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WO2011065336A1 - Procédé de production d'un corps stratifié - Google Patents

Procédé de production d'un corps stratifié Download PDF

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Publication number
WO2011065336A1
WO2011065336A1 PCT/JP2010/070835 JP2010070835W WO2011065336A1 WO 2011065336 A1 WO2011065336 A1 WO 2011065336A1 JP 2010070835 W JP2010070835 W JP 2010070835W WO 2011065336 A1 WO2011065336 A1 WO 2011065336A1
Authority
WO
WIPO (PCT)
Prior art keywords
resin composition
curable resin
substrate
bubbles
precursor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2010/070835
Other languages
English (en)
Japanese (ja)
Inventor
泰則 伊藤
裕 野尻
建郎 馬場
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AGC Inc
Original Assignee
Asahi Glass Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Priority to JP2011543248A priority Critical patent/JPWO2011065336A1/ja
Priority to CN2010800539074A priority patent/CN102639327A/zh
Publication of WO2011065336A1 publication Critical patent/WO2011065336A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/0007—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality
    • B32B37/003—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality to avoid air inclusion
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • 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
    • B32B17/10005—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 laminated safety glass or glazing
    • B32B17/10009—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 laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
    • B32B17/10036—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 laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
    • 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
    • B32B17/10005—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 laminated safety glass or glazing
    • B32B17/1055—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 laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10706—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 laminated safety glass or glazing characterized by the resin layer, i.e. interlayer being photo-polymerized
    • 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
    • B32B17/10005—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 laminated safety glass or glazing
    • B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
    • B32B17/10899—Making laminated safety glass or glazing; Apparatus therefor by introducing interlayers of synthetic resin
    • B32B17/10908—Making laminated safety glass or glazing; Apparatus therefor by introducing interlayers of synthetic resin in liquid form
    • B32B17/10917—Making laminated safety glass or glazing; Apparatus therefor by introducing interlayers of synthetic resin in liquid form between two pre-positioned glass layers
    • 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
    • B32B17/10005—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 laminated safety glass or glazing
    • B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
    • B32B17/10972—Degassing during the lamination
    • 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06—Joining glass to glass by processes other than fusing
    • C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B2037/1253—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives curable adhesive
    • 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
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/12—Pressure
    • 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
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/60—In a particular environment
    • B32B2309/68—Vacuum
    • 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
    • B32B2457/00—Electrical equipment
    • B32B2457/12—Photovoltaic modules
    • 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

Definitions

  • the present invention relates to a method for producing a laminate having a pair of substrates and a cured product layer of a curable resin composition existing between the pair of substrates.
  • the laminate produced by the method of the present invention includes laminated glass, a front panel plate of an image display device, more specifically, a liquid crystal display device (LCD), an EL (electroluminescence) display device such as an organic EL or an inorganic EL, It is suitable for uses such as a front panel plate of a flat panel display (FPD) such as a plasma display device and an electronic ink type image display device, a thin-layer solar cell device, a protective plate for a touch panel, and the like.
  • FPD flat panel display
  • Laminated glass that integrates a pair of glass substrates through an adhesive layer is used as a windshield for automobiles because broken glass fragments adhere to the film and do not scatter, and it is difficult to penetrate and has excellent strength. It is used as building window glass (safety glass, security glass) (see Patent Documents 1 and 2). From the viewpoint of preventing damage to the liquid crystal panel and preventing light reflection, a liquid crystal display device in which a front panel in which a transparent intermediate film is sealed between a transparent protective plate and a polarizing plate is provided on the front surface of the liquid crystal panel is known. (See Patent Document 3).
  • a solar cell module having a solar cell device sealed with a sealing material such as a resin between a transparent front surface material and a back surface material serving as a light receiving surface is known (see Patent Document 4).
  • a sealing material such as a resin between a transparent front surface material and a back surface material serving as a light receiving surface.
  • Patent Documents 1 and 2 are not limited to the type of substrate used, and are sandwiched between the substrates to form an intermediate layer.
  • the degree of freedom of the type of the curable resin composition is large, resources for forming the intermediate layer can be effectively used, the productivity is excellent, and the environmental load is small.
  • a seal portion for containing the curable resin composition is formed in the peripheral portion on one substrate, and then the curable resin composition is supplied to a region surrounded by the seal portion on the substrate.
  • the other substrate is overlaid on one substrate in a reduced-pressure atmosphere, whereby the curable resin composition is sandwiched and sealed between the pair of substrates.
  • the pair of substrates sandwiched and sealed with the curable resin composition is placed under a pressure atmosphere (for example, atmospheric pressure) higher than the above-described reduced-pressure atmosphere.
  • a pressure atmosphere for example, atmospheric pressure
  • the pair of transparent substrates are pressed in the direction in which they are in close contact with each other, and the volume of bubbles remaining in the sealed space is reduced according to the pressure difference of the atmosphere.
  • the curable resin composition flows into the decompressed space in the sealed space sealed by the seal portion, and the entire sealed space is uniformly filled with the curable resin composition. Then, a laminated body is obtained by hardening a curable resin composition.
  • the manufacturing method of the laminated body described in Patent Documents 1 and 2 is such that the curable resin composition is sandwiched between a pair of transparent substrates in a reduced-pressure atmosphere and sealed, and then the reduced-pressure atmosphere described above is used.
  • the sealed space uniformly filled with the curable resin composition By placing it under a high atmospheric pressure (for example, under atmospheric pressure), the laminate is obtained by curing the curable resin composition. Is.
  • bubbles exist in the curable resin composition at the time of curing the curable resin composition bubbles remain in the resin layer obtained by curing the curable resin composition. If bubbles having a size larger than the reference value depending on the use of the laminate remain in the resin layer, it becomes a bubble defect of the laminate, which is a problem.
  • produce often depend on the delicate manufacturing conditions of a laminated body. Further, when the resin is applied in a certain thickness, it is difficult to eliminate all the bubbles at the time of application so that there are no nonstandard bubbles due to the viscosity and the like.
  • the present invention aims to provide a novel method capable of producing a laminate having no bubble defect in order to solve the above-described problems of the prior art.
  • the present invention provides: Prepare two substrates, at least one of which is a transparent substrate, Forming a seal part for containing the curable resin composition in the peripheral part on the one substrate; Supplying a curable resin composition to a region surrounded by the seal portion on the one substrate; The curable resin composition is sandwiched and sealed between a pair of substrates formed by superimposing the other substrate on at least one of the curable resin composition and the seal portion in a reduced-pressure atmosphere.
  • the laminated precursor After obtaining the laminated precursor Placing the lamination precursor in a second pressure atmosphere having a higher atmospheric pressure than the reduced-pressure atmosphere; Observe the diameter and shape of the bubbles present in the curable resin composition layer, Provided is a method for producing a laminate, wherein the laminate precursor is allowed to stand for a predetermined time based on a result obtained by observing the diameter and shape of the bubbles, and then the curable resin composition is cured. To do.
  • the present invention provides two substrates, at least one of which is a transparent substrate, Forming a seal part for containing the curable resin composition for resin layer formation in the peripheral part on the one substrate; Supplying a resin layer forming curable resin composition to a region surrounded by the seal part on the one substrate; Between the pair of substrates formed by superposing the other substrate on at least one of the curable resin composition layer for resin layer formation and the seal portion under a reduced pressure atmosphere, After sandwiching and sealing the resin composition to obtain a lamination precursor, the lamination precursor is subjected to the curable resin composition for forming a resin layer in a second pressure atmosphere having an atmospheric pressure higher than that of the reduced pressure atmosphere.
  • a method for producing a laminate by performing a curing treatment to cure Before performing the curing treatment on the lamination precursor, it is set in advance according to the diameter and shape of the bubbles present in the resin layer forming curable resin composition layer and the viscosity of the curable resin composition.
  • the present invention provides a method for producing a laminate, wherein the laminate precursor is allowed to stand for an estimated bubble disappearance time.
  • the bubble disappearance prediction time is predicted for the air bubbles having the largest equivalent circle diameter among the floating bubbles present in the curable resin composition layer for resin layer formation of the laminate precursor in advance. However, it is preferable to leave the bubble disappearance prediction time set based on the prediction result.
  • the laminated precursor is allowed to stand for a preset bubble disappearance prediction time in the second pressure atmosphere.
  • the method for producing a laminate of the present invention after placing the lamination precursor in the second pressure atmosphere, after leaving the lamination precursor for a predetermined time according to the viscosity of the curable resin composition, It is preferable to perform a step of observing the diameter and shape of the bubbles.
  • the curable resin composition when the curable resin composition is cured, the curable resin composition does not contain bubbles having a size larger than a reference value according to the use of the laminate. Therefore, it is possible to produce a high-quality laminate without bubble defects.
  • FIG. 1 is a plan view of a substrate, showing a state where a seal portion is formed in the peripheral portion on the substrate.
  • FIG. 2 is a diagram for schematically explaining the shape of bubbles present in the curable resin composition layer of the laminated precursor.
  • FIG. 3 is a graph showing the relationship between the equivalent circle diameter of floating bubbles in the curable resin composition layer and the elapsed time until the floating bubbles disappear.
  • 4 (a) to 4 (d) are diagrams for schematically explaining the change in the shape of floating bubbles in the curable resin composition layer.
  • FIG. 1 is a plan view of the substrate, and shows a state in which a seal portion 20 is formed in the peripheral portion on the substrate 10.
  • the diameter and shape of the bubbles present in the curable resin composition layer for resin layer formation are determined.
  • at least one of the pair of substrates needs to be a transparent substrate.
  • only one of the pair of substrates may be a transparent substrate and the other may be an opaque substrate, or both substrates may be transparent substrates.
  • a seal portion may be formed around the transparent substrate, or a seal portion may be formed around the opaque substrate.
  • the transparent substrate is not particularly limited as long as it is a substrate having such a transparency that the diameter and shape of the bubbles present in the curable resin composition layer for resin layer formation can be observed from the substrate surface.
  • Specific examples of the transparent substrate include a glass substrate and a transparent resin substrate.
  • a glass substrate is preferable because it has transparency, light resistance, low birefringence, high planar accuracy, surface scratch resistance, and high mechanical strength.
  • Examples of the material for the glass substrate include soda lime glass, highly transmissive glass (white plate) having lower iron content and less bluishness, and borosilicate glass.
  • Examples of the material for the transparent resin substrate include highly transparent resin materials (polycarbonate, polymethyl methacrylate, etc.).
  • a transparent substrate on which a plurality of transparent substrates are bonded or a transparent substrate on which an optical film or the like is bonded can also be used as an integrated transparent substrate.
  • a structure including a transparent substrate as a part of the constituent elements can also be used as the transparent substrate.
  • Specific examples of the structure including such a transparent substrate as a component include a liquid crystal display (LCD), an EL (electroluminescence) display device such as an organic EL or an inorganic EL, a plasma display device, and an electronic ink image.
  • LCD liquid crystal display
  • EL electroluminescence
  • plasma display device such as an organic EL or an inorganic EL
  • FPD flat panel displays
  • the opaque substrate When one of the pair of substrates is an opaque substrate, specific examples of the opaque substrate include a substrate made of a metal material such as stainless steel, a substrate made of a ceramic material, and a filler that absorbs visible light in the substrate. Examples thereof include a resin substrate that is shielded from light by being dispersed.
  • both the pair of substrates are transparent substrates
  • the pair of transparent substrates may be formed of the same material or different materials. That is, both of the pair of transparent substrates may be a glass substrate or a transparent resin substrate, and one of the pair of transparent substrates may be a glass substrate and the other may be a transparent resin substrate.
  • the thickness of the substrate is not particularly limited, but in the case of a transparent substrate, from the viewpoint of mechanical strength and transparency, it is usually 1 to 6 mm for a glass substrate, and usually 0.1 to 3 mm for a transparent resin substrate. It is. On the other hand, in the case of an opaque substrate, the thickness is usually 0.8 to 4 mm from the viewpoint of mechanical strength and reduction in thickness and weight. Note that the thickness of the pair of substrates may be the same or different.
  • the surface of the substrate more specifically, the surface on the side where the seal portion is formed in the peripheral portion may be subjected to surface treatment in order to improve the interfacial adhesive force with the seal portion.
  • the surface treatment may be performed only on the peripheral portion of the substrate, or may be performed on the entire surface of the substrate.
  • Examples of the surface treatment method include a method of treating the surface of the substrate with a silane coupling agent.
  • the seal portion dams up the curable resin composition for forming a resin layer supplied to the region surrounded by the seal portion on the substrate, and then is sandwiched and sealed between the pair of substrates in a reduced-pressure atmosphere. Since it is provided for the purpose of containing the curable resin composition for forming a resin layer, the curable resin composition supplied to the region surrounded by the seal portion in the production process of the laminate of the present invention is more than the extent that does not leak. It is required to have such an interfacial adhesive strength and to have a hardness that can maintain the shape in the production process of the laminate of the present invention.
  • a seal portion that satisfies such requirements can be formed by providing a seal member having an adhesive or a pressure-sensitive adhesive on the surface of one substrate.
  • a sealing member having an adhesive or a pressure-sensitive adhesive on the surface of one substrate.
  • Specific examples of such a sealing member include the following. -A tape-like or rod-like long body (double-sided adhesive tape, etc.) with a pressure-sensitive adhesive layer or adhesive layer provided on the surface in advance. -An adhesive layer or a pressure-sensitive adhesive layer is formed on the peripheral edge of the surface of one substrate, and a long body is pasted on this.
  • a dam-like seal precursor was formed on the peripheral edge of the surface of one substrate by printing or dispensing using the curable resin composition for forming a seal part, and the curable resin composition for forming a seal part was cured. Thereafter, an adhesive layer or a pressure-sensitive adhesive layer is formed on the surface.
  • the seal portion that satisfies the above requirements uses a dispenser as the second curable resin composition so that the high-viscosity curable resin composition has a predetermined thickness on the periphery of one substrate. It can also be formed by coating.
  • the curable resin composition used for forming the seal portion is also referred to as a second curable resin composition.
  • the curable resin composition for forming a resin layer corresponds to the first curable resin composition.
  • the second curable resin composition may be cured at the same time as the cured curable resin composition sandwiched between the pair of substrates and cured in the procedure to be described later. The resin composition may be cured before curing.
  • the “seal part” herein includes a seal precursor before curing in which a curable resin composition is formed in a dam shape on the peripheral part of the surface of one of the substrates for forming the seal part.
  • the viscosity of the second curable resin composition is preferably 200 to 3000 Pa ⁇ s, and more preferably 500 to 2000 Pa ⁇ s.
  • the seal portion can be deformed according to the thickness of the layer of the curable resin composition present in the substrate.
  • the seal portion can have a strength that can withstand atmospheric pressure, and can be applied industrially at high speed using a dispenser or the like. From the above, the above viscosity range is preferable.
  • spacer particles having a predetermined particle diameter may be blended in the second curable resin composition.
  • the seal portion is cured to be supplied to the region surrounded by the seal portion in order to prevent leakage of the curable resin composition for forming a resin layer supplied to the region surrounded by the seal portion on the substrate. It is preferable to form the layer slightly thicker than the predetermined thickness of the layer formed by the curable resin composition (hereinafter, sometimes simply referred to as “curable resin composition layer” in the present specification).
  • the thickness of the seal portion is preferably 1.1 to 2 times the predetermined thickness of the curable resin composition layer.
  • the width of the seal portion varies depending on the thickness of the curable resin composition layer, but is preferably 0.5 to 5 mm, particularly preferably 0.8 to 3 mm.
  • the second curable resin composition used for forming the seal part is surrounded by the seal part because it has a high viscosity.
  • its shape does not change with time after application. Therefore, when the formed seal part is partially broken or thinned so that the width of the seal part is partially narrowed, these drawbacks are not eliminated over time. For this reason, when a partial defect or thinning occurs in the formed seal portion, the seal portion is supplied to the region surrounded by the seal portion before or after performing vacuum lamination in the procedure described later.
  • the seal portion when forming the seal portion, if the curable resin composition overlaps at the start and end points of the application, it will not be eliminated over time, so when performing vacuum lamination in the procedure described later When the thickness of the seal portion is partially non-uniform, large bubbles may be generated in the curable resin composition existing in the space sealed by the pair of substrates and the seal portion. Moreover, there exists a possibility that the designability of the laminated body manufactured may be impaired by the width
  • a partial defect may be caused so that the above-described problems do not occur. It is preferable to inspect for defects such as thinning and overlapping. However, depending on the size of the defect, the above-described problem may not occur. Therefore, it is preferable to inspect for the presence or absence of a defect exceeding a predetermined allowable range.
  • the following standards can be considered as acceptable defect standards. However, the acceptable defect criterion is not limited to this, and can be appropriately selected as necessary.
  • the inspection method for defects is not particularly limited. Specific examples include a method of visually inspecting the presence or absence of defects in the curable resin composition after coating, and a method of confirming by image processing the presence or absence of defects in the curable resin composition after coating.
  • the curable resin composition When no defect exceeding the reference value is found in the defect inspection, the curable resin composition is supplied to the region surrounded by the seal portion on the substrate according to the procedure described later. On the other hand, if a defect exceeding the reference value is found in the defect inspection, a curable resin composition is applied to the area where the defect exists and the defect is repaired. A curable resin composition may be supplied to the region. In this case, after repairing the defect, the defect inspection may be performed again. Further, when the repair of the defect does not meet the cost, the defect that exceeds the reference value in the defect inspection may be discarded without being repaired. In addition, also when forming a seal part by methods other than application
  • the curable resin composition is supplied to a region surrounded by the seal portion on the substrate.
  • the supply amount of the curable resin composition is such that when the curable resin composition is sandwiched and sealed between the pair of substrates in the procedure described later, the space sealed by the pair of substrates and the seal portion is the curable resin composition.
  • the supply amount of the curable resin composition can be determined in consideration of the volume reduction due to the curing shrinkage of the curable resin composition in advance.
  • the thickness of the resin composition layer is preferably 30 to 3000 ⁇ m.
  • the curable resin composition layer requires not only a function as an adhesive between a pair of substrates, but also a thickness to provide the layer with a function of imparting mechanical strength. This is because it is not preferable to unnecessarily increase the thickness because a thin and light weight is required as represented by an opening member and a display member.
  • the thickness of the curable resin composition layer existing in the space sealed by the pair of substrates and the seal portion is 30. It is more preferably from 800 to 800 ⁇ m, further preferably from 100 to 400 ⁇ m. In some cases, it may be preferable that the thickness of the curable resin composition is thin. In this case, 30 to 400 ⁇ m is preferable, 100 to 200 ⁇ m is more preferable, and 100 to 160 ⁇ m is more preferable.
  • Examples of the method for supplying the curable resin composition include a method in which the substrate on which the seal portion is formed is placed flat by the above procedure, and is supplied dropwise by a supply means such as a dispenser in the form of dots or lines.
  • a conventional method of injecting a curable resin into the gap between the previously formed laminates for example, the method described in JP-A-57-165411, JP-A-2001-339088) is used.
  • a curable resin composition having a relatively high viscosity can be used.
  • decrease of the cure shrinkage at the time of hardening a curable resin composition, and the improvement of the mechanical strength of the resin layer after hardening can be aimed at.
  • the viscosity of the curable resin composition for forming a resin film to be used is 0.2 to 50 Pa ⁇ s, it is easy to handle industrially in the process of producing, transferring and applying a large amount of curable resin composition.
  • the viscosity of the curable resin composition for forming a resin film referred to here is a viscosity in a temperature region at the time of carrying out the manufacturing method of the laminate of the present invention, and in particular, cured in a region surrounded by a seal portion. It is the viscosity in a temperature range until it implements vacuum lamination according to the procedure mentioned later after supplying a conductive resin composition. For example, when these procedures are performed at room temperature, it is the viscosity of the curable resin composition at room temperature. Therefore, although it depends on the temperature at the time of carrying out these procedures, in any case, it is within a temperature range of 5 to 80 ° C.
  • the viscosity of the 2nd curable resin composition used for formation of the sealing part mentioned above is also the same.
  • the viscosity of the curable resin composition to be used is more preferably 1 to 20 Pa ⁇ s, particularly preferably 0.2 to 10 Pa ⁇ s.
  • a curable resin composition containing a high molecular weight curable compound (oligomer or the like) as described below can be used. Since the high molecular weight curable compound can reduce the number of chemical bonds in the curable resin composition, the curing shrinkage when curing the curable resin composition is reduced, and the mechanical properties of the resin layer after curing are reduced. Strength is improved. On the other hand, many high molecular weight curable compounds are highly viscous. Therefore, from the viewpoint of suppressing the remaining of bubbles while ensuring the mechanical strength of the cured resin layer, it is possible to adjust the viscosity by dissolving a curable monomer having a lower molecular weight in a high molecular weight curable compound.
  • the viscosity of the curable resin composition is lowered, but the curing shrinkage when the curable resin composition is cured is large, and the mechanical strength of the resin layer after curing is large. Is prone to decline.
  • the curable resin composition to be used is preferably a photocurable resin composition.
  • the photocurable resin composition is cured in a short time with less heat energy than the thermosetting resin composition. Therefore, the environmental load at the time of manufacturing a laminated body becomes small by using a photocurable resin composition in this invention. Moreover, since the photocurable resin composition can be substantially cured in several minutes to several tens of minutes, the production efficiency of the laminate is high.
  • a photocurable resin composition is a material that is cured by the action of light to form a resin layer.
  • a photocurable resin composition the following are mentioned, for example, It can use in the range which the hardness of the resin layer after hardening does not become high too much.
  • a composition comprising a compound having an addition polymerizable unsaturated group and a photopolymerization initiator.
  • a polyene compound having 1 to 6 unsaturated groups triallyl isocyanurate, etc.
  • a polythiol compound having 1 to 6 thiol groups triethylene glycol dimercaptan
  • a composition containing a photopolymerization initiator which is contained in a proportion in which the number of moles is substantially equal.
  • a composition comprising an epoxy compound having two or more epoxy groups and a photocation generator.
  • the photocurable resin composition has one or more groups selected from the group consisting of an acryloyloxy group and a methacryloyloxy group (hereinafter referred to as “(meta)” because the curing rate is high and the cured resin layer has high transparency. It is more preferable that it contains at least one compound having a acryloyloxy group and a photopolymerization initiator.
  • a compound having a (meth) acryloyloxy group (hereinafter also referred to as a (meth) acrylate-based compound)
  • a compound having 1 to 6 (meth) acryloyloxy groups per molecule is preferable.
  • a compound having 1 to 3 (meth) acryloyloxy groups per molecule is particularly preferred because it is not too hard.
  • the (meth) acrylate-based compound an aliphatic or alicyclic compound that contains as few aromatic rings as possible is preferable from the viewpoint of light resistance of the cured resin layer.
  • the compound which has a hydroxyl group is more preferable from the point of the improvement of the interface adhesive force with a board
  • the content of the (meth) acrylate compound having a hydroxyl group is preferably 25% by mass or more, more preferably 40% by mass or more, of all (meth) acrylate compounds.
  • the compound having a hydroxyl group tends to have a high modulus of elasticity of the resin layer after curing.
  • the resin layer after curing becomes hard depending on the use of the laminate. There is a risk of passing.
  • the content of (meth) acrylate having a hydroxyl group is all (meta).
  • the resin layer has a good adhesion to any substrate on the substrate surface with different surface energy.
  • a resin layer exhibiting a low-elastic modulus adhesive state can be used so that it can be expressed.
  • the content of the (meth) acrylate having a hydroxyl group can be 60% by mass or more.
  • the (meth) acrylate compound may be a relatively low molecular compound (hereinafter referred to as an acrylate monomer), and a relatively high molecular weight compound having a repeating unit (hereinafter referred to as a (meth) acrylate oligomer). May be).
  • Examples of the (meth) acrylate compound include one or more (meth) acrylate monomers, one or more (meth) acrylate oligomers, one or more (meth) acrylate monomers (meth) )
  • One or more acrylate oligomers are mentioned, and one or more acrylate oligomers, or one or more acrylate oligomers and one or more (meth) acrylate monomers Is preferred.
  • a urethane oligomer having an average of 1.8 to 4 curable functional groups consisting of one or both of an acryloyloxy group and a methacryloyloxy group, and a hydroxyl group number of 1
  • a curable resin composition containing one or two hydroxyalkyl methacrylates having a hydroxyalkyl group having 3 to 8 carbon atoms is particularly preferable.
  • the cured resin is used so that shrinkage of the resin during the curing process does not adversely affect the display performance of the flat panel display (FPD).
  • the layer has a lower modulus. Therefore, an oligomer having an average of 1.8 to 4 curable functional groups composed of (meth) acryloyloxy groups, and a hydroxyalkyl group having 3 to 8 carbon atoms having 1 or 2 hydroxyl groups.
  • a curable resin composition containing a hydroxyalkyl methacrylate having at least one of a (meth) acrylate monomer having no hydroxyl group is preferred.
  • the total content of the (meth) acrylate monomer having no hydroxyl group is larger in mass ratio than the content of the (meth) acrylate monomer having a hydroxyl group.
  • a hydroxyalkyl (meth) acrylate hydroxyl group having a hydroxyalkyl group having 12 to 22 carbon atoms and having one hydroxyl group can be used instead of the (meth) acrylate monomer having no hydroxyl group.
  • the (meth) acrylate monomer a compound having a vapor pressure that is low enough to sufficiently suppress volatility is preferable considering that the curable resin composition is placed in a reduced pressure atmosphere in a reduced pressure apparatus.
  • the curable resin composition contains a (meth) acrylate monomer having no hydroxyl group, an alkyl (meth) acrylate having 8 to 22 carbon atoms, a polyether such as polyethylene glycol or polypropylene glycol having a relatively low molecular weight
  • a diol mono (meth) acrylate or di (meth) acrylate can be used, and an alkyl methacrylate having 8 to 22 carbon atoms is preferred.
  • the (meth) acrylate oligomer is a (meth) acrylate polymer having a molecular structure having a chain (polyurethane chain, polyester chain, polyether chain, polycarbonate chain, etc.) having two or more repeating units and a (meth) acryloyloxy group. Oligomers are preferred. Examples of the (meth) acrylate oligomer include a urethane bond (usually further including a polyester chain and a polyether chain) called a urethane acrylate oligomer and two or more (meth) acryloyloxy groups (meth). Examples include acrylate oligomers. The urethane acrylate oligomer is more preferable because the mechanical design of the cured resin layer and the adhesion to the substrate can be widely adjusted by the molecular design of the urethane chain.
  • the number average molecular weight of the (meth) acrylate oligomer is preferably from 1,000 to 100,000, more preferably from 10,000 to 70,000. When the number average molecular weight is less than 1000, the crosslink density of the cured resin layer becomes high and the flexibility of the resin layer may be impaired. If the number average molecular weight is greater than 100,000, the viscosity of the uncured curable resin composition may be too high. When the viscosity of the (meth) acrylate oligomer is too high, it is preferable to reduce the viscosity of the curable resin composition as a whole in combination with the (meth) acrylate monomer.
  • the second curable resin composition used for forming the seal portion when used as the second curable resin composition used for forming the seal portion, it has a curable group and has a number average because the viscosity is easily adjusted to the range of 200 to 3000 Pa ⁇ s. It includes one or more curable oligomers having a molecular weight of 30,000 to 100,000, and one or more (meth) acrylate monomers having a curable group, and the ratio of the monomers is the sum of the oligomer and the monomer ( 100% by mass) is preferably 15 to 50% by mass.
  • the (meth) acrylate oligomer is more preferably an acrylate oligomer that can increase the reactivity in curing.
  • Examples of the photopolymerization initiator include acetophenone-based, ketal-based, benzoin or benzoin ether-based, phosphine oxide-based, benzophenone-based, thioxanthone-based, and quinone-based photopolymerization initiators. Photoinitiators are preferred. When curing with visible light having a short wavelength, a phosphine oxide photopolymerization initiator is more preferable from the absorption wavelength region of the photopolymerization initiator. By using two or more kinds of photopolymerization initiators having different absorption wavelength ranges, the curing time can be further accelerated, or the surface curability can be enhanced in the second curable resin composition used for forming the seal portion. More preferred. Examples of the photo cation generator include onium salt compounds.
  • the curable resin composition may contain a polymerization inhibitor, a photocuring accelerator, a chain transfer agent, a light stabilizer (such as an ultraviolet absorber or a radical scavenger), an antioxidant, a flame retardant, and an adhesive as necessary.
  • a polymerization inhibitor such as an ultraviolet absorber or a radical scavenger
  • a light stabilizer such as an ultraviolet absorber or a radical scavenger
  • an antioxidant such as an ultraviolet absorber or a radical scavenger
  • a flame retardant such as an adhesive
  • Various additives such as an improver (such as a silane coupling agent), a pigment, and a dye may be included, and a polymerization inhibitor and a light stabilizer are preferably included.
  • an improver such as a silane coupling agent
  • a pigment such as a silane coupling agent
  • a dye such as a pigment
  • a dye such as a pigment, and a dye
  • the laminate it is not preferable to include an additive that may hinder the transmission of light in the cured resin layer.
  • the use of the laminate is a front panel plate of a flat panel display (FPD) or a thin-layer solar cell device
  • the former is a light emitted from a flat panel display (FPD) that forms a display image.
  • sunlight permeate transmits the resin layer after hardening, it is not preferable to contain the additive which may prevent transmission of those light rays.
  • the ultraviolet absorber absorbs the ultraviolet component of sunlight transmitted through the resin layer to reduce the amount of light incident on the thin-layer solar cell device, or adversely affects the color tone of the display image of the flat panel display (FPD).
  • FPD flat panel display
  • the resin layer through which sunlight passes is required to have light resistance, particularly durability against light having a short wavelength such as ultraviolet rays. Therefore, when an ultraviolet absorber or the like is included, it is preferable to appropriately adjust the absorption characteristics, blending amount, and the like.
  • the chain transfer agent which has a thiol group in a molecule
  • Polymerization inhibitors include hydroquinone (2,5-di-t-butylhydroquinone, etc.), catechol (pt-butylcatechol, etc.), anthraquinone, phenothiazine, hydroxytoluene and the like. Can be mentioned.
  • the light stabilizer include ultraviolet absorbers (benzotriazole series, benzophenone series, salicylate series, etc.), radical scavengers (hindered amine series), and the like.
  • Examples of the antioxidant include phosphorus-based and sulfur-based compounds.
  • a compound having a relatively large molecular weight and a low vapor pressure under reduced pressure is preferable because the curable resin composition is placed under a reduced pressure atmosphere.
  • the other substrate is overlaid on the curable resin composition supplied to the region surrounded by the seal portion on the substrate by the above procedure.
  • the surface on the side to which the curable resin composition is supplied in the above procedure is directed to the other substrate, and the pair of substrates and the other substrate What is necessary is just to overlap
  • substrates is obtained.
  • the procedure of superimposing the other substrate on the curable resin composition supplied to the region surrounded by the seal portion under a reduced pressure atmosphere may be simply referred to as “vacuum lamination”. is there.
  • vacuum lamination can be performed by the following procedure.
  • the substrate on the side where the seal portion and the layer of the curable resin composition are formed on the surface is referred to as one substrate, and the side on which the surface is not formed on the surface.
  • the substrate is referred to as the other substrate.
  • One substrate is put in a decompression device, and the substrate is placed flat on a fixed support plate in the decompression device so that the surface of the curable resin composition is on the top.
  • a movement support mechanism that can move in the vertical direction is provided in the upper part of the decompression device, and the other substrate is attached to the movement support mechanism.
  • the thin film solar cell device is formed on the surface of the other substrate, the surface on the side where the thin film solar cell device is formed is directed downward.
  • the use of the laminate is a flat panel display (FPD)
  • the surface on the image display side is directed downward.
  • the antireflection layer is provided on the surface of the other substrate, the surface on the side where the antireflection layer is not formed is directed downward.
  • the other substrate is placed above one substrate and in a position not in contact with the curable resin composition. That is, the curable resin composition on one substrate and the other substrate are opposed to each other without being brought into contact with each other.
  • a movable support mechanism that can move in the vertical direction may be provided in the lower part of the decompression device, and one substrate may be placed on the movable support mechanism.
  • the other substrate is attached to a fixed support plate provided at an upper portion in the decompression device, and the one substrate and the other substrate are opposed to each other.
  • you may support both one board
  • the inside of the decompression device is decompressed to obtain a predetermined decompressed atmosphere.
  • one substrate and the other substrate may be positioned at predetermined positions in the decompression apparatus during the decompression operation or after a predetermined decompression atmosphere.
  • the inside of the decompression device becomes a predetermined decompression atmosphere, the other substrate supported by the moving support mechanism is moved downward, and the other substrate is superimposed on the curable resin composition on the one substrate. .
  • the curable resin composition is sealed in the space surrounded by the surface of one substrate, the lower surface of the other substrate, and the seal portion.
  • the curable resin composition is spread by the weight of the other substrate, the pressure from the moving support mechanism, and the like, and the curable resin composition is filled in the above-described space.
  • the atmospheric pressure of the reduced-pressure atmosphere at the time of superposition is 1000 Pa or less, preferably 0.1 Pa or more. If the atmospheric pressure of the reduced-pressure atmosphere is too low, each component (curable compound, photopolymerization initiator, polymerization inhibitor, light stabilizer, etc.) contained in the curable resin composition may be adversely affected. For example, if the reduced-pressure atmosphere is too low, each component may be vaporized, and it may take time to provide the reduced-pressure atmosphere.
  • the atmospheric pressure in the reduced pressure atmosphere is more preferably 1 to 100 Pa. More preferably, it is 3 to 30 Pa.
  • the laminate precursor obtained by vacuum lamination is placed in a pressure atmosphere higher than the atmospheric pressure of the reduced-pressure atmosphere in which the vacuum lamination is performed.
  • the high pressure atmosphere described above is, for example, atmospheric pressure.
  • the pressure atmosphere higher than the reduced pressure atmosphere in which the vacuum lamination is performed is referred to as a second pressure atmosphere with respect to the reduced pressure atmosphere.
  • the reduced-pressure atmosphere corresponds to a first pressure atmosphere with respect to the second pressure atmosphere.
  • this procedure may be referred to as “releasing the reduced-pressure atmosphere”.
  • the pair of substrates As the atmospheric pressure is increased by releasing the reduced-pressure atmosphere, the pair of substrates is pressed in the direction in which the substrates are in close contact with each other, and the volume of bubbles remaining in the curable resin composition layer is reduced according to the pressure difference of the atmosphere. By doing so, the whole sealed space sealed by the pair of substrates and the seal portion is uniformly filled with the curable resin composition.
  • the second pressure atmosphere is preferably 50 kPa or more higher than the atmospheric pressure of the reduced pressure atmosphere in which the vacuum lamination is performed.
  • the pressure in the second pressure atmosphere is usually preferably 80 to 120 kPa.
  • the second pressure atmosphere may be an atmospheric pressure atmosphere or a higher pressure.
  • An atmospheric pressure atmosphere is most preferable because operations such as curing of the curable resin composition can be performed without requiring special equipment.
  • the chamber may be adjusted to a pressure of 80 to 120 kPa (for example, to be atmospheric pressure), and a treatment for curing the curable resin composition for forming a resin layer may be performed under this pressure atmosphere, or a vacuum may be applied. Transfer from the depressurized apparatus to another curing apparatus, adjust the pressure in the curing apparatus to 80 to 120 kPa, and cure the curable resin composition for resin layer formation in this pressure atmosphere You may perform the process to make.
  • a pressure of 80 to 120 kPa for example, to be atmospheric pressure
  • a treatment for curing the curable resin composition for forming a resin layer may be performed under this pressure atmosphere, or a vacuum may be applied.
  • Transfer from the depressurized apparatus to another curing apparatus adjust the pressure in the curing apparatus to 80 to 120 kPa, and cure the curable resin composition for resin layer formation in this pressure atmosphere You may perform the process to make.
  • the time from when the one substrate and the other substrate are overlapped to the time when the reduced pressure atmosphere is released is not particularly limited, and the reduced pressure atmosphere may be released immediately after sealing the curable resin composition.
  • the reduced pressure state may be maintained for a predetermined time.
  • the curable resin composition flows in the sealed space, the interval between one substrate and the other substrate becomes uniform, and the reduced pressure atmosphere is released by releasing the reduced pressure atmosphere. Even when placed in a second pressure atmosphere higher than the atmosphere, the sealed state is easily maintained.
  • the time for maintaining the reduced pressure state may be several hours or longer, but is preferably within 1 hour, more preferably within 10 minutes from the viewpoint of production efficiency.
  • the diameter and shape of the bubbles present in the curable resin composition layer of the laminated precursor after the release of the reduced-pressure atmosphere are observed.
  • the diameter and shape of the bubbles present in the curable resin composition layer are observed from the surface of the transparent substrate. be able to.
  • the increase in the atmospheric pressure due to the release of the reduced-pressure atmosphere causes the pair of substrates to be pressed in the direction in which they are in close contact with each other, and the volume of bubbles remaining in the curable resin composition layer is the differential pressure of the atmosphere. Accordingly, the entire sealed space sealed by the pair of substrates and the seal portion is uniformly filled with the curable resin composition.
  • the time required for the bubbles remaining in the curable resin composition layer to be reduced and disappeared according to the pressure difference of the atmosphere depends on the size and shape of the bubbles remaining in the curable resin composition layer Depending on the viscosity of the cured curable resin composition, air bubbles may remain in the curable resin composition layer of the laminated precursor after the release of the reduced-pressure atmosphere.
  • the foam of the laminated body When the laminated body is used for building window glass (safety glass, security glass) or thin-layer solar cell devices, if bubbles with an equivalent circle diameter of 500 ⁇ m or more exist in the cured resin layer, the foam of the laminated body It can be a drawback.
  • the diameter and shape of the bubbles present in the curable resin composition layer of the laminate precursor after the release of the reduced-pressure atmosphere are observed, and the laminate precursor is based on the obtained observation results.
  • the foam By allowing the foam to remain in a state where no bubbles larger than the reference value corresponding to the use of the laminate are present in the curable resin composition layer, and then curing the curable resin composition. A laminate without defects can be produced.
  • FIG. 2 is a diagram for schematically explaining the shape of bubbles present in the curable resin composition layer of the lamination precursor, and corresponds to a side view (cross-sectional view) of the lamination precursor.
  • bubbles 41, 42, 43, and 44 are present in the curable resin composition layer 30 sandwiched between the pair of substrates 10a and 10b.
  • the bubbles 41 are present in a floating state in the curable resin composition layer 30, and all of the periphery is surrounded by the curable resin composition that forms the layer 30.
  • the bubbles that exist in a floating state in the curable resin composition layer 30 and are surrounded by the curable resin composition that forms the layer 30 are hereinafter referred to as the present invention.
  • the bubbles 42, 43 and 44 are partly in contact with either or both of the substrates 10a and 10b.
  • the bubble 42 has an equivalent circle diameter larger than the thickness of the curable resin composition layer 30, and a part of the periphery thereof is in contact with the substrates 10 a and 10 b.
  • a part of the periphery of the bubble 43 is in contact with the substrate 10a.
  • a part of the periphery of the bubble 44 is in contact with the substrate 10b.
  • the bubbles that exist in a state in which a part of the periphery thereof is in contact with at least one of the pair of substrates constituting the laminated precursor are hereinafter referred to as “contact bubbles”.
  • the present inventors have (1) floating bubbles compared to contact bubbles. Disappears in a short time, and (2) in the case of floating bubbles, there is a relationship between the size, specifically, the diameter of the floating bubbles and the time required for the bubbles to disappear That is confirmed experimentally.
  • stacking precursor is set from the following viewpoints ((a), (b)) based on the knowledge of said (1), (2).
  • FIG. 2 although the shape at the time of seeing a lamination
  • the time required for contact bubbles remaining in the curable resin composition layer to disappear varies depending on the viscosity of the curable resin composition, but the viscosity of the curable resin composition is 0.2 to 50 Pa ⁇
  • the contact bubbles remaining in the curable resin composition layer disappear if the laminated precursor is left for 6 hours or longer. Therefore, the laminated precursor should be left for 6 hours or longer. That's fine.
  • the time required for the contact bubbles remaining in the curable resin composition layer to disappear depends on the position where the contact bubbles exist (for example, the contact bubbles exist near the center of the lamination precursor or the lamination precursor. It is preferable that the laminated precursor is allowed to stand for 12 hours or more because it varies somewhat depending on the size of the contact bubbles.
  • the diameter of the floating bubbles in the curable resin composition layer is the projection onto the surface of the transparent substrate.
  • the circle-equivalent diameter of the floating bubbles in the projected shape on the surface of the transparent substrate is simply referred to as “circle-equivalent diameter of the floating bubbles”.
  • FIG. 3 shows a curable resin composition layer having the same viscosity as that of the curable resin composition layer of the example, that is, a photocurable resin composition Y for forming a resin layer, which will be described later.
  • the equivalent circle diameter of the floating bubbles in the curable resin composition layer and the process until the floating bubbles disappear It is the graph which showed the relationship between time.
  • the inventors of the present application provide a circle-equivalent diameter of the floating bubbles in the curable resin composition layer and an elapsed time until the floating bubbles disappear.
  • the curable resin composition layer can be left if the laminated precursor is allowed to stand for at least the time corresponding to the longest time of the expected bubble disappearance time of each floating bubble. It is thought that all the air bubbles inside disappear.
  • the bubble disappearance prediction time of the largest equivalent circle diameter is the longest, so in the curable resin composition layer
  • the bubble disappearance prediction time of the bubble having the largest equivalent circle diameter among the floating bubbles present in the above is specified, and the layered precursor may be left at least for a time corresponding to the bubble disappearance prediction time.
  • the curable resin composition can be cured immediately according to the procedure described below without leaving the laminate precursor.
  • the use of the laminate is a front panel plate of a flat panel display (FPD)
  • the equivalent circle diameter of all floating bubbles present in the curable resin composition layer is less than 50 ⁇ m
  • the cured resin layer Even if air bubbles remain in the layered product, it does not become a foam defect of the laminate, so that the curable resin composition can be cured immediately according to the procedure described later without leaving the layered precursor.
  • FIGS. 4 (a) and 4 (b) show the release of the reduced-pressure atmosphere.
  • FIG. 4A is a plan view of the lamination precursor
  • FIG. 4B is a side view (cross-sectional view) of the lamination precursor.
  • FIGS. 4C and 4D are views showing the lamination precursor after a certain time has passed since the release of the reduced pressure atmosphere
  • FIG. 4C is a plan view of the lamination precursor.
  • FIG. 4D is a side view (cross-sectional view) of the laminated precursor.
  • the shape of the floating bubbles present in the curable resin composition layer is like the floating bubbles 44. In some cases, it may be a spherical shape, and in other cases, it may be elliptical like the floating bubbles 45 and 46. These elliptical floating bubbles 45 and 46 change in shape with time due to pressure from the surrounding curable resin composition, and when a certain amount of time elapses, FIGS. 4C and 4D show. As shown, the shape becomes a spherical shape, and the equivalent circle diameter of the floating bubbles, that is, the equivalent circle diameter of the floating bubbles in the projected shape on the transparent substrate surface changes.
  • the bubble disappearance prediction time is specified based on the equivalent circle diameter of the floating bubbles in the projected shape on the transparent substrate surface. Therefore, the change in the equivalent circle diameter due to the change in the shape of the floating bubbles is caused by the bubble disappearance prediction time specified based on the equivalent circle diameter of the floating bubbles and the floating bubbles present in the curable resin composition layer. There may be a discrepancy between the actual time taken to disappear. For example, in the case of the floating bubbles 45, the equivalent circle diameter immediately after the release of the reduced-pressure atmosphere is 200 ⁇ m, whereas the equivalent circle diameter after a certain amount of time is 300 ⁇ m.
  • the bubble disappearance prediction time is specified based on the equivalent circle diameter (200 ⁇ m) of the floating bubbles 45 immediately after the release of the reduced-pressure atmosphere, and the laminated precursor is left for a time corresponding to the bubble disappearance time. Then, since the leaving time of the lamination precursor is shorter than the estimated bubble time of floating bubbles having an equivalent circle diameter of 300 ⁇ m, the bubbles in the curable resin composition layer disappear when the standing of the lamination precursor is completed. In some cases, bubbles may remain in the curable resin composition layer.
  • the equivalent circle diameter immediately after the release of the reduced pressure atmosphere is 500 ⁇ m
  • the equivalent circle diameter after a certain amount of time is 300 ⁇ m.
  • the bubble disappearance prediction time is specified based on the equivalent circle diameter (500 ⁇ m) of the floating bubble 45 immediately after the release of the reduced pressure atmosphere, and the laminated precursor is left for a time corresponding to the bubble disappearance time. Then, since the leaving time of the lamination precursor is longer than the estimated bubble time of floating bubbles having an equivalent circle diameter of 300 ⁇ m, the bubbles in the curable resin composition layer disappear when the standing of the lamination precursor is finished. However, since the standing time of the laminated precursor is too long for the time required for the bubbles present in the curable resin composition layer to disappear, the production efficiency decreases due to the increase in the tact time, or This is not preferable because it obstructs downsizing of the equipment.
  • the shape of the floating bubbles in the curable resin composition layer becomes a true sphere by leaving the laminate precursor for a predetermined time, not immediately after releasing the reduced-pressure atmosphere. After that, it is preferable to observe bubbles in the curable resin composition layer.
  • the time required for the shape of the floating bubbles in the curable resin composition layer to become a spherical shape varies depending on the viscosity of the curable resin composition constituting the curable resin composition layer, and the following true spheres: The inventors of the present application have experimentally confirmed that 95% or more of the air bubbles present in the curable resin composition layer become spherical when the predicted conversion time has elapsed.
  • Viscosity of curable resin composition ⁇ Sphericalization prediction time 3 Pa ⁇ s or less 15 sec 3 Pa ⁇ s over 10 Pa ⁇ s or less 30 sec Over 10 Pa ⁇ s 60 sec Therefore, according to the viscosity of the curable resin composition to be used, the laminated precursor is allowed to stand for at least a time corresponding to the above-described sphericity prediction time, and then the bubbles in the curable resin composition layer are observed. Is preferred.
  • the method for observing the diameter and shape of the bubbles present in the curable resin composition layer is not particularly limited. For example, from the surface of the transparent substrate into the curable resin composition layer. The diameter and shape of the existing bubbles can be visually observed. It is also possible to observe the diameter and shape of the bubbles present in the curable resin composition layer by image processing.
  • the curable resin composition layer is observed from the surface of the transparent substrate, and a reference value according to the use of the laminate. It is preferable to confirm the presence or absence of bubbles of the above size.
  • the laminate precursor is allowed to stand for a predetermined time according to the above-described procedures (a) and (b). Then, the bubbles in the curable resin composition layer are eliminated. Taking the procedure of (b) described above as an example, the slope of the graph shown in FIG.
  • the region where the equivalent circle diameter of the floating bubbles is smaller than 400 ⁇ m has the equivalent circle diameter.
  • the slope of the graph is much smaller than in the region larger than 400 ⁇ m. From this, when comparing the region where the equivalent circle diameter of the floating bubbles is smaller than 400 ⁇ m and the region where the equivalent circle diameter is larger than 400 ⁇ m, the region where the equivalent circle diameter is smaller than 400 ⁇ m is the region of the floating bubbles. It is considered that the accuracy of the bubble disappearance prediction time specified based on the equivalent diameter is increased.
  • the estimated bubble disappearance time is the material and physical properties of the substrate for producing the laminate, the seal portion forming curable resin composition, and the resin layer forming curable resin composition, application conditions, vacuum lamination conditions, and conditions for releasing the reduced-pressure atmosphere. Alternatively, it may be obtained separately under other conditions equivalent to various conditions. Then, separately, the lamination precursor after vacuum lamination may be allowed to stand for a predetermined bubble disappearance prediction time, and then the lamination precursor may be cured.
  • the bubble disappearance prediction time does not mean the time until the bubbles in the curable resin composition layer for resin layer formation of the lamination precursor completely disappear, but depends on the use of the laminate. It means the time until bubbles having a size larger than the reference value are not present in the curable resin composition layer.
  • the curable resin composition After confirming that bubbles having a size equal to or larger than the reference value according to the use of the laminate are not present in the curable resin composition layer of the laminate precursor, the curable resin composition is cured. Thereby, the laminated body which has a pair of board
  • thermosetting or photocuring is used depending on the type of the curable resin composition.
  • the curable resin composition to be used is preferably a photocurable resin composition.
  • a photocurable resin composition for example, by irradiating ultraviolet light or short wavelength visible light from a light source (ultraviolet lamp, high pressure mercury lamp, etc.) and curing the photocurable resin composition, A laminate having a cured product layer of the curable resin composition existing between the pair of substrates is produced.
  • a light source ultraviolet lamp, high pressure mercury lamp, etc.
  • Light is irradiated from the transparent substrate side of the pair of substrates.
  • irradiation may be performed from both sides.
  • the laminate to be manufactured is a flat panel display (FPD)
  • FPD flat panel display
  • the flat panel display uses a transmissive display device
  • light transmission can be obtained by operating the device, but it is not operated. Since there are many things which do not have a light transmittance in a state, the light which hardens a photocurable resin composition is irradiated from the transparent substrate used as a protective plate.
  • a transmission-scattering display device that exhibits a transparent state when the flat panel display is not operating is used, light from the display device side can also be used.
  • the light is preferably ultraviolet light or visible light of 450 nm or less.
  • an antireflection layer is provided on a transparent substrate and the resin film used for forming the antireflection layer or the antireflection layer does not transmit ultraviolet rays, curing with visible light is required.
  • the laminate obtained by the production method of the present invention is suitably used for thin-layer solar cell devices, image display devices, and the like.
  • the thin layer solar cell device include a thin film silicon solar cell device, a compound semiconductor solar cell device such as a chalcopyrite system and a CdTe system.
  • a flat panel display such as a liquid crystal display device (LCD), an EL (electroluminescence) display device such as an organic EL or an inorganic EL, a plasma display device, or an electronic ink type image display device.
  • FPD flat panel display
  • the thin-layer solar cell device may be formed only on one of the pair of substrates constituting the laminate, or the thin-layer solar cell device may be formed on both substrates. Good.
  • Examples 1 and 2 are examples, examples 3 and 4 are comparative examples, and examples 5 to 8 are reference examples.
  • Example 1 Preparation of photocurable resin composition for forming seal part (second curable resin composition)
  • Bifunctional polypropylene glycol having a molecular end modified with ethylene oxide (number average molecular weight calculated from hydroxyl value: 4000) and hexamethylene diisocyanate were mixed in a molar ratio of 6 to 7, and then isobornyl acrylate (Osaka)
  • IBXA Organic Chemical Industries, Ltd.
  • 2-hydroxyethyl acrylate is added to the prepolymer obtained by the reaction in the presence of a tin compound catalyst in a molar ratio of about 1: 2, and reacted.
  • UC-1 urethane acrylate oligomer
  • the number of curable groups of UC-1 was 2, and the number average molecular weight was about 55000.
  • the viscosity of the UC-1 solution at 60 ° C. was about 580 Pa ⁇ s. 90 parts by mass of the UC-1 solution and 10 parts by mass of 2-hydroxybutyl methacrylate (manufactured by Kyoeisha Chemical Co., Ltd., light ester HOB) were uniformly mixed to obtain a mixture.
  • the defoaming treatment was performed by placing the photocurable resin composition X for forming a seal part in a decompression device in an open state while being put in a container, and reducing the pressure in the decompression device to about 20 Pa and holding it for 10 minutes. . It was about 1400 Pa.s when the viscosity at 25 degrees C of the photocurable resin composition X for sealing part formation was measured.
  • a soda lime glass substrate having a length of 1100 mm, a width of 900 mm, and a thickness of 2 mm (hereinafter referred to as “substrate A”, which corresponds to one substrate in the present invention) extends along the entire circumference along a position 5 mm inside.
  • substrate A which corresponds to one substrate in the present invention
  • a urethane acrylate oligomer (hereinafter referred to as UA-2) was obtained.
  • the number of curable groups of UA-2 was 2, the number average molecular weight was about 19000, and the viscosity at 25 ° C. was about 1300 Pa ⁇ s.
  • UV absorber manufactured by Ciba Specialty Chemicals, TINUVIN 109
  • the above-mentioned photocurable resin composition Y for resin layer formation is placed in a decompression device in an open state while being put in a container, and the defoaming treatment is performed by reducing the pressure in the decompression device to about 20 Pa and holding for 10 minutes. went. It was 14 Pa * s when the viscosity at 25 degrees C of the photocurable resin composition Y for resin layer formation was measured.
  • the substrate A after the dispersion and dropping of the resin layer forming curable resin composition was placed on the upper surface of the lower surface plate on the lower side of the lifting device in the vacuum chamber of the decompression device.
  • a soda-lime glass plate (referred to as substrate B.
  • substrate B Corresponding to the other substrate in the present invention) having the same shape and thickness as that used for substrate A was electrostatically adsorbed to the lower surface of the upper surface plate on the upper side of the lifting device.
  • the vacuum chamber was sealed and evacuated until the inside of the chamber became 30 Pa. Thereafter, the upper and lower surface plates were brought close to each other by the lifting device in the vacuum chamber, and the substrate A and the substrate B were vacuum laminated.
  • the time from completion of dropping of the curable resin composition for forming a resin layer to vacuum lamination was 120 seconds. Thereafter, the inside of the vacuum chamber was returned to atmospheric pressure (that is, the decompressed atmosphere was released).
  • a laminated precursor composed of the substrate A and the substrate B (referred to as a laminated precursor C), which is separated from the upper and lower surface plates by an elevating device and adhered to the suction pad of the upper upper surface plate, It peeled from the upper surface plate. Thereafter, the laminated precursor C was kept horizontal, and light from the surface light source was transmitted from the lower surface of the substrate B in order to observe the bubbles in the curable resin composition layer for resin layer formation and the shape thereof.
  • a CCD camera is installed above the substrate A to receive light, and the outline of bubbles in the curable resin composition layer is determined by scattered light, and the shape of the bubbles and the equivalent circle diameter are determined by image processing. Carried out.
  • This inspection procedure was performed on 100 samples (laminated precursor C), but no contact bubbles were present in the curable resin composition in all samples.
  • the curable resin composition can be immediately photocured without leaving the laminated precursor C.
  • the equivalent circle diameters of the floating bubbles present in these samples were all 50 ⁇ m or more. Therefore, for all the samples, the bubble disappearance prediction time is specified in advance using FIG.
  • the stacking precursor after vacuum stacking according to Example 1 was subjected to the inspection before the leaving and the re-inspection after the leaving.
  • the ratio of non-defective products is shown in Table 1.
  • the laminated body is manufactured by irradiating the non-defective laminated precursor C with light from the light source to cure the photocurable resin composition for resin layer formation.
  • Example 2 After releasing the reduced-pressure atmosphere, the same procedure as in Example 1 was performed except that the layered precursor C was allowed to stand for 120 seconds at atmospheric pressure and then the above-described inspection was performed. Also in this example, 100 samples (laminated precursor C) were inspected, but in all samples, no contact bubbles were present in the curable resin composition. In addition, for all of the buoyant resin composition layers having an equivalent circle diameter of less than 50 ⁇ m, the curable resin composition can be immediately photocured without leaving the laminated precursor C. The equivalent circle diameters of the floating bubbles present in these samples were all 50 ⁇ m or more.
  • Table 1 shows the ratio of non-defective products during the re-inspection after the re-examination (non-defective product rate).
  • the laminated body is manufactured by irradiating the non-defective laminated precursor C with light from the light source to cure the photocurable resin composition for resin layer formation.
  • Example 3 The same procedure as in Example 2 was performed except that the standing time of the laminated precursor C was shortened by 30 seconds from the estimated bubble disappearance time. Also in this example, 100 samples (laminated precursor C) were inspected, but in all samples, no contact bubbles were present in the curable resin composition. In addition, for all of the buoyant resin composition layers having an equivalent circle diameter of less than 50 ⁇ m, the curable resin composition can be immediately photocured without leaving the laminated precursor C. The equivalent circle diameters of the floating bubbles present in these samples were all 50 ⁇ m or more.
  • Example 4 Without carrying out the above inspection, the same procedure as in Example 1 was carried out except that the re-inspection was carried out after the laminated precursor C was left for 300 seconds. Table 1 shows the percentage of non-defective products at the time of re-inspection in all samples.
  • Example 5 Without carrying out the above inspection, the same procedure as in Example 1 was carried out except that the layered precursor C was allowed to stand for 900 seconds and then the above reinspection was performed. Table 1 shows the percentage of non-defective products at the time of re-inspection in all samples.
  • Example 1 in which the layered precursor C is left for a time corresponding to the bubble disappearance prediction time specified from the equivalent circle diameter of the floating bubbles in the curable resin composition layer are present in the curable resin composition layer. Since the standing time of the laminated precursor C was sufficient with respect to the time required for the floating bubbles to disappear, the non-defective product rate at the re-inspection was excellent at 90% or more. In particular, in Example 2, in which inspection was performed after leaving the reduced-pressure atmosphere for 120 seconds, the non-defective product rate at the time of re-inspection was 100%.
  • Example 3 in which the standing time of the laminated precursor C was shorter by 30 seconds than the estimated bubble disappearance time, the standing time was insufficient, so the yield rate at the time of reinspection was inferior at 85%.
  • Example 4 in which the laminated precursor C was uniformly left for 300 seconds without specifying the bubble disappearance prediction time, the standing time was insufficient, so the yield rate at the time of re-inspection was extremely inferior at 40%.
  • Example 5 in which the laminated precursor C was uniformly left for 900 seconds without specifying the bubble disappearance prediction time, the non-defective product rate at the time of reinspection was excellent at 98%. It is considered that the standing time was slightly excessive as compared with the prepared examples 1 and 2.
  • Example 6 A laminated precursor C was prepared in the same procedure as in Example 1. In this example, after forming the seal portion on the outer peripheral portion of the substrate A, the defect inspection of the seal portion was performed visually. The results were as follows. Defect: The length of the defect portion is less than 0.5 mm in the length of the coating line direction -Thinning: The length of the portion where the coating width is less than 80% (length in the coating line direction) with respect to the reference coating width is continuously less than 10 mm. -Overlap: The overlap of the coating line length is less than 5 mm. All of the defects, thinnings, and overlaps satisfied the criteria for the seal portion described in Paragraph [0025], and no problem occurred in the laminated precursor C to be produced.
  • Example 7 A laminated precursor C was prepared in the same procedure as in Example 1. In this example, after forming the seal portion on the outer peripheral portion of the substrate A, the defect inspection of the seal portion was performed visually. The results were as follows. Defect: The length of the defect portion is 0.5 mm or more in the length of the coating line direction. -Thinning: The length of the portion where the coating width is less than 80% (length in the coating line direction) with respect to the reference coating width is continuously less than 10 mm. -Overlap: The overlap of the coating line length is less than 5 mm. The defect does not satisfy the standard of the seal part described in paragraph [0025], and the curable resin composition protrudes from the region surrounded by the seal part when the vacuum lamination is performed. Bubbles (bubbles with an equivalent circle diameter of 500 ⁇ m or more) were generated.
  • Example 8 A laminated precursor C was prepared in the same procedure as in Example 1. In this example, after forming the seal portion on the outer peripheral portion of the substrate A, the defect inspection of the seal portion was performed visually. The results were as follows. Defect: The length of the defect portion is less than 0.5 mm in the length of the coating line direction -Thinning: The length of the portion where the coating width is less than 80% (length in the coating line direction) with respect to the reference coating width is continuously less than 10 mm. -Overlap: The overlap of the coating line direction length is 5 mm or more.
  • the method for producing a laminate of the present invention at the time of curing the curable resin composition, there are no bubbles in the curable resin composition that are larger than the reference value according to the use of the laminate. Since it can be in a state, it is possible to produce a high-quality laminate without bubble defects.
  • Substrate 20 Seal part 30: Curable resin composition layer 41, 42, 43, 44, 45, 46: Air bubbles

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  • Materials Engineering (AREA)
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  • Ceramic Engineering (AREA)
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Abstract

L'invention concerne un procédé de production d'un corps stratifié par durcissement d'une composition de résine durcissable maintenue et isolée entre une paire de plaques de base, par lequel un corps stratifié exempt de défauts de mousse peut être produit. Le procédé de production d'un corps stratifié comporte les étapes consistant à maintenir et à isoler une composition de résine durcissable entre une paire de plaques de base sous une atmosphère à pression réduite pour obtenir un précurseur de stratifié, puis à placer le précurseur de stratifié sous une deuxième atmosphère sous pression dont la pression atmosphérique est supérieure à celle de l'atmosphère sous pression réduite, et à durcir la composition de résine durcissable sous la deuxième atmosphère sous pression, le procédé comportant une étape consistant à observer les diamètres et les formes de bulles d'air présentes dans la couche de composition de résine durcissable après que le précurseur de stratifié a été placé sous la deuxième atmosphère sous pression, et une étape consistant à laisser reposer le précurseur de stratifié pendant une durée prédéterminée sur la base du résultat obtenu lors de l'étape d'observation des diamètres et les formes des bulles d'air, la composition de résine durcissable étant durcie après ces étapes.
PCT/JP2010/070835 2009-11-24 2010-11-22 Procédé de production d'un corps stratifié Ceased WO2011065336A1 (fr)

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WO2013024725A1 (fr) * 2011-08-12 2013-02-21 旭硝子株式会社 Procédé de fabrication d'un corps en couches
JP2020159553A (ja) * 2019-03-25 2020-10-01 三菱ケミカル株式会社 圧力容器
WO2021020295A1 (fr) * 2019-07-29 2021-02-04 デクセリアルズ株式会社 Procédé de production de dispositif optique

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KR102254291B1 (ko) * 2013-10-16 2021-05-21 니폰 덴키 가라스 가부시키가이샤 유리 필름 적층체의 제조 방법, 유리 필름 적층체, 전자 디바이스의 제조 방법

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JPH02226151A (ja) * 1988-12-23 1990-09-07 E I Du Pont De Nemours & Co 流体加圧による泡のない液体ソルダマスク被覆プリント回路板の製造方法
JPH06305781A (ja) * 1993-04-26 1994-11-01 Fujikura Ltd 光ファイバコーティング樹脂の気泡検出方法及び気泡検出装置
JP2005201785A (ja) * 2004-01-16 2005-07-28 Toppan Printing Co Ltd 混入気泡検知方法、検知装置ならびに複製方法
WO2009016943A1 (fr) * 2007-07-30 2009-02-05 Asahi Glass Company, Limited Composition de résine durcissable, stratifié transparent l'utilisant et procédé pour produire le stratifié transparent
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WO2013024725A1 (fr) * 2011-08-12 2013-02-21 旭硝子株式会社 Procédé de fabrication d'un corps en couches
CN103732380A (zh) * 2011-08-12 2014-04-16 旭硝子株式会社 层叠体的制造方法
JPWO2013024725A1 (ja) * 2011-08-12 2015-03-05 旭硝子株式会社 積層体の製造方法
JP2020159553A (ja) * 2019-03-25 2020-10-01 三菱ケミカル株式会社 圧力容器
JP7318578B2 (ja) 2019-03-25 2023-08-01 三菱ケミカル株式会社 圧力容器
WO2021020295A1 (fr) * 2019-07-29 2021-02-04 デクセリアルズ株式会社 Procédé de production de dispositif optique
JP2021021859A (ja) * 2019-07-29 2021-02-18 デクセリアルズ株式会社 光学装置の製造方法
CN114126849A (zh) * 2019-07-29 2022-03-01 迪睿合株式会社 光学装置的制造方法
JP7274966B2 (ja) 2019-07-29 2023-05-17 デクセリアルズ株式会社 光学装置の製造方法

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