the glass substrate 12 and the resin layer 14 will be described in detail in the column of Examples.
- the average linear expansion coefficient of the polyimide film as the resin layer 14 can be easily controlled by the molecular weight of the precursor (polyamic acid) and heat treatment conditions. Further, in the formation of the resin layer 14, it is necessary to control the conditions of the drying and imidization steps so as to suppress the disorder in the molecular direction and take a uniform structure.
- the thickness of the resin layer 14 is not particularly limited, but is preferably 0.1 mm or less from the viewpoint of weight reduction and thinning.
- the thickness of the resin layer 14 is preferably 0.02 mm or more from the viewpoint of impact resistance.
- the manufacturing method of the glass / resin laminated body 10 is not specifically limited, For example, the glass substrate 12 and the polyimide film which is the resin layer 14 are prepared separately, and the glass substrate 12 and the polyimide film are laminated by heat fusion or the like. And a method of directly forming the resin layer 14 on the glass substrate 12.
- At least one of the surfaces 12a and 14a on the side of the polyimide film that is the glass substrate 12 and the resin layer 14 that are in contact with each other is previously cleaned before lamination. It is preferable to perform a treatment and / or a surface treatment.
- the cleaning process may be a general process used for cleaning glass or resin.
- glass cleaning includes ultrasonic cleaning, ceria polishing using ceria abrasive grains, acid cleaning using hydrofluoric acid or nitric acid, alkali cleaning using ammonia or potassium hydroxide, surfactants (including detergents) ), Photochemical cleaning using ultraviolet light or ozone, and physical cleaning using plasma. These washing treatments are used alone or in combination. After the cleaning, if necessary, drying is performed so that no cleaning agent remains.
- the surface treatment may be a general treatment used for glass or resin surface treatment, and examples thereof include corona treatment, plasma treatment, flame treatment, and silane coupling treatment. These surface treatments may be used alone or in combination.
- silane coupling agent examples include 3- (meth) acryloxypropyltrimethoxysilane, 3- (meth) acryloxypropyltriethoxysilane, 3-aminopropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3 -Isocyanatopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and the like.
- the polyimide is applied to the glass substrate 12 using a laminating apparatus or a pressing apparatus.
- a film may be laminated.
- a green film is formed by applying a polyamic acid solution on the glass substrate 12 and drying, and then, similarly to the imidization reaction of the green film.
- the resin layer 14 may be formed by heating in a state where a green film is formed on the glass substrate 12 and imidizing the green film.
- FIG. 2 is a side view showing another embodiment of the glass / resin laminate according to the present invention.
- the configuration of the glass / resin laminate 20 shown in FIG. 2 will be described, but the same components as those of the glass / resin laminate 10 shown in FIG.
- the glass / resin laminate 10 shown in FIG. 1 has a configuration in which the glass substrate 12 and the resin layer 14 are in direct contact.
- the glass / resin laminate 20 shown in FIG. 2 has a configuration in which the glass substrate 12 and the resin layer 14 are laminated via the adhesive layer 22.
- the glass substrate 12 and the resin layer 14 can be reliably fixed by the adhesive force of the adhesive layer 22.
- thermoplastic polyamideimide thermoplastic polyimide
- thermoplastic polyimidesiloxane thermoplastic polyamideimidesiloxane
- polyetheretherketone liquid crystal polymer
- polyphenylene examples thereof include oxides and epoxy resins.
- thermoplastic polyamideimide and thermoplastic polyimide are preferable from the viewpoint of heat resistance.
- the adhesive layer 22 mainly composed of thermoplastic polyamideimide and thermoplastic polyimide has a 5% heating weight loss temperature of 400 ° C. or higher, and has high heat resistance.
- the 5% heating weight loss temperature refers to a temperature at which a weight loss of 5% occurs when about 10 mg of a sample is heated by a differential thermal balance at a heating rate of 10 ° C./min.
- These materials may be used alone or in combination of two or more.
- organic and inorganic fillers, flame retardants, and the like may be added to these materials.
- the glass transition point Tg of the adhesive layer 22 is preferably 130 to 400 ° C. If the glass transition point Tg of the adhesive layer 22 is lower than 130 ° C., the adhesive layer 22 may be deformed during the heat treatment in the manufacturing process of the electronic device. On the other hand, when the glass transition point Tg of the adhesive layer 22 is higher than 400 ° C., it becomes difficult to form a multilayer film described later. A more preferable glass transition point Tg is 240 to 400 ° C.
- the manufacturing method of the glass / resin laminated body 20 is not specifically limited, For example, after forming the adhesive layer 22 on the surface 12a on the resin layer 14 side of the glass substrate 12, the side that contacts the resin layer 14 of the adhesive layer 22 A method of laminating a polyimide film as the resin layer 14 on the surface of the glass substrate 12, a surface of the multilayer film adhesive layer 22 in which the resin layer 14 and the adhesive layer 22 are integrated, on the surface in contact with the glass substrate 12. There is a method of laminating.
- the adhesive layer 22 is made of thermoplastic polyimide will be described.
- a precursor layer is formed by applying and drying a polyamic acid solution that becomes a thermoplastic polyimide on the glass substrate 12, and then an adhesive layer 22 is formed by imidizing the precursor layer. To do.
- the multilayer film is formed by co-extrusion, by casting the other polyamic acid solution on the polyimide film as one layer 14 (22), and imidizing it.
- the glass substrate 12 / adhesive layer 22 / resin layer 14 may be laminated using a laminating apparatus or a pressing apparatus. Thereby, adhesiveness can be improved.
- the resin layer 14 polycondenses the aromatic diamine having the benzoxazole structure and the aromatic tetracarboxylic acid anhydride. Therefore, the resin layer 14 has higher heat resistance than the case where the resin layer 14 is made of general polyimide, and the difference in average linear expansion coefficient between the resin layer 14 and the glass substrate 12 is ⁇ 100. It is within ⁇ 10 ⁇ 7 to + 100 ⁇ 10 ⁇ 7 / ° C. For this reason, while being able to improve heat resistance, the curvature at the time of heating and cooling and peeling can be suppressed.
- At least one outermost layer is the glass substrate 12
- surface flatness can be improved compared with the case where both outermost layers are resin layers.
- a constituent member (for example, an organic EL element) of an electronic device can be accurately formed on the surface of the glass / resin laminate 10 (20) on the glass substrate 12 side.
- both outermost layers are glass substrates. There may be. Further, it may be a glass / resin laminate in which a plurality of glasses and resin layers are alternately laminated, such as glass / resin / glass / resin or glass / resin / glass / resin / glass. In this case, the number of repetitions of the glass and the resin layer is not particularly limited.
- the method for producing a glass / resin laminate in which a plurality of glass and resin layers are alternately laminated is not particularly limited.
- a glass / resin laminate can be produced by a method such as an imidization reaction method or a combination of these methods.
- the thus obtained glass / resin laminate 10 (20) is suitably used for electronic devices such as direct top emission type organic EL panels, solar cells, thin film secondary batteries and the like.
- the manufacturing method of the organic EL panel includes a step of forming an organic EL element on the glass substrate 12 of the glass / resin laminate 10 (20).
- a well-known vapor deposition technique, a sealing technique, etc. are used.
- the organic EL element may have a general configuration, and includes, for example, an electrode layer sequentially stacked on the glass substrate 12, an organic layer including a light emitting layer, a transparent electrode layer, and the like.
- the method for manufacturing a solar cell includes a step of forming a solar cell element on the glass substrate 12 of the glass / resin laminate 10 (20). In this step, a well-known photolithography technique, film forming technique, vapor deposition technique, sealing technique, or the like is used.
- the solar cell element may have a general configuration, and includes, for example, an electrode layer sequentially stacked on the glass substrate 12, a semiconductor layer made of a p-type semiconductor and an n-type semiconductor, a transparent electrode layer, and the like.
- the method for manufacturing a thin film secondary battery includes a step of forming a thin film secondary battery element on the glass substrate 12 of the glass / resin laminate 10 (20). In this step, a well-known photolithography technique or the like is used.
- the thin film secondary battery element may have a general configuration, for example, a first current collector layer, a positive electrode layer, a solid electrolyte layer, a negative electrode layer, and a second current collector layer sequentially stacked on the glass substrate 12. Etc.
- an electronic device can be formed on the glass substrate 12 as it is in a roll-to-roll manufacturing process.
- a glass / resin laminate 10 (20) obtained by cutting the belt-shaped glass / resin laminate 10 (20) into a rectangular shape, a rectangular glass substrate 12 and a resin film as the rectangular resin layer 14 were laminated.
- the thickness of the glass / resin laminate 10 (20) is the same. When it is thin, there are the following problems.
- the glass / resin laminate 10 (20) When the glass / resin laminate 10 (20) is thin, the glass / resin laminate 10 (20) has flexibility. Therefore, when the glass / resin laminate 10 (20) is put into a general sheet-fed electronic device manufacturing process, There is a possibility that the resin laminate 10 (20) is bent and the constituent members of the electronic device cannot be accurately formed on the glass substrate 12 of the glass / resin laminate 10 (20).
- the glass / resin laminate 10 (20) it is possible to prevent the glass / resin laminate 10 (20) from being bent by attaching a support plate described later to the glass / resin laminate 10 (20) to obtain a glass substrate laminate.
- the thickness of glass / resin laminated body 10 (20) is 50 micrometers or more from a viewpoint of handling property.
- FIG. 3 is a side view showing an embodiment of the glass substrate laminate according to the present invention.
- the glass substrate laminate 30 includes a glass / resin laminate 10, a support plate 32, and a peelable resin layer 34 having a peelable surface (hereinafter referred to as “peelable resin layer 34”).
- the glass substrate laminate 30 has a rectangular shape, and is formed by closely contacting the outermost surface of the other outermost layer of the glass / resin laminate 10 and the peelable surface of the peelable resin layer 34.
- the other outermost layer of the glass / resin laminate means the outermost layer on the opposite side of one outermost layer formed of the glass substrate in the glass / resin laminate.
- the glass substrate laminate 30 shown in FIG. 3 has a configuration in which the glass / resin laminate 10 and the support plate 32 shown in FIG. 1 are laminated via the peelable resin layer 34, but the glass shown in FIG. Of course, it is possible to use the glass / resin laminate 20 shown in FIG. 2 instead of the resin laminate 10.
- the other outermost layer of the glass / resin laminate is also a glass substrate. is there. Therefore, in this case, the glass substrate and the peelable resin layer 34 are in close contact.
- the support plate 32 is not particularly limited as long as it supports the glass / resin laminate 10 via a peelable resin layer 34 described later and reinforces the strength of the glass / resin laminate 10.
- the material of the support plate 32 is not particularly limited, but a glass plate, a silicon wafer, a metal plate, a plastic plate, and the like are preferable examples from the viewpoint of industrial availability.
- the composition thereof may be the same as, for example, glass containing an alkali metal oxide or alkali-free glass.
- alkali-free glass is preferable because of its low thermal shrinkage rate.
- the difference in linear expansion coefficient between the glass / resin laminate 10 and the glass used for the support plate 32 is preferably ⁇ 150 ⁇ 10 ⁇ 7 to + 150 ⁇ 10 ⁇ 7 / ° C. or less, and ⁇ 100 ⁇ 10 ⁇ 7 to It is more preferably + 100 ⁇ 10 ⁇ 7 / ° C. or less, and further preferably ⁇ 50 ⁇ 10 ⁇ 7 to + 50 ⁇ 10 ⁇ 7 / ° C. or less.
- the type is not particularly limited.
- polyethylene terephthalate resin, polycarbonate resin, polyimide resin, fluorine resin, polyamide resin, polyaramid resin, polyethersulfone resin, polyetherketone resin examples include polyether ether ketone resins, polyethylene naphthalate resins, polyacrylic resins, various liquid crystal polymer resins, and polysilicon resins.
- the type thereof is not particularly limited, and examples thereof include a stainless steel plate and a copper plate.
- the heat resistance of the support plate 32 is not particularly limited. However, when the glass / resin laminate 10 is laminated on the support plate 32 and a TFT array or the like that is a component of an electronic device is formed, the heat resistance is high. Is preferred. Specifically, the 5% heating weight loss temperature (temperature increase rate: 10 ° C./min) is preferably 300 ° C. or higher. Furthermore, it is more preferable that it is 350 degreeC or more.
- any of the above glass plates is applicable in terms of heat resistance.
- plastic plates include polyimide resin, fluororesin, polyamide resin, polyaramid resin, polyethersulfone resin, polyetherketone resin, polyetheretherketone resin, polyethylene naphthalate resin, various liquid crystal polymer resins, etc. Is exemplified.
- the thickness of the support plate 32 is not particularly limited, but is preferably 0.3 mm or more from the viewpoint of reinforcing the strength of the glass / resin laminate 10.
- the thickness of the support plate 32 is a thickness that can be input to a general electronic device manufacturing process of a single sheet.
- the thickness is preferably 0.1 to 1.1 mm, more preferably 0.3 to 0.8 mm, and still more preferably 0.4 to 0.7 mm.
- the current electronic device manufacturing process is designed to process a substrate having a thickness of 0.5 mm, and the thickness of the glass / resin laminate 10 is 0.1 mm, The sum of the thickness and the thickness of the peelable resin layer 34 is 0.4 mm.
- the support plate 32 is preferably thicker than the glass / resin laminate 10.
- the surface of the support plate 32 composed of the various materials described above may be a polished surface that has been polished or a non-etched surface (fabric surface) that has not been polished. There may be. From the viewpoint of productivity and cost, a non-etched surface (fabric surface) is preferable.
- the shape of the support plate 32 is not limited, but is preferably rectangular.
- the rectangle is substantially a rectangle and includes a shape obtained by cutting off the corners of the peripheral portion (corner cut).
- the size of the support plate 32 is not limited, for example, in the case of a rectangle, it may be 100 to 2000 mm ⁇ 100 to 2000 mm, and preferably 500 to 1000 mm ⁇ 500 to 1000 mm.
- the peelable resin layer 34 is fixed on the support plate 32 described above, and the glass / resin laminate 10 is laminated.
- the peelable surface of the peelable resin layer 34 is in close contact with the outermost surface of the other outermost layer of the glass / resin laminate 10, but has surface characteristics that allow the glass / resin laminate 10 to be easily peeled off. . That is, the peelable surface of the peelable resin layer 34 is bonded to the outermost surface of the other outermost layer of the glass / resin laminate 10 with a certain amount of bonding force, and the glass / resin laminate 10 is displaced.
- the glass / resin laminate 10 is peeled from the glass substrate laminate 30, the glass / resin laminate 10 is bonded with a binding force that can be easily peeled without breaking the glass / resin laminate 10. Yes.
- the property which can peel this resin layer surface easily is called peelability.
- the peelable surface of the peelable resin layer 34 and the outermost surface of the other outermost layer of the glass / resin laminate 10 are not attached by the adhesive force that the adhesive has, and solid molecules It is preferable that it is attached by the force resulting from the van der Waals force between them, that is, the adhesion force.
- the bond strength of the peelable resin layer 34 to the surface of the support plate 32 is relatively higher than the bond strength of the peelable surface of the peelable resin layer 34 to the outermost surface of the other outermost layer of the glass / resin laminate 10.
- the bonding of the peelable resin layer 34 to the glass / resin laminate 10 is referred to as adhesion
- the bonding to the support plate 32 is referred to as fixing.
- the thickness of the peelable resin layer 34 is not particularly limited. It is preferably 5 to 50 ⁇ m, more preferably 5 to 30 ⁇ m, and even more preferably 7 to 20 ⁇ m. This is because when the thickness of the peelable resin layer 34 is in such a range, the glass / resin laminate 10 and the peelable resin layer 34 are sufficiently adhered. Moreover, even if air bubbles or foreign substances are present, the occurrence of distortion defects in the glass / resin laminate 10 can be suppressed. On the other hand, if the resin layer is too thick, it takes time and materials to form the resin layer, which is not economical.
- the peelable resin layer 34 may be composed of two or more layers.
- “the thickness of the peelable resin layer” means the total thickness of all the peelable resin layers 34.
- the type of resin forming each layer may be different.
- the peelable resin layer 34 preferably has a surface tension of 30 mN / m or less, more preferably 25 mN / m or less, and even more preferably 22 mN / m or less. Moreover, it is preferable that it is 15 mN / m or more. If the surface tension is in such a range, the glass / resin laminate 10 can be more easily peeled, and at the same time, the adhesion with the glass / resin laminate 10 becomes sufficient.
- the glass transition point of the peelable resin layer 34 is preferably lower than room temperature (about 25 ° C.) or made of a material having no glass transition point. By satisfying this condition, it becomes a non-adhesive resin layer, has more releasability, can be more easily peeled off from the glass / resin laminate 10, and at the same time has sufficient adhesion to the glass / resin laminate 10 Because there is a tendency to become.
- the peelable resin layer 34 has heat resistance.
- the glass / resin laminate 10 can be subjected to a heat treatment in the electronic device manufacturing process.
- the required heat resistance varies depending on the electronic device manufacturing process, but is preferably 180 ° C. or higher, particularly preferably 300 ° C. or higher.
- the elastic modulus of the peelable resin layer 34 is too high, the adhesion with the glass / resin laminate 10 tends to be low. If the elastic modulus is too low, the peelability is lowered.
- the type of resin that forms the peelable resin layer 34 is not particularly limited.
- acrylic resin, polyolefin resin, polyurethane resin, and silicone resin can be used.
- Several types of resins can be mixed and used. Of these, silicone resins are preferred. This is because the silicone resin is excellent in heat resistance and excellent in peelability from the glass / resin laminate 10.
- the support plate 32 is a glass plate, it is easy to fix to the support glass plate by a condensation reaction with the silanol group on the surface. It is also preferable that the silicone resin layer does not substantially deteriorate peelability even when it is treated at about 300 to 400 ° C. for about 1 hour, for example.
- the peelable resin layer 34 is preferably made of a silicone resin (cured product) used for release paper among the silicone resins.
- a peelable resin layer 34 formed by curing a curable resin composition to be a silicone resin for release paper on the surface of the support plate 32 is preferable because it has excellent peelability.
- the flexibility is high, even if foreign matter such as bubbles or dust is mixed between the glass / resin laminate 10 and the peelable resin layer 34, the occurrence of distortion defects in the glass / resin laminate 10 is suppressed. be able to.
- the curable silicone that becomes the silicone resin for the release paper is classified into a condensation reaction type silicone, an addition reaction type silicone, an ultraviolet curable type silicone, and an electron beam curable type silicone, depending on the curing mechanism. Can do.
- addition reaction type silicone is preferable. This is because the addition reaction type silicone is easy to cure, has a good degree of peelability when the peelable resin layer 34 is formed, and has high heat resistance.
- Addition reaction type silicone is a curable resin composition comprising a combination of an organoalkenylpolysiloxane having an unsaturated group such as a vinyl group, an organohydrogenpolysiloxane having a hydrogen atom bonded to a silicon atom, and a catalyst such as a platinum-based catalyst. It is a silicone resin that is cured by curing at room temperature or by heating.
- the curable silicone that becomes the silicone resin for the release paper is classified into a solvent type, an emulsion type, and a solventless type, and any type can be used.
- a solventless type is preferable. This is because the solventless type is excellent in terms of productivity, safety, and environmental characteristics. Further, it does not contain a solvent that causes foaming at the time of curing at the time of forming the resin layer, that is, at the time of heat curing, ultraviolet curing, or electron beam curing, so that bubbles are unlikely to remain in the peelable resin layer 34.
- curable silicone used as the silicone resin for release paper specifically, commercially available product names or model numbers are KNS-320A, KS-847 (both manufactured by Shin-Etsu Silicone), TPR6700 (manufactured by GE Toshiba Silicone).
- KNS-320A, KS-847, and TPR6700 are curable silicones that contain a main agent and a crosslinking agent in advance.
- the silicone resin forming the peelable resin layer 34 preferably has a property that the components in the silicone resin layer are difficult to migrate to the glass / resin laminate 10, that is, low silicone migration.
- the method for producing the glass substrate laminate of the present embodiment is not particularly limited.
- a peelable resin layer forming step for forming and fixing the peelable resin layer 34 on the support plate 32 (step S10).
- an adhesion step (step S12) for closely adhering the outermost surface of the other outermost layer of the glass / resin laminate 10 and the peelable surface of the peelable resin layer 34 to the glass substrate laminate. It is preferable.
- such a manufacturing method is also referred to as “the manufacturing method of the present embodiment”.
- step S10 the peelable resin layer forming step
- the method for forming the peelable resin layer 34 on the support plate 32 is not particularly limited.
- the method of fixing film-like peelable resin to the surface of a support plate is mentioned.
- a method of performing surface modification treatment (priming treatment) on the surface of the support plate and fixing it on the support plate can be mentioned.
- a chemical method (primer treatment) that improves the fixing force chemically such as a silane coupling agent
- a physical method that increases surface active groups such as a flame (flame) treatment
- a surface such as a sandblast treatment Examples of such a mechanical processing method increase the catch by increasing the roughness of the material.
- a method of coating the support plate 32 with a curable resin composition that becomes the peelable resin layer 34 by a known method may be mentioned.
- Known methods include spray coating, die coating, spin coating, dip coating, roll coating, bar coating, screen printing, and gravure coating. From such a method, it can select suitably according to a kind to a resin composition.
- the coating amount is preferably 1 to 100 g / m 2 and 5 to 20 g / m 2. Is more preferable.
- a curable resin composition comprising a mixture of an alkenylpolysiloxane, an organohydrogenpolysiloxane, and a catalyst is used for the known spray coating method. It can be coated on the support plate 32 by the above method, and then cured by heating.
- the heat curing conditions vary depending on the blending amount of the catalyst. For example, when 2 parts by weight of a platinum-based catalyst is blended with respect to 100 parts by weight of the total amount of alkenylpolysiloxane and organohydrogenpolysiloxane, 50 in the atmosphere.
- the reaction is carried out at a temperature of from ° C to 250 ° C, preferably 100 ° C to 200 ° C. In this case, the reaction time is 5 to 60 minutes, preferably 10 to 30 minutes.
- the reaction temperature and reaction time as described above are preferable because almost no unreacted silicone component remains in the silicone resin layer. If the reaction time is too long or the reaction temperature is too high, the oxidative decomposition of the silicone resin occurs at the same time, and a low molecular weight silicone component is produced, which may increase the silicone transferability. It is preferable to allow the curing reaction to proceed as much as possible so that almost no unreacted silicone component remains in the silicone resin layer in order to improve the peelability after the heat treatment.
- the peelable resin layer 34 is manufactured using a curable resin composition that becomes a silicone resin for release paper
- the curable resin composition coated on the support plate 32 is heated and cured to form a silicone resin layer.
- the silicone resin is chemically bonded to the support plate 32 during the curing reaction.
- the silicone resin layer is bonded to the support plate 32 by the anchor effect. By these actions, the silicone resin layer is firmly fixed to the support plate 32.
- step S12 the adhesion process
- the adhesion step is a step of bringing the outermost surface of the other outermost layer of the glass / resin laminate 10 into close contact with the peelable surface of the peelable resin layer 34.
- the outermost surface of the other outermost layer of the glass / resin laminate 10 and the peelable surface of the peelable resin layer 34 are in close proximity to each other due to van der Waals forces between opposing solid molecules, that is, It is preferable that it adheres by adhesive force.
- the support plate 32 and the glass / resin laminate 10 can be held in a laminated state.
- the method for laminating the glass / resin laminate 10 on the peelable surface of the peelable resin layer 34 fixed to the support plate 32 is not particularly limited. For example, it can implement using a well-known method. For example, after the glass / resin laminate 10 is stacked on the peelable surface of the peelable resin layer 34 under a normal pressure environment, the peelable resin layer 34 and the glass / resin laminate 10 are pressure-bonded using a roll or a press. A method is mentioned. It is preferable because the peelable resin layer 34 and the glass / resin laminate 10 are more closely adhered by pressure bonding with a roll or a press.
- air bubbles mixed between the peelable resin layer 34 and the glass / resin laminate 10 are relatively easily removed by pressure bonding with a roll or a press.
- pressure bonding is performed by a vacuum laminating method or a vacuum pressing method, it is more preferable because suppression of mixing of bubbles and securing of good adhesion are more preferably performed.
- press-bonding under vacuum even if minute bubbles remain, there is an advantage that the bubbles do not grow by heating and are not likely to lead to a distortion defect of the glass / resin laminate 10.
- the adhesion step when the glass / resin laminate 10 is laminated on the peelable resin layer 34 on the support plate 32, the other outermost surface of the glass / resin laminate 10 and the peelable resin layer 34 are peeled off. It is preferable that the surface is sufficiently washed and laminated in a clean environment. Even if a foreign substance is mixed between the peelable resin layer 34 and the glass / resin laminate 10, the peelable resin layer 34 is deformed so that the flatness of the surface of the glass / resin laminate 10 is not affected. However, the higher the degree of cleanness, the better the flatness.
- the glass substrate laminate 30 can be manufactured by such a manufacturing method of the present embodiment.
- Method for manufacturing electronic device is not specifically limited, For example, as shown in FIG. 5, on the surface of the glass substrate 12 of the glass substrate laminated body 30, the structural member formation process of forming at least one part of the structural member of an electronic device ( It is preferable to manufacture by the method provided with the isolation
- step S20 the constituent member forming step
- a method for forming at least a part of the constituent members of the electronic device on the surface of the glass substrate 12 of the glass / resin laminate is not particularly limited, and a conventionally known method is performed according to the type of the constituent members of the electronic device.
- a process for forming an organic EL structure on the glass substrate 12 of the glass / resin laminate 10 As a process for forming an organic EL structure on the glass substrate 12 of the glass / resin laminate 10, a process of forming a transparent electrode, a hole injection layer and hole transport Various processes such as a process of depositing a layer, a light emitting layer, an electron transport layer, and the like, and a sealing process are included. Specific examples of the process performed in these steps include a film forming process, a vapor deposition process, and a sealing plate bonding process. The formation of these components may be part of the formation of all components required for the electronic device.
- the method for separating the glass / resin laminate 10 and the peelable resin layer 34 is not particularly limited. Specifically, for example, a sharp blade-like object was inserted into the interface between the outermost surface of the other outermost layer of the glass / resin laminate 10 and the peelable surface of the peelable resin layer 34 to give a trigger for peeling.
- the glass / resin laminate 10 and the peelable resin layer 34 can be separated by spraying a mixed fluid of water and compressed air. Preferably, it is placed on a surface plate so that the peelable resin layer 34 is on the upper side and the glass / resin laminate 10 is on the lower side, and the glass / resin laminate 10 side is vacuum-adsorbed on the surface plate in this state.
- the blade is inserted into the interface between the outermost surface of the other outermost layer of the glass / resin laminate 10 and the peelable surface of the peelable resin layer 34.
- the peelable resin layer 34 is adsorbed by a plurality of vacuum suction pads, and the vacuum suction pads are raised in order from the vicinity of the place where the blade is inserted. If it does so, an air layer will be formed in the said interface, the air layer will spread over the whole surface of an interface, and the glass / resin laminated body 10 and the peelable resin layer 34 can be isolate
- an electronic device in which at least a part of the constituent members of the electronic device is formed on the glass substrate 12 of the glass / resin laminate 10 is obtained.
- the constituent members on the glass substrate 12 at the time of separation are part of the formation of all the constituent members necessary for the electronic device, the remaining constituent members are then used as the glass substrate of the glass / resin laminate 10. 12 on the electronic device.
- Test piece warpage Place a test piece (50 mm x 300 mm) on a surface plate, and measure the maximum value of each gap between the surface plate and the longitudinal center of the test piece and both ends in the longitudinal direction using a gap gauge. did. 5.
- Example 1 In Example 1, a glass / resin laminate 10 shown in FIG. 1 was produced as a test piece.
- a non-alkali glass substrate (AN100 manufactured by Asahi Glass Co., Ltd.) having a width of 500 mm and a thickness of 70 ⁇ m obtained by a float process was used.
- the average linear expansion coefficient of the glass substrate 12 was 38 ⁇ 10 ⁇ 7 / ° C.
- this glass substrate 12 was activated by UV cleaning. Next, the glass substrate 12 was rolled up while laminating protective films on both surfaces of the glass substrate 12.
- Example 2 In Example 2, the glass / resin laminate 20 shown in FIG. 2 was manufactured as a test piece.
- Glass substrate 12 As the glass substrate 12, a non-alkali glass substrate (AN100 manufactured by Asahi Glass Co., Ltd.) having a length of 500 mm, a width of 500 mm, and a thickness of 45 ⁇ m obtained by a float process was used.
- the average linear expansion coefficient of the glass substrate 12 was 38 ⁇ 10 ⁇ 7 / ° C.
- Resin layer 14 As the resin layer 14, a heat-resistant polyimide film having a length of 500 mm ⁇ width of 500 mm ⁇ thickness of 30 ⁇ m produced in the same manner as in Example 1 was used. This heat-resistant polyimide film had an average linear expansion coefficient of 30 ⁇ 10 ⁇ 7 / ° C., and the difference from the average linear expansion coefficient with the glass substrate 12 was 8 ⁇ 10 ⁇ 7 / ° C.
- thermoplastic polyimide film as adhesive layer 22 After purging the inside of the reaction vessel equipped with a nitrogen introduction tube, a thermometer, and a stirring rod with nitrogen, 368.4 parts by mass of 4,4′-bis (3-aminophenoxy) biphenyl, 59.24 parts by mass of phthalic anhydride 174.5 parts by mass of pyromellitic anhydride and 172 parts by mass of m-cresol 2 were added and stirred at 200 ° C. for 6 hours. Toluene was added to this stirred solution, and then the precipitate was filtered off, further washed with toluene three times, and then dried at 250 ° C. for 6 hours under a nitrogen atmosphere to obtain 510 parts by mass (yield 90.1). %) Of polyimide powder.
- the polyimide powder was kneaded at 380 to 410 ° C. using a twin screw extruder, melted and extruded to be granulated into pellets.
- the obtained pellets were supplied to a single screw extruder (molding temperature 420 ° C.) having a diameter of 50 mm, passed through a 10 ⁇ m leaf disk type filter attached to the front part of the T die, extruded from a 1100 mm wide T die, and an adhesive layer.
- a thermoplastic polyimide film having a thickness of 25 and a thickness of 25 ⁇ m was obtained.
- the thermoplastic polyimide film had a 5% weight loss by heating (temperature increase rate: 10 ° C./min) of 580 ° C. and a glass transition point Tg of 270 ° C.
- thermoplastic polyimide film was set between the glass substrate 12 and the heat-resistant polyimide film, and was pressed at 300 ° C. and 1 MPa for 5 minutes by a hot press apparatus to obtain a glass / resin laminate 20 shown in FIG.
- Comparative Example 1 a glass / resin laminate was obtained in the same manner as in Example 2 except that a polyimide film (manufactured by Toray DuPont, Kapton H) having a thickness of 30 ⁇ m was used as the resin layer 14.
- the polyimide film (Kapton H) is obtained by condensation polymerization of pyromellitic anhydride and diaminodiphenyl ether, has an average linear expansion coefficient of 270 ⁇ 10 ⁇ 7 / ° C., and an average line with the glass substrate 12. The difference in expansion coefficient was 232 ⁇ 10 ⁇ 7 / ° C.
- Comparative Example 2 In Comparative Example 2, the polyimide film (Kapton H) was used as a test piece.
- Comparative Example 3 a non-alkali glass film (manufactured by Asahi Glass Co., Ltd., AN100) having a thickness of 100 ⁇ m was used as a test piece.
- Table 1 summarizes the above evaluation results for each example and comparative example.
- Example 3 a glass / resin laminate 10 shown in FIG. 1 was produced as a test piece by a method different from that in Example 1.
- a non-alkali glass substrate (AN100 manufactured by Asahi Glass Co., Ltd.) having a width of 500 mm and a thickness of 70 ⁇ m obtained by a float process was used.
- the average linear expansion coefficient of the glass substrate 12 was 38 ⁇ 10 ⁇ 7 / ° C.
- this glass substrate 12 was activated by UV cleaning. Next, the glass substrate 12 was rolled up while laminating protective films on both surfaces of the glass substrate 12.
- This polyamic acid solution is applied onto the glass substrate 12 after the silane coupling treatment using a comma coater, passed through a continuous heat treatment furnace, heat treated at 110 ° C. for 2 minutes, and heat treated at 150 ° C. for 2 minutes. Then, heat treatment was performed at 220 ° C. for 2 minutes, and then heat treatment was performed at 475 ° C. for 4 minutes to obtain the glass / resin laminate 10 shown in FIG.
- Example 4 First, a support glass plate (Asahi Glass Co., Ltd., AN100) having a length of 500 mm, a width of 500 mm, a thickness of 0.6 mm, and a linear expansion coefficient of 38 ⁇ 10 ⁇ 7 / ° C. is cleaned with pure water and UV to clean the surface. Prepared as a support plate.
- a support glass plate Asahi Glass Co., Ltd., AN100
- a resin for forming the peelable resin layer linear dimethylpolysiloxane having vinyl groups at both ends and methylhydrogenpolysiloxane having hydrosilyl groups in the molecule were used. Then, this is mixed with a platinum-based catalyst to prepare a mixture, which is coated on a first main surface of the support glass plate with a size of 499 mm in length and 499 mm in width with a die coater (coating amount 20 g / m). 2 ) Heat-cured in air
- the mixing ratio of linear dimethylpolysiloxane and methylhydrogenpolysiloxane was adjusted so that the molar ratio of hydrosilyl group and vinyl group was 0.9 / 1.
- the platinum-based catalyst was added in an amount of 5 parts by mass with respect to a total of 100 parts by mass of linear dimethylpolysiloxane and methylhydrogenpolysiloxane.
- the peelable surface of the silicone resin layer fixed to the surface of the supporting glass plate and the outermost surface of the resin layer 14 of the glass / resin laminate 10 A laminated glass substrate laminate A (glass substrate laminate A of the present invention) was obtained by vacuum pressing at room temperature so that the centers of gravity of both substrates overlap.
- Example 5 an OLED is manufactured using the glass substrate laminate A obtained in Example 4.
- the glass / resin laminate 10 is cut using a laser cutter or a scribe-break method, and divided into 80 cells of 41 mm in length and 30 mm in width, and then a glass / resin laminate in which an organic EL structure is formed.
- the body 10 and the counter substrate are assembled, and a module forming process is performed to create an OLED.
- the OLED obtained in this way does not have a problem in characteristics.
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- Electroluminescent Light Sources (AREA)
Abstract
Description
前記樹脂層は、ベンゾオキサゾール構造を有する芳香族ジアミン類と、芳香族テトラカルボン酸無水物類とを縮重合させてなるポリイミドを含み、
前記ガラス基板と前記樹脂層との、25~300℃における平均線膨張係数の差が-100×10-7~+100×10-7/℃であり、
積層体の少なくとも一方の最外層が前記ガラス基板であるガラス/樹脂積層体に関する。
本発明のガラス/樹脂積層体、支持板、ならびに剥離性表面を有する剥離性樹脂層、を有し、
前記ガラス/樹脂積層体の他方の最外層の最外面と、前記支持板の表面(第1主面)に固定された前記剥離性樹脂層の剥離性表面とが密着するように、前記ガラス/樹脂積層体と前記支持板とが前記剥離性樹脂層を介して積層された、ガラス基板積層体及びその製造方法に関する。
本実施形態で用いられるベンゾオキサゾール構造を有する芳香族ジアミン類の分子構造は、特に限定されるものではないが、合成し易さの観点から、アミノ(アミノフェニル)ベンゾオキサゾールの各異性体(例えば、下記式(1)~式(4)で表される各化合物)が好ましい。ここで、「各異性体」とは、アミノ(アミノフェニル)ベンゾオキサゾールが有する2つのアミノ基の配位位置に応じて定められる各異性体である。これらのジアミンは、単独で用いてもよいし、二種以上を併用してもよい。
本実施形態で用いられるテトラカルボン酸無水物類は芳香族テトラカルボン酸二無水物類である。芳香族テトラカルボン酸二無水物類としては、具体的には、以下のものが挙げられる。
また、ガラス/樹脂/ガラス/樹脂や、ガラス/樹脂/ガラス/樹脂/ガラスのように、ガラスと樹脂層が交互に複数積層されたガラス/樹脂積層体であってもよい。この場合、ガラスと樹脂層の繰り返し回数は特に限定されない。また、ガラスと樹脂層を交互に複数積層したガラス/樹脂積層体を製造する方法は特に限定されない。例えば、複数のガラスと複数のポリイミドフィルムとを交互に重ねて熱融着する方法、もしくは接着剤層を介して積層する方法、複数のガラスの間に複数のグリーンフィルムを形成した後、加熱によりイミド化反応を行う方法、これらを組み合わせた方法、などの方法で、ガラス/樹脂積層体を製造することができる。
<支持板>
支持板32は、後述する剥離性樹脂層34を介してガラス/樹脂積層体10を支持し、ガラス/樹脂積層体10の強度を補強するためのものであれば、特に限定されない。
剥離性樹脂層34は、上述した支持板32上に固定され、ガラス/樹脂積層体10を積層する。なお、剥離性樹脂層34の剥離性表面は、ガラス/樹脂積層体10の他方の最外層の最外面と密着するが、ガラス/樹脂積層体10を容易に剥離することができる表面特性を有する。すなわち、剥離性樹脂層34の剥離性表面は、ガラス/樹脂積層体10の他方の最外層の最外面に対してある程度の結合力で結合して、ガラス/樹脂積層体10の位置ずれなどを防止していると同時に、ガラス基板積層体30からガラス/樹脂積層体10を剥離する際には、ガラス/樹脂積層体10を破壊することなく、容易に剥離できる程度の結合力で結合している。本発明では、この樹脂層表面の容易に剥離できる性質を剥離性という。
<電子デバイスの製造方法>
電子デバイスの製造方法は特に限定されないが、例えば図5に示すように、ガラス基板積層体30のガラス基板12の表面上に、電子デバイスの構成部材の少なくとも一部を形成する構成部材形成工程(ステップS20)と、構成部材形成工程(ステップS20)後に、ガラス/樹脂積層体10と剥離性樹脂層34とを分離する分離工程(ステップS22)とを備える方法で製造することが好ましい。
1.ポリアミド酸の還元粘度(ηsp/C)
ポリマー濃度が0.2g/dlとなるようにN-メチル-2-ピロリドンに溶解した溶液をウベローデ型の粘度管により30℃で測定した。
2.ガラス基板12及び樹脂層14であるポリイミドフィルムの厚さ
マイクロメータ(ミツトヨ社製、MDC25J)を用いて測定した。
3.ガラス基板12及び樹脂層14であるポリイミドフィルムの平均線膨張係数
下記条件で伸縮率を測定し、平均線膨張係数を求めた。
試料長さ ; 20mm
試料幅 ; 2mm
昇温開始温度 ; 20℃
昇温終了温度 ; 310℃
昇温速度 ; 5℃/分
雰囲気 ; アルゴン
4.試験片の反り
試験片(50mm×300mm)を定盤上に載置し、定盤と試験片の長手方向中央部及び長手方向両端部との間のそれぞれの隙間の最大値を隙間ゲージにより測定した。
5.試験片の最小曲げ半径
試験片(50mm×200mm)を23℃、50%RHの環境下で48時間放置した後にステンレス鋼製の円柱体に巻き付けて屈曲させ、外観を観察して破損がないときの最小曲げ半径を測定した。
6.試験片の水蒸気透過量
水蒸気透過率測定装置(DKSH社製、Model7001)を用い、38℃、90%RHの環境下で、ASTM E-96-63Tに準拠した方法で測定した。
実施例1では、試験片として、図1に示すガラス/樹脂積層体10を製造した。
ガラス基板12は、フロート法により得られた幅500mm×厚さ70μmの無アルカリガラス基板(旭硝子社製、AN100)を用いた。このガラス基板12の平均線膨張係数は、38×10-7/℃であった。
ロール状に巻き取られたガラス基板12を巻き出しながら、ガラス基板12の両面に積層された保護フィルムを剥離し、ガラス基板12の樹脂層14に接触する側の面12aにシランカップリング処理を施した。具体的には、ガラス基板12の樹脂層14に接触する側の面12aに、3-グリシドキシプロピルトリメトキシシラン(信越シリコーン社製、KBM-403)1質量%のエタノール溶液をスプレーし、次いで温風乾燥を行った。
窒素導入管、温度計、攪拌棒を備えた反応容器内を窒素置換した後、500質量部の5-アミノ-2-(p-アミノフェニル)ベンゾオキサゾールを入れた。次いで、8000質量部のN,N-ジメチルアセトアミドを加えて完全に溶解させてから、485質量部のピロメリット酸二無水物を加えて、25℃にて48時間攪拌すると、褐色で粘調なポリアミド酸溶液が得られた。得られた溶液の還元粘度(ηsp/C)は4.0dl/gであった。
このポリアミド酸溶液を、ポリエチレンテレフタレートフィルム(東洋紡績社製、A-4100)の無滑剤面上にコンマコーターを用いて塗布し、110℃にて5分間乾燥してポリアミド酸フィルム(グリーンフィルム)を得た。
このポリアミド酸フィルムを、ピンテンタで保持して、連続式の熱処理炉に通し、150℃にて2分間熱処理し、次いで220℃にて2分間熱処理し、次いで475℃にて4分間熱処理した後、冷却し切断して幅500mm×厚さ30μmの耐熱性ポリイミドフィルムを得た。得られた耐熱性ポリイミドフィルムは、平均線膨張係数が30×10-7/℃であり、ガラス基板12との平均線膨張係数との差が8×10-7/℃であった。また、5%加熱重量減温度は、550℃であった。
この耐熱性ポリイミドフィルムをロール状に巻き取った後、巻き出しながら、耐熱性ポリイミドフィルムのガラス基板12に接触する側の面に、常圧リモートプラズマ装置(積水化学社製)を用いてプラズマを照射した。ここで処理条件は、出力3kw、窒素/空気流量比=600slm/750sccm、搬送速度1m/min.とした。
上記シランカップリング処理後のガラス基板12、及び上記プラズマ処理後の耐熱性ポリイミドフィルムを、表面温度315℃の金属ローラ(直径200mm)の間に5m/分の速度で通し、図1に示すガラス/樹脂積層体10を得た。
実施例2では、試験片として、図2に示すガラス/樹脂積層体20を製造した。
ガラス基板12は、フロート法により得られた縦500mm×横500mm×厚さ45μmの無アルカリガラス基板(旭硝子社製、AN100)を用いた。このガラス基板12の平均線膨張係数は、38×10-7/℃であった。
樹脂層14は、実施例1と同様にして作製した縦500mm×横500mm×厚さ30μmの耐熱性ポリイミドフィルムを用いた。この耐熱性ポリイミドフィルムは、平均線膨張係数が30×10-7/℃であり、ガラス基板12との平均線膨張係数との差が8×10-7/℃であった。
窒素導入管、温度計、攪拌棒を備えた反応容器内を窒素置換した後、368.4質量部の4,4'-ビス(3-アミノフェノキシ)ビフェニル、59.24質量部の無水フタル酸、174.5質量部の無水ピロメリット酸、及び172質量部のm-クレゾール2を入れ、200℃にて6時間撹拌した。この撹拌溶液にトルエンを加えた後、析出物を濾別し、さらにトルエンによる洗浄を3回行った後、窒素雰囲気下250℃にて6時間乾燥して、510質量部(収率90.1%)のポリイミド粉を得た。
ガラス基板12と、耐熱ポリイミドフィルムとの間に熱可塑性ポリイミドフィルムをセットし、加熱プレス装置により300℃、1MPaにて5分間加圧し、図2に示すガラス/樹脂積層体20を得た。
比較例1では、樹脂層14として厚さ30μmのポリイミドフィルム(東レ・デュポン社製、カプトンH)を用いた以外は、実施例2と同様にして、ガラス/樹脂積層体を得た。上記ポリイミドフィルム(カプトンH)は、ピロメリット酸無水物とジアミノジフェニルエーテルとを縮重合してなるものであり、平均線膨張係数が270×10-7/℃であり、ガラス基板12との平均線膨張係数の差が232×10-7/℃であった。
比較例2では、試験片として、上記ポリイミドフィルム(カプトンH)を用いた。
比較例3では、試験片として、厚さ100μmの無アルカリガラスフィルム(旭硝子社製、AN100)を用いた。
実施例3では、試験片として、図1に示すガラス/樹脂積層体10を実施例1とは別の方法で製造した。
ガラス基板12は、フロート法により得られた幅500mm×厚さ70μmの無アルカリガラス基板(旭硝子社製、AN100)を用いた。このガラス基板12の平均線膨張係数は、38×10-7/℃であった。
ロール状に巻き取られたガラス基板12を巻き出しながら、ガラス基板12の両面に積層された保護フィルムを剥離し、ガラス基板12の樹脂層14に接触する側の面12aにシランカップリング処理を施した。具体的には、ガラス基板12の樹脂層14に接触する側の面12aに、3-グリシドキシプロピルトリメトキシシラン(信越シリコーン社製、KBM-403)1質量%のエタノール溶液をスプレーし、次いで温風乾燥を行った。
窒素導入管、温度計、攪拌棒を備えた反応容器内を窒素置換した後、500質量部の5-アミノ-2-(p-アミノフェニル)ベンゾオキサゾールを入れた。次いで、8000質量部のN,N-ジメチルアセトアミドを加えて完全に溶解させてから、485質量部のピロメリット酸二無水物を加えて、25℃にて48時間攪拌すると、褐色で粘調なポリアミド酸溶液が得られた。得られた溶液の還元粘度(ηsp/C)は4.0dl/gであった。
このポリアミド酸溶液を、上記シランカップリング処理後のガラス基板12上にコンマコーターを用いて塗布し、連続式の熱処理炉に通し、110℃にて2分間熱処理し、150℃にて2分間熱処理し、次いで220℃にて2分間熱処理し、次いで475℃にて4分間熱処理し、図1に示すガラス/樹脂積層体10を得た。
初めに縦500mm、横500mm、板厚0.6mm、線膨張係数38×10-7/℃の支持ガラス板(旭硝子株式会社製、AN100)を純水洗浄、UV洗浄して表面を清浄化し、支持板として用意した。
本例では、実施例4で得たガラス基板積層体Aを用いてOLEDを製造する。
本出願は、2009年9月8日出願の日本国特許出願2009-207411に基づくものであり、その内容はここに参照として取り込まれる。
12 ガラス基板
14 樹脂層
22 接着剤層
30 ガラス基板積層体
32 支持板
34 剥離性樹脂層
Claims (18)
- ガラス基板と樹脂層とを有するガラス/樹脂積層体において、
前記樹脂層は、ベンゾオキサゾール構造を有する芳香族ジアミン類と、芳香族テトラカルボン酸無水物類とを縮重合させてなるポリイミドを含み、
前記ガラス基板と前記樹脂層との、25~300℃における平均線膨張係数の差が-100×10-7~+100×10-7/℃であり、
積層体の少なくとも一方の最外層が前記ガラス基板であるガラス/樹脂積層体。 - 前記ガラス基板と前記樹脂層とが直接接触している請求項1記載のガラス/樹脂積層体。
- 前記ガラス基板及び前記樹脂層の互いに接触する側の面のうち少なくともいずれか一方の面が、表面処理されたものである請求項2記載のガラス/樹脂積層体。
- 前記表面処理が、少なくともコロナ処理、プラズマ処理、フレーム処理、及びシランカップリング処理のいずれか1種を含む請求項3記載のガラス/樹脂積層体。
- 前記ガラス基板と前記樹脂層とが接着剤層を介して積層されている請求項1記載のガラス/樹脂積層体。
- 前記接着剤層が、熱可塑性ポリイミド、及び熱可塑性ポリアミドイミドから選ばれた一種以上の材料で形成される請求項5記載のガラス/樹脂積層体。
- 前記ガラス基板は矩形状又は帯状であり、
前記ガラス基板の幅方向寸法が2000mm以下である請求項1~6いずれか一項記載のガラス/樹脂積層体。 - 前記ガラス基板の厚さが0.3mm以下である請求項1~7いずれか一項記載のガラス/樹脂積層体。
- 前記樹脂層の厚さが0.1mm以下である請求項1~8いずれか一項記載のガラス/樹脂積層体。
- 請求項1~9いずれか一項記載のガラス/樹脂積層体を備える電子デバイス。
- 請求項1~9のいずれか一項記載のガラス/樹脂積層体、支持板、ならびに剥離性表面を有する剥離性樹脂層、を有し、
前記ガラス/樹脂積層体の他方の最外層の最外面と、前記支持板の表面に固定された前記剥離性樹脂層の剥離性表面とが密着するように、前記ガラス/樹脂積層体と前記支持板とが前記剥離性樹脂層を介して積層された、ガラス基板積層体。 - 前記剥離性樹脂層が、少なくともアクリル樹脂、ポリオレフィン樹脂、ポリウレタン樹脂、及びシリコーン樹脂のいずれか一種を含む請求項11記載のガラス基板積層体。
- 前記ガラス/樹脂積層体の厚さが50~400μmである請求項11又は12記載のガラス基板積層体。
- 前記支持板の材料が、5%加熱重量減温度が300℃以上の材料を含む請求項11~13のいずれか一項記載のガラス基板積層体。
- 前記支持板は、厚さが0.3mm以上であり、ガラス板、シリコンウエハ、プラスチック板、又は金属板からなる請求項11~14のいずれか一項記載のガラス基板積層体。
- 請求項11~15のいずれか一項記載のガラス基板積層体の製造方法であって、
前記支持板上に前記剥離性樹脂層を形成し固定する剥離性樹脂層形成工程と、
前記ガラス/樹脂積層体の他方の最外層の最外面と、前記剥離性樹脂層の剥離性表面とを密着する密着工程とを備える、ガラス基板積層体の製造方法。 - 請求項11~15のいずれか一項記載のガラス基板積層体の前記ガラス基板表面上に、電子デバイスの構成部材の少なくとも一部を形成してなる、電子デバイス製造用のガラス基板積層体。
- 請求項11~15のいずれか一項記載のガラス基板積層体の前記ガラス基板表面上に、電子デバイスの構成部材の少なくとも一部を形成し、その後、前記ガラス/樹脂積層体と前記剥離性樹脂層とを分離する、ガラス/樹脂積層体を有する電子デバイスの製造方法。
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CN102481764A (zh) | 2012-05-30 |
CN102481764B (zh) | 2014-11-05 |
KR20120064676A (ko) | 2012-06-19 |
TW201127620A (en) | 2011-08-16 |
US8609229B2 (en) | 2013-12-17 |
JPWO2011030716A1 (ja) | 2013-02-07 |
TWI476100B (zh) | 2015-03-11 |
US20120171454A1 (en) | 2012-07-05 |
KR101723254B1 (ko) | 2017-04-04 |
JP5723776B2 (ja) | 2015-05-27 |
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