WO2013058217A1 - Stratifié, procédé de fabrication de stratifié et procédé de fabrication d'un substrat de verre ayant un élément pour des dispositifs électroniques attachés à celui-ci - Google Patents

Stratifié, procédé de fabrication de stratifié et procédé de fabrication d'un substrat de verre ayant un élément pour des dispositifs électroniques attachés à celui-ci Download PDF

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Publication number
WO2013058217A1
WO2013058217A1 PCT/JP2012/076641 JP2012076641W WO2013058217A1 WO 2013058217 A1 WO2013058217 A1 WO 2013058217A1 JP 2012076641 W JP2012076641 W JP 2012076641W WO 2013058217 A1 WO2013058217 A1 WO 2013058217A1
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Prior art keywords
glass substrate
resin layer
support plate
resin
laminate
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PCT/JP2012/076641
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English (en)
Japanese (ja)
Inventor
研一 江畑
俊彦 ▲樋▼口
Original Assignee
旭硝子株式会社
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Application filed by 旭硝子株式会社 filed Critical 旭硝子株式会社
Priority to CN201280051485.6A priority Critical patent/CN103889712B/zh
Priority to KR1020147010179A priority patent/KR101973826B1/ko
Priority to JP2013539636A priority patent/JP5924344B2/ja
Publication of WO2013058217A1 publication Critical patent/WO2013058217A1/fr

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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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • 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
    • B32B17/10018—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 only one glass sheet
    • 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
    • B32B17/10009—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
    • B32B17/10082—Properties of the bulk of a glass sheet
    • B32B17/10119—Properties of the bulk of a glass sheet having a composition deviating from the basic composition of soda-lime glass, e.g. borosilicate
    • 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
    • B32B17/10798—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 containing silicone
    • 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
    • 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
    • B32B7/06—Interconnection of layers permitting easy separation
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/133302—Rigid substrates, e.g. inorganic substrates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/136—Liquid crystal cells structurally associated with a semi-conducting layer or substrate, e.g. cells forming part of an integrated circuit
    • G02F1/1362—Active matrix addressed cells
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F2202/00—Materials and properties
    • G02F2202/28—Adhesive materials or arrangements
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/582—Recycling of unreacted starting or intermediate materials

Definitions

  • the present invention relates to a laminate, a method for producing a laminate, and a method for producing a glass substrate with a member for electronic devices.
  • devices such as solar cells (PV), liquid crystal panels (LCD), and organic EL panels (OLED) have been made thinner and lighter, and the glass substrates used in these devices have been made thinner. Progressing. If the strength of the glass substrate is insufficient due to the thinning, the handling property of the glass substrate is lowered in the device manufacturing process.
  • PV solar cells
  • LCD liquid crystal panels
  • OLED organic EL panels
  • a method in which a device member for example, a thin film transistor is formed on a glass substrate thicker than the final thickness and then the glass substrate is thinned by chemical etching is widely used.
  • a device member for example, a thin film transistor
  • this method for example, when the thickness of one glass substrate is reduced from 0.7 mm to 0.2 mm or 0.1 mm, most of the original glass substrate material is scraped off with an etching solution. Therefore, it is not preferable from the viewpoint of productivity and use efficiency of raw materials.
  • a laminated body in which a thin glass substrate and a reinforcing plate are laminated is prepared, and a member for an electronic device such as a display device is formed on the thin glass substrate of the laminated body.
  • a method of separating the support plate from the substrate has been proposed (see, for example, Patent Document 1).
  • the reinforcing plate has a support plate and a resin layer fixed on the support plate, and the resin layer and the thin glass substrate are in close contact with each other in a peelable manner.
  • the interface between the resin layer of the laminate and the thin glass substrate is peeled off, and the reinforcing plate separated from the thin glass substrate can be laminated with a new thin glass substrate and reused as a laminate.
  • a resin layer obtained using the thermosetting resin described in Patent Document 2 is known as a heat-resistant resin layer.
  • a silicone resin having a high heat resistance a silicone resin crosslinked by a condensation reaction is known.
  • the silicone resin described in Patent Document 1 is a silicone resin crosslinked by a hydrosilylation reaction.
  • a silicone resin having a unit in which an aryl group such as a phenyl group is bonded to a silicon atom has particularly high heat resistance.
  • a silicone resin described in Patent Document 2 is known.
  • the present invention has been made in view of the above problems, and can be used even under high-temperature heat treatment conditions, and can maintain the cleanliness of the peeled surface of a glass substrate separated by performing a cleaning treatment. It aims at providing a manufacturing method of a body and this layered product. Another object of the present invention is to provide a method for producing a glass substrate with a member for electronic devices using the laminate.
  • the first aspect of the present invention comprises a support plate layer, a resin layer, and a glass substrate layer in this order, and the peel strength (y) at the interface between the support plate layer and the resin layer is It is higher than the peel strength (x) at the interface between the resin layer and the glass substrate or the cohesive failure strength (z) of the resin layer, the resin of the resin layer is a crosslinked silicone resin, and the crosslinked silicone resin will be described later.
  • the crosslinked silicone resin further comprises an organosiloxy unit (A-2) represented by the following formula (3) and an organosiloxy unit (B-2) represented by the following formula (4).
  • A-2) represented by the following formula (3)
  • B-2 organosiloxy unit
  • the ratio of [(A-1) + (B-2)] to [(A-1) + (A-2) + (B-1) + (B-2)] It is preferably 15 to 50 mol%.
  • the ratio of [(A-1) + (A-2) + (B-1) + (B-2)] to the total organosiloxy unit is preferably 95 to 100 mol%.
  • the organosiloxy units represented by the formulas (1) to (4) described later are preferably units derived from an organoalkoxysilane compound.
  • the peel strength (x) is preferably higher than the cohesive failure strength (z).
  • the thickness of the resin layer is preferably 1 to 5 ⁇ m, and the support plate is preferably a glass plate. Further, the difference in average linear expansion coefficient between the support plate and the glass substrate at 25 to 300 ° C. is preferably 0 to 500 ⁇ 10 ⁇ 7 / ° C.
  • a second aspect of the present invention is a method for producing a laminate according to the first aspect of the present invention, in which a film of a curable silicone resin that is crosslinked and cured to become a crosslinked silicone resin described later is formed on the surface of a support plate. Then, a curable silicone resin is crosslinked and cured on the surface of the support plate to form a crosslinked silicone resin film, and then a glass substrate is laminated on the surface of the crosslinked silicone resin film. is there.
  • the curable silicone resin comprises a partially hydrolyzed condensate of a mixture of organoalkoxysilane compounds, and a solution containing the curable silicone resin and a solvent is applied to the surface of the support plate to remove the solvent.
  • a solution containing the curable silicone resin and a solvent is applied to the surface of the support plate to remove the solvent.
  • the weight average molecular weight of the partial hydrolysis-condensation product is preferably 10,000 to 200,000. Further, the weight average molecular weight of the partial hydrolysis-condensation product is more preferably 10,000 to 100,000.
  • an electronic device member is formed on the glass substrate in the laminate of the first aspect of the present invention to produce a laminate with an electronic device member, and the electronic device member Separation of the glass substrate with an electronic device member from the laminated body is separated into a glass substrate with an electronic device member and a support plate with a resin layer using the glass substrate side interface of the resin layer or the inside of the resin layer as a peeling surface.
  • the cleaning is preferably cleaning using a solvent, and the cleaning is preferably cleaning using a solvent having a solubility parameter of 7 to 15.
  • the said glass substrate with a member for electronic devices is hereafter called "a glass substrate with a member.”
  • the laminated body which can be used also on high temperature heat processing conditions, and can maintain the cleanliness of the peeling surface of the glass substrate isolate
  • FIG. 1 is a schematic cross-sectional view of an embodiment of a laminate according to the present invention.
  • FIG. 2 is a schematic cross-sectional view showing an embodiment of a method for manufacturing an electronic device according to the present invention in the order of steps.
  • the laminate of the present invention includes a support plate layer, a resin layer, and a glass substrate layer in this order. That is, a resin layer is provided between the support plate layer and the glass substrate layer. Therefore, one side of the resin layer is in contact with the support plate layer, and the other side is in contact with the glass substrate layer.
  • the interface between the resin layer and the glass substrate has a peel strength (x). When a stress in the peeling direction exceeding the peel strength (x) is applied to the interface between the resin layer and the glass substrate, the interface between the resin layer and the glass substrate becomes Peel off.
  • the interface between the resin layer and the support plate has a peel strength (y).
  • the interface between the resin layer and the support plate becomes Peel off.
  • the resin of the resin layer has a strength to resist the destruction of itself, and if the resin layer is subjected to a stress in the direction of peeling the glass substrate and the support plate, the resin layer can withstand the stress without breaking to a certain extent. .
  • the resin layer is broken, and the strength that this resin layer can withstand is called the cohesive failure strength (z).
  • the peel strength (y) is higher than the peel strength (x) or the cohesive failure strength (z). Therefore, when a stress in the direction of peeling the glass substrate and the support plate is applied to the laminate of the present invention, the laminate of the present invention peels off at the interface between the resin layer and the glass substrate, and the support plate with the glass substrate and the resin layer is provided. Or a glass substrate to which resin is adhered and a support plate to which resin is adhered due to cohesive failure of the resin layer.
  • the peel strength (x) in the laminate of the present invention is higher than the cohesive failure strength (z)
  • the resin-attached glass substrate and A support plate to which the resin has adhered is generated.
  • the separated glass substrate is a glass substrate with a member. Since it is not preferable that the resin adheres to the peeling surface of the glass substrate with a member (the surface of the glass substrate on which the electronic device member is not formed), it is preferable to remove the resin adhering to the peeling surface. Furthermore, even if the attached resin is removed, the smaller the amount, the easier the removal is.
  • the amount of resin attached to the peeled surface immediately after separation is small.
  • the amount of resin adhering to the release surface of the glass substrate is compared to the amount of resin adhering to the support plate. It is thought that it will decrease.
  • the peel strength (x) and the cohesive failure strength (z) are substantially equal, it is considered that a glass substrate having a resin adhered to the peel surface is likely to be formed. Therefore, in the present invention, the peel strength (x) Is higher than the cohesive failure strength (z).
  • the peel strength (x) in the laminate of the present invention is lower than the cohesive failure strength (z)
  • the glass substrate and the support plate are peeled off to support the glass substrate and the resin layer.
  • a board is produced.
  • the peel strength (x) and the cohesive failure strength (z) are close to each other, there is a possibility that a glass substrate to which a resin is attached and a glass substrate to which no resin is attached are generated for each laminate. Therefore, even if it is considered that there is no resin adhesion, it is preferable to perform an operation of removing the resin in consideration of the possibility of a small amount of resin adhesion to the separation surface of the glass substrate after separation. .
  • the peel strength (y) is preferably sufficiently higher than both the peel strength (x) and the cohesive failure strength (z). Thereby, the resin amount adhering to the support plate after separation can be relatively increased as compared with the glass substrate.
  • Increasing the peel strength (y) means increasing the adhesion of the resin layer to the support plate and maintaining a relatively higher adhesion than the glass substrate after the heat treatment.
  • the resin layer bonded with a high bonding force to the support plate can be formed by the adhesive force at the time of crosslinking and curing.
  • the bonding force of the crosslinked silicone resin after crosslinking and curing to the glass substrate is usually lower than the bonding force generated during the crosslinking and curing. Therefore, it is preferable that a curable silicone resin is crosslinked and cured on a support plate to form a resin layer, and then a glass substrate is laminated on the surface of the resin layer made of the crosslinked and cured silicone resin to produce a laminate.
  • the adhesion of the layer surface of the crosslinked silicone resin crosslinked by the condensation reaction is higher than the layer surface of the crosslinked silicone resin crosslinked by the hydrosilylation reaction described in Patent Document 1. Therefore, in the present invention, when a glass substrate is laminated on the surface of the silicone resin layer that has been sufficiently crosslinked and cured on the support plate, the adhesion between the resin layer surface and the glass substrate surface is the case of the laminate described in Patent Document 1. Is considered to be higher. Therefore, it is considered that the peel strength (x) of the laminate of the present invention is higher than the peel strength at the interface between the resin layer and the glass substrate layer in the laminate described in Patent Document 1.
  • the reactivity of the curable silicone resin that is crosslinked and cured by the condensation reaction is considered to be lower than the reactivity of the curable silicone resin that is crosslinked and cured by the hydrosilylation reaction. Therefore, it is not easy to sufficiently complete the crosslinking reaction of the resin of the resin layer formed on the support plate before laminating with the glass substrate.
  • a glass substrate is laminated on a resin layer made of crosslinked silicone in which unreacted crosslinking points remain, the unreacted crosslinking points are crosslinked after the lamination, and the resin adheres to the glass substrate, which may increase the peel strength (x). Conceivable.
  • the curable silicone resin that is cross-linked and cured by the condensation reaction can sufficiently advance the cross-linking reaction by heating without using a curing catalyst.
  • the crosslinked silicone resin in which the curing catalyst remains there is a risk of generation of low molecular weight silicone due to depolymerization of the crosslinked silicone resin due to the action of the curing catalyst. Therefore, the generation of low molecular weight silicone can be reduced by not using the curing catalyst. . Due to the low amount of low molecular weight silicone, there is little gas generation due to low molecular weight silicone under high temperature conditions when forming electronic device members on the glass substrate surface of the laminate, and contamination of electronic device members due to gas generation The characteristic that there is little fear of this is demonstrated.
  • an easy peeling treatment may be applied to the interface to be laminated using a silicon compound or a fluorine compound for the purpose of adjusting the peeling strength before the lamination.
  • the separation of the glass substrate and the support plate is usually performed on the laminated body (laminated body with the electronic device member) after the formation of the electronic device member. It is considered that the resin adheres to the peeling surface of the attached glass substrate. As described above, it is not preferable that the resin adheres to the peeling surface of the glass substrate with a member, and the resin attached to the peeling surface of the glass substrate with a member usually needs to be removed.
  • the resin in the present invention has solvent solubility. Therefore, it is preferable to remove the resin by a removing operation using a solvent.
  • FIG. 1 is a schematic cross-sectional view of an example of a laminate according to the present invention.
  • the laminated body 10 is a laminated body in which the layer of the support plate 12, the layer of the glass substrate 16, and the resin layer 14 exist between them.
  • the resin layer 14 has one surface in contact with the layer of the support plate 12 and the other surface in contact with the first main surface 16 a of the glass substrate 16. In other words, the resin layer 14 is in contact with the first main surface 16 a of the glass substrate 16.
  • the two-layer portion composed of the layer of the support plate 12 and the resin layer 14 reinforces the glass substrate 16 in a member forming process for manufacturing a member for an electronic device such as a liquid crystal panel.
  • the two-layer part which consists of the layer of the support plate 12 manufactured beforehand for manufacture of the laminated body 10 and the resin layer 14 is called the support plate 18 with a resin layer.
  • This laminate 10 is used until the member forming step. That is, the laminate 10 is used until a member for an electronic device such as a liquid crystal display device is formed on the surface of the second main surface 16b of the glass substrate 16. Then, the laminated body in which the member for electronic devices was formed is isolate
  • the support plate 12 to which the resin is attached (or the support plate 12 having the resin layer 14) is not a part constituting the electronic device. The separated support plate 12 is laminated with a new glass substrate 16 after removing the adhering resin or resin layer 14 if necessary, and can be reused as the laminate 10.
  • each layer glass substrate, support plate, resin layer
  • resin material constituting the laminate will be described in detail, and then the laminate and the method for manufacturing the electronic device will be described in detail.
  • the 1st main surface 16a touches the resin layer 14, and the member for electronic devices is provided in the 2nd main surface 16b on the opposite side to the resin layer 14 side.
  • the glass substrate 16 may be of a general type, and examples thereof include a glass substrate for a display device such as an LCD or an OLED.
  • the glass substrate 16 is excellent in chemical resistance and moisture permeability and has a low heat shrinkage rate.
  • As an index of the heat shrinkage rate a linear expansion coefficient defined in JIS R 3102 (revised in 1995) is used.
  • the member forming process often involves heat treatment, and various inconveniences are likely to occur.
  • the TFT may be displaced excessively due to thermal contraction of the glass substrate 16.
  • the glass substrate 16 is obtained by melting a glass raw material and molding the molten glass into a plate shape.
  • a molding method may be a general one, and for example, a float method, a fusion method, a slot down draw method, a full call method, a rubber method, or the like is used.
  • the glass substrate 16 having a particularly small thickness can be obtained by heating a glass once formed into a plate shape to a moldable temperature and then stretching it by means of stretching or the like to make it thin (redraw method).
  • the glass of the glass substrate 16 is not particularly limited, but non-alkali borosilicate glass, borosilicate glass, soda lime glass, high silica glass, and other oxide-based glasses mainly composed of silicon oxide are preferable.
  • oxide-based glass a glass having a silicon oxide content of 40 to 90% by mass in terms of oxide is preferable.
  • glass suitable for the type of electronic device member and the manufacturing process thereof is employed.
  • a glass substrate for a liquid crystal panel is made of glass (non-alkali glass) that does not substantially contain an alkali metal component because the elution of an alkali metal component easily affects the liquid crystal (however, usually an alkaline earth metal) Ingredients are included).
  • the glass of the glass substrate 16 is appropriately selected based on the type of device to be applied and its manufacturing process.
  • the thickness of the glass substrate 16 is preferably 0.3 mm or less, more preferably 0.15 mm or less, from the viewpoint of reducing the thickness and / or weight of the glass substrate 16. In the case of 0.3 mm or less, it is possible to give good flexibility to the glass substrate 16. In the case of 0.15 mm or less, the glass substrate 16 can be rolled up. Further, the thickness of the glass substrate 16 is preferably 0.03 mm or more for reasons such as easy manufacture of the glass substrate 16 and easy handling of the glass substrate 16.
  • the glass substrate 16 may be composed of two or more layers.
  • the material forming each layer may be the same material or a different material.
  • the thickness of the glass substrate 16 means the total thickness of all the layers.
  • the support plate 12 supports and reinforces the glass substrate 16, and the glass substrate is deformed, scratched, damaged, etc. during the manufacture of the electronic device member in the member forming step (step of manufacturing the electronic device member) described later. To prevent.
  • the support plate 12 for example, a metal plate such as a glass plate, a plastic plate, or a SUS plate is used.
  • the support plate 12 is preferably formed of a material having a small difference in linear expansion coefficient from the glass substrate 16, and more preferably formed of the same material as the glass substrate 16.
  • the support plate 12 is preferably a glass plate.
  • the support plate 12 is preferably a glass plate made of the same glass material as the glass substrate 16.
  • the thickness of the support plate 12 may be thicker or thinner than the glass substrate 16.
  • the thickness of the support plate 12 is selected based on the thickness of the glass substrate 16, the thickness of the resin layer 14, and the thickness of the laminate 10.
  • the support is provided.
  • the thickness of the plate 12 is 0.4 mm.
  • the thickness of the support plate 12 is preferably 0.2 to 5.0 mm.
  • the thickness of the glass plate is preferably 0.08 mm or more because it is easy to handle and difficult to break. Further, the thickness of the glass plate is preferably 1.0 mm or less because the rigidity is desired so that the glass plate is appropriately bent without being broken when it is peeled off after forming the electronic device member.
  • the difference in average linear expansion coefficient between the support plate 12 and the glass substrate 16 at 25 to 300 ° C. is preferably 500 ⁇ 10 ⁇ 7 / ° C. or less, more preferably It is 300 ⁇ 10 ⁇ 7 / ° C. or less, more preferably 200 ⁇ 10 ⁇ 7 / ° C. or less. If the difference is too large, the laminated body 10 may be warped severely or the support plate 12 and the glass substrate 16 may be peeled off during heating and cooling in the member forming process. When the material of the support plate 12 is the same as the material of the glass substrate 16, it can suppress that such a problem arises.
  • the resin layer 14 prevents displacement of the glass substrate 16 until the operation of separating the glass substrate 16 and the support plate 12 is performed, and prevents the glass substrate 16 and the like from being damaged by the separation operation.
  • the surface 14 a of the resin layer 14 that contacts the glass substrate 16 is in close contact with the first main surface 16 a of the glass substrate 16.
  • the resin layer 14 is bonded to the first main surface 16a of the glass substrate 16 with a weak bonding force, and the peel strength (x) of the interface is the peel strength (y of the interface between the resin layer 14 and the support plate 12). ) In many cases.
  • the bonding force at the interface between the resin layer 14 and the glass substrate 16 may change before and after the electronic device member is formed on the surface (second main surface 16b) of the glass substrate 16 of the laminate 10 (that is, peeling). Intensity (x) may vary). However, even after the electronic device member is formed, the peel strength (x) is preferably lower than the peel strength (y).
  • the resin layer 14 and the glass substrate 16 are bonded to each other with a bonding force resulting from a weak adhesive force or van der Waals force.
  • the cross-linked silicone resin of the resin layer 14 is sufficiently cross-linked so as not to exhibit adhesive strength, the bonding force due to van der Waals force It is thought that it is united.
  • the crosslinked silicone resin of the resin layer 14 often has a certain degree of weak adhesive strength. Even when the adhesion is extremely low, when a member for an electronic device is formed on the laminate after the laminate is manufactured, the crosslinked silicone resin of the resin layer 14 is adhered to the glass substrate surface by a heating operation or the like.
  • the bonding force between the resin layer 14 and the glass substrate 16 is considered to increase.
  • the surface of the resin layer 14 before lamination or the first main surface 16a of the glass substrate 16 before lamination can be laminated by performing a treatment for weakening the bonding force between them.
  • the bonding strength at the interface between the resin layer 14 and the glass substrate 16 can be weakened, and the peel strength (x) can be lowered.
  • the resin layer 14 is bonded to the surface of the support plate 12 with a strong bonding force such as an adhesive force or an adhesive force.
  • a strong bonding force such as an adhesive force or an adhesive force.
  • the cross-linked resin can be adhered to the surface of the support plate 12 to obtain a high bonding strength.
  • the process for example, process using a coupling agent
  • the bond force between the support plate 12 surface and the resin layer 14 can be raised.
  • the fact that the resin layer 14 and the layer of the support plate 12 are bonded with a high bonding force means that the peel strength (y) at the interface between them is high.
  • the thickness of the resin layer 14 is not particularly limited, but is preferably 1 to 5 ⁇ m, more preferably 1 to 4 ⁇ m, and still more preferably 1 to 3 ⁇ m. When the thickness of the resin layer 14 is within such a range, even if bubbles or foreign matter may be present between the resin layer 14 and the glass substrate 16, the occurrence of distortion defects in the glass substrate 16 can be suppressed. Can do. In addition, if the thickness of the resin layer 14 is too thick, it takes time and materials to form the resin layer 14 and is not economical.
  • the resin layer 14 may be composed of two or more layers. In this case, “the thickness of the resin layer 14” means the total thickness of all the layers. Moreover, when the resin layer 14 consists of two or more layers, the resin which forms each layer may consist of a different crosslinked silicone resin.
  • the resin of the resin layer 14 has its own strength as a characteristic of the material, and the resin breaks when subjected to a stress greater than the cohesive failure strength (z). Therefore, when the resin layer 14 receives stress in the thickness direction and in the extending direction, and the stress exceeds the cohesive failure strength (z), the resin layer 14 breaks inside the layer. As a result, the resin layer on the glass substrate side from the fracture surface adheres to the glass substrate surface, and the resin layer 14 on the support plate 12 side from the fracture surface adheres to the glass substrate 16 surface. Therefore, when the resin of the resin layer 14 cohesively breaks in the laminate with the member for electronic devices, one becomes a glass substrate with a member with the resin attached to the first main surface 16a, and the other has the support plate 12 with the resin attached to the surface.
  • the cohesive failure strength (z) of the cross-linked silicone resin is higher than the peel strength (y) as long as the bonding strength between the resin layer 14 and the support plate 12 is not particularly lowered as a characteristic of the material. It is rare to get high.
  • the cohesive failure strength (z) may be lower or higher than the peel strength (x).
  • the peel strength (x) can be adjusted and can vary. In particular, when the electronic device member is formed on the second main surface 16b of the glass substrate 16, the peel strength (x) is likely to increase, whereby the cohesive failure strength (z) is lower than the peel strength (x). Prone.
  • the resin layer 14 When the resin layer 14 is coherently broken, the resin does not always adhere to the entire first main surface 16a of the glass substrate 16.
  • the difference between the cohesive failure strength (z) and the peel strength (x) is small, the resin layer 14 and the glass substrate 16 are partially peeled at the interface, and the resin is formed on a part of the first main surface 16a on the glass substrate surface. There may be a surface that is not attached.
  • the resin layer 14 is made of a crosslinked silicone resin.
  • the crosslinked silicone resin is obtained by crosslinking and curing a curable silicone resin.
  • the curable silicone resin in the present invention is a mixture (monomer mixture) of hydrolyzable organosilane compounds as monomers, or a partial hydrolysis condensate obtained by subjecting the monomer mixture to a partial hydrolysis condensation reaction. Moreover, the mixture of a partial hydrolysis-condensation product and a monomer may be sufficient.
  • the curable silicone resin in the present invention is preferably a partially hydrolyzed condensate of a monomer mixture.
  • the curable silicone resin In order to crosslink and cure the curable silicone resin, it is usually cured by proceeding with a crosslinking reaction by heating (that is, thermosetting).
  • a crosslinked silicone resin can be obtained by thermally curing the curable silicone resin.
  • heating is not necessarily required for curing, and room temperature curing can also be performed.
  • the crosslinked silicone resin is composed of a trifunctional organosiloxy unit called a T unit and a bifunctional organosiloxy unit called a D unit.
  • a monofunctional organosiloxy unit called M unit or a tetrafunctional organosiloxy unit called Q unit may be contained.
  • the Q unit is a unit that does not have an organic group bonded to a silicon atom (an organic group having a carbon atom bonded to a silicon atom), but is regarded as an organosiloxy unit in the present invention.
  • the organosiloxy unit (A-1) and organosiloxy unit (B-2) described later in the present invention are T units, and the organosiloxy unit (B-1) and organosiloxy unit (A-2) described below are T units.
  • T units Is D units.
  • the organosiloxy unit (A-1) is also simply referred to as (A-1) unit
  • the organosiloxy unit (B-1) is also simply referred to as (B-1) unit.
  • the M unit in the crosslinked silicone resin is used to adjust the molecular weight of the crosslinked silicone resin or curable silicone resin
  • the Q unit is used to increase the crosslinking point.
  • the cross-linked silicone resin in the present invention does not require M units or Q units, and preferably contains neither M units nor Q units, and even if included, the number is preferably small.
  • the ratio of the total of T units and D units to all organosiloxy units of the crosslinked silicone resin is preferably 90 to 100 mol%, more preferably 95 to 100 mol%, from the viewpoint that the effect of the present invention is more excellent.
  • the proportion of M units and Q units is preferably less than 10 mol% (however, the sum of both is less than 10 mol%), and each is 5 mol%. Is preferable (however, the sum of both is less than 5 mol%).
  • the crosslinked silicone resin in the present invention contains neither M units nor Q units.
  • the cross-linked silicone resin contains a large amount of M units, the heat resistance of the resin tends to decrease, and when it contains a large amount of Q units, the brittleness of the resin tends to increase, which may not be suitable as a material for the resin layer in the present invention. Arise.
  • the crosslinked silicone resin in the present invention includes an organosiloxy unit (A-1) represented by the formula (1) described later and an organosiloxy unit (B-1) represented by the formula (2) described later. .
  • the ratio of the total amount of (A-1) units and (B-1) units (represented by (A-1) + (B-1)) to all organosiloxy units is 70 to 100 mol%, and 30 mol% Below is the total amount of T units other than (A-1) units, D units other than (B-1) units, M units and Q units. M units and Q units are preferably not included. In this case, less than 30 mol% is the total amount of T units other than (A-1) units and D units other than (B-1) units.
  • the ratio of (A-1) + (B-1) to all organosiloxy units is preferably 85 to 100 mol%, more preferably 90 to 100 mol%.
  • the remaining units are T units other than the (A-1) unit (especially the organosiloxy unit (B-2) described later is preferred) and / or D units other than the (B-1) unit (especially the organosiloxy unit described later ( A-2) is preferred).
  • the ratio of the (A-1) unit to the total of the (A-1) unit and the (B-1) unit is 15 to 50 mol%.
  • a more preferred ratio is 20 to 40 mol%.
  • the (A-1) unit is less than 15 mol%, the heat resistance of the crosslinked silicone resin is poor, and voids and the like are likely to occur in the resin layer.
  • the (A-1) unit is more than 50 mol%, The brittleness increases and cracks or the like are likely to occur in the resin layer. In either case, the flatness of the surface tends to be lowered during the formation of the resin layer, and it is difficult to laminate a glass substrate on the surface of the resin layer.
  • the crosslinked silicone resin contains T units other than (A-1) units and D units other than (B-1) units, all T units including (A-1) units and (B-1) units are included.
  • the ratio of all T units to the total amount of all D units, that is, T / [T + D] is preferably 15 to 50 mol%, more preferably 20 to 40 mol%.
  • the organosiloxy unit (A-1) is a unit represented by the following formula (1)
  • the organosiloxy unit (B-1) is a unit represented by the following formula (2).
  • R 1 represents a hydrogen atom or an alkyl group having 1 to 4 carbon atoms.
  • R 6 and R 7 each independently represents an alkyl group having 1 to 4 carbon atoms.
  • the unit (A-1) is a T unit having a phenyl group, and the phenyl group may have an alkyl group having 1 to 4 carbon atoms.
  • R 1 is preferably a hydrogen atom or an alkyl group having 1 or 2 carbon atoms, and particularly preferably a hydrogen atom.
  • the unit (B-1) is a D unit having two alkyl groups.
  • the two alkyl groups are each preferably a methyl group or an ethyl group, more preferably a methyl group.
  • a crosslinked silicone resin having an organosiloxy unit in which an aromatic ring is bonded to a silicon atom has higher heat resistance than a crosslinked silicone resin having an organosiloxy unit in which an alkyl group is bonded to a silicon atom.
  • Crosslinked silicone resins having a large proportion of T units tend to be brittle even when heat resistance is good, but the crosslinked silicone resin in the present invention has a T unit having an aromatic ring so that the proportion of T units is small to some extent. Even if it is a thing, it becomes a crosslinked silicone resin with high heat resistance and low brittleness.
  • the organosiloxy unit in which an aromatic ring other than the unit (A-1) is bonded to a silicon atom is preferably an organosiloxy unit (A-2) represented by the following formula (3), and other than the organosiloxy unit (B-1)
  • the organosiloxy unit in which the alkyl group is bonded to a silicon atom is preferably an organosiloxy unit (B-2) represented by the following formula (4).
  • the unit (A-2) is a D unit
  • the unit (B-2) is a T unit.
  • R 1 represents a hydrogen atom or an alkyl group having 1 to 4 carbon atoms
  • R 2 represents an alkyl group having 1 to 4 carbon atoms.
  • R 6 represents an alkyl group having 1 to 4 carbon atoms.
  • An organosiloxy unit in which an aromatic ring other than the unit (A-1) or the unit (A-2) is bonded to a silicon atom includes a D unit having two aromatic rings.
  • Examples of the organosiloxy unit in which an alkyl group other than the (B-1) unit or the (B-2) unit is bonded to a silicon atom include a D unit and a T unit having an alkyl group having 5 or more carbon atoms.
  • the crosslinked silicone resin having these units may have insufficient properties such as mechanical properties, and the crosslinked silicone resin in the present invention preferably does not contain such an organosiloxy unit.
  • the crosslinked silicone resin in the present invention may contain at least one of (A-2) unit and (B-2) unit.
  • the crosslinked silicone resin in the present invention comprises at least one of (A-1) unit, (B-1) unit, and (A-2) unit and (B-2) unit, the above T unit and D unit
  • the ratio of T unit to the total of [(A-1) + (A-2) + (B-1) + (B-2)] is the ratio of [(A-1) + (B-2)] 15 to 50 mol% is preferable, and 20 to 40 mol% is more preferable.
  • the ratio of the organosiloxy unit having an aromatic ring to the total organosiloxy unit that is, [(A-1) to [(A-1) + (A-2) + (B-1) + (B-2)].
  • the ratio of + (A-2)] is preferably 20 to 40 mol%. A more preferable ratio is 20 to 30 mol%.
  • the ratio of [(A-1) + (B-1)] to (B-2)] is 70 to 100 mol%, preferably 85 to 100 mol%, and 95 to 100 mol%. Is more preferable.
  • the cross-linked silicone resin in the present invention includes a phenyl group (X) represented by the following formula (9) in the above formulas (1) and (3), and R 6 and / or R in the above formulas (2) and (4).
  • R 1 represents a hydrogen atom or an alkyl group having 1 to 4 carbon atoms.
  • Each organosiloxy unit in the crosslinked silicone resin in the present invention is generated from a hydrolyzable organosilane compound as a monomer.
  • the hydrolyzable group in the hydrolyzable organosilane compound is preferably an alkoxy group, but is not limited thereto, and may be a halogen atom such as a chlorine atom, an acyl group, an amino group, or an alkoxyalkoxy group.
  • the curable silicone resin to be a crosslinked silicone resin may be a mixture of hydrolyzable organosilane compounds as monomers, but a partial hydrolysis condensate obtained from a mixture of hydrolyzable organosilane compounds is preferred.
  • the partially hydrolyzed condensate has silanol groups and is crosslinked by dehydration condensation between the silanol groups to form a crosslinked silicone resin.
  • the partially hydrolyzed condensate may contain a hydrolyzable group, and may be crosslinked and cured by a condensation reaction between the hydrolyzable group and the silanol group or a condensation reaction between the hydrolyzable groups.
  • an alkoxysilane compound having an alkoxy group as a hydrolyzable group is preferable.
  • the alkoxysilane compound serving as the (A-1) unit a compound represented by the following formula (5) is preferable, and as the alkoxysilane compound serving as the (B-1) unit, a compound represented by the following formula (6) is preferable.
  • R 1, R 6, R 7 are each the above formula (1) is the same as R 1, R 6, R 7 in formula (2).
  • R 3 , R 4 , R 5 , R 8 , and R 9 each independently represents an alkyl group having 1 to 4 carbon atoms.
  • R 3 , R 4 , R 5 , R 8 , and R 9 are each independently preferably a methyl group or an ethyl group, and R 3 , R 4 , and R 5 are preferably all methyl groups.
  • R 8 and R 9 are all preferably ethyl groups.
  • alkoxysilane compound serving as the (A-2) unit a compound represented by the following formula (7) is preferable, and as the alkoxysilane compound serving as the (B-2) unit, a compound represented by the following formula (8) is preferable.
  • R 1, R 2, R 6 are each the above formula (3) is the same as R 1, R 2, R 6 in the formula (4).
  • R 3 , R 4 , R 8 , R 9 and R 10 each independently represents an alkyl group having 1 to 4 carbon atoms.
  • R 3, R 4, R 8, R 9, R 10 each independently represents preferably a methyl group or an ethyl group, particularly preferably R 3, R 4 are each a methyl group, R 8 , R 9 and R 10 are all preferably ethyl groups.
  • each hydrolyzable organosilane compound and one of each organosiloxy unit have a one-to-one correspondence. That is, the proportion of each organosiloxy unit in the crosslinked silicone resin corresponds to the proportion of each hydrolyzable organosilane compound (monomer). Therefore, by using a monomer mixture mixed in the same proportion as the proportion of each organosiloxy unit or a partially hydrolyzed condensate obtained from the monomer mixture as a curable silicone resin, a crosslinked silicone having an organosiloxy unit in the proportion described above. A resin is obtained.
  • hydrolyzable organosilane compound used as M unit trialkyl alkoxysilane compounds, such as a trimethylethoxysilane, are preferable, and the hydrolyzable silane compound used as Q unit (however, in this specification, hydrolyzable organosilane compound and Tetraalkoxysilane compounds such as tetraethoxysilane are preferred.
  • the curable silicone resin may be a monomer mixture in which the hydrolyzable organosilane compound is mixed so as to have a proportion of each organosiloxy unit. However, it is preferably a partially hydrolyzed condensate from the aspects of reaction control and handling. Hereinafter, the partially hydrolyzed condensate is also referred to as a curable oligomer.
  • the partially hydrolyzed condensate is obtained by partially hydrolyzing and condensing a monomer mixture in which a hydrolyzable organosilane compound is mixed so as to have the ratio of each of the above organosiloxy units.
  • the method of partially hydrolytic condensation is not particularly limited.
  • the catalyst an acid catalyst or an alkali catalyst can be used, but an alkali catalyst is preferably used in order to control the reaction and obtain a partial hydrolysis-condensation product having an appropriate molecular weight.
  • water it is usually preferable to use water for the hydrolysis reaction.
  • the partial hydrolysis-condensation product used in the present invention is preferably a product produced by reacting a mixture of a hydrolyzable organosilane compound in a solvent in the presence of an aqueous alkaline solution.
  • Patent Document 2 As a specific method for producing a partially hydrolyzed condensate, the method described in Patent Document 2 (particularly, the method described in the Examples) is preferable.
  • the curable silicone resin in the present invention is the curable oligomer (that is, a partially hydrolyzed condensate)
  • the polystyrene-reduced weight average molecular weight is 5,000 or more by GPC (gel permeation chromatography) measurement. It is preferable.
  • the weight average molecular weight is more preferably 10,000 or more. If the molecular weight is too low, the amount of water or alkanol by-produced in the crosslinking reaction increases, and the risk of voids occurring in the crosslinked silicone resin increases.
  • the weight average molecular weight of the curable oligomer is preferably 200,000 or less, preferably 100,000.
  • the molecular weight of the curable oligomer can be adjusted by controlling the reaction conditions. For example, by adjusting the amount of the solvent in producing the curable oligomer and increasing the concentration of the hydrolyzable organosilane compound, a high molecular weight product is obtained, and when the concentration is lowered, a low molecular weight product is obtained.
  • the curable oligomer mainly has a silanol group as a reactive group, and is crosslinked by a reaction between the silanol groups to become a crosslinked silicone resin.
  • the silanol group cross-linking reaction is a dehydration condensation reaction, and water is by-produced.
  • the thin resin layer of the laminate of the present invention causes water to be by-produced when, for example, a curable oligomer film is cured on a support plate. Can be sufficiently removed.
  • the temperature conditions for crosslinking are not particularly limited as long as the heat resistance of the crosslinked silicone resin and the adhesion to the support plate are maintained, but are preferably 300 to 475 ° C, more preferably 350 to 450 ° C.
  • the heating time is usually preferably 30 to 300 minutes, more preferably 60 to 120 minutes. If the temperature is too low, the resin will not be sufficiently crosslinked and the heat resistance of the resin will decrease or the flatness of the resin layer will tend to decrease, while if the temperature is too high, the adhesive strength of the resin layer to the support plate will be low. It tends to decline.
  • alkanol and the like may be by-produced in addition to water due to the crosslinking reaction, but can be easily removed from the resin like water.
  • the amount of volatile components such as water in the resin layer of the laminate can be made extremely small, and low molecules such as water under high temperature conditions when the electronic device member is formed on the glass substrate surface of the laminate. Gas generation caused by the compound can be reduced.
  • a layer of a curable silicone resin is formed on the support plate 12 and the curable silicone resin is crosslinked and cured to form the resin layer 14.
  • a solution in which the curable silicone resin is dissolved in a solvent is used, and this solution is applied on the support plate 12 to form a solution layer.
  • the solvent is preferably removed to form a curable silicone resin layer.
  • the thickness of the curable silicone resin layer can be controlled by adjusting the concentration of the solution.
  • the solvent is not particularly limited as long as it can easily dissolve the curable silicone resin in a working environment and can be easily volatilized and removed.
  • the solid content concentration of the solution containing the curable silicone resin and the curable oligomer is preferably 30 to 70% by mass, and more preferably 40 to 60% by mass.
  • the laminate 10 of the present invention is a laminate in which the support plate 12, the glass substrate 16, and the resin layer 14 exist between them.
  • the method for producing the laminate 10 of the present invention is not particularly limited, but is curable on the surface of the support plate in order to obtain a laminate having a peel strength (y) higher than the peel strength (x) or the cohesive failure strength (z).
  • a method of forming a resin layer by crosslinking and curing a silicone resin is preferable. That is, a curable silicone resin film is formed on the surface of the support plate, and the curable silicone resin is crosslinked and cured on the surface of the support plate to form a crosslinked silicone resin film.
  • a glass substrate is laminated to produce a laminate.
  • the step of forming a curable silicone resin film on the surface of the support plate and crosslinking and curing the curable silicone resin on the surface of the support plate to form a crosslinked silicone resin film is a resin layer forming step
  • the process of laminating a glass substrate on the surface of the film to form a laminate is referred to as a lamination process, and the procedure of each process will be described in detail.
  • the resin layer forming step the above-described solution containing the curable silicone resin and the solvent is applied on the surface of the support plate 12, and the solvent is removed to form a film of the curable silicone resin on the surface of the support plate 12.
  • the curable silicone resin film on the support plate 12 is thermally cured to form the resin layer 14. More specifically, as shown in FIG. 2A, in this step, the resin layer 14 is formed on at least one surface of the support plate 12.
  • the method of applying the curable silicone resin solution on the surface of the support plate 12 is not particularly limited, and a known method can be used. Examples thereof include spray coating, die coating, spin coating, dip coating, roll coating, bar coating, screen printing, and gravure coating.
  • the curable silicone resin is preferably cured by precuring (precuring) and then curing (main curing). By performing precure, a resin layer having excellent heat resistance can be obtained.
  • Pre-curing is preferably performed following removal of the solvent. In that case, there is no particular distinction between the step of removing the solvent from the solution film to form the curable silicone resin film and the step of pre-curing.
  • the removal of the solvent is preferably performed by heating to 100 ° C. or higher, and precure can be continued by heating to 150 ° C. or higher.
  • the temperature at which the solvent is removed and precured and the heating time are preferably 100 to 300 ° C. and 5 to 60 minutes, more preferably 150 to 250 ° C. and 10 to 30 minutes.
  • the temperature condition for thermosetting the curable silicone resin is not particularly limited as long as the heat resistance of the resin layer is improved and the peel strength (x) after lamination with the glass substrate can be controlled as described above. 475 ° C is preferable, and 350 to 450 ° C is more preferable.
  • the heating time is usually preferably 30 to 300 minutes, more preferably 60 to 120 minutes. If the temperature of thermosetting is too low, the heat resistance and the flatness of the resin layer will be reduced. On the other hand, if the temperature is too high, the peel strength (x) will be too low, making it difficult to laminate the glass substrates. is there.
  • the glass substrate 16 is laminated on the resin layer 14 obtained in the resin layer formation step, and the support plate 12, the resin layer 14, and the glass substrate 16 are provided in this order.
  • This is a step of obtaining a laminate. More specifically, as shown in FIG. 2B, a glass substrate 16 having a surface 14a opposite to the support plate 12 side of the resin layer 14, and a first main surface 16a and a second main surface 16b.
  • the resin layer 14 and the glass substrate 16 are laminated by using the first main surface 16a as a laminated surface to obtain the laminated body 10.
  • stacking the glass substrate 16 on the resin layer 14 is not restrict
  • the surface of the glass substrate 16 in contact with the resin layer 14 is sufficiently washed and laminated in an environment with a high degree of cleanliness.
  • pre-annealing process heat processing
  • the adhesion of the laminated glass substrate 16 to the resin layer 14 is improved, and an appropriate peel strength (x) can be obtained. This makes it difficult to cause misalignment and improves the productivity of electronic devices.
  • the conditions for the pre-annealing process are appropriately selected according to the type of resin layer to be used, but from the viewpoint of making the peel strength (x) between the glass substrate 16 and the resin layer 14 more appropriate, Heat treatment is preferably performed at 300 ° C. or higher (preferably 300 to 400 ° C.) for 5 minutes or longer (preferably 5 to 30 minutes).
  • the laminate 10 of the present invention can be used for various applications, for example, for manufacturing electronic parts such as a display device panel, PV, a thin film secondary battery, and a semiconductor wafer having a circuit formed on the surface. Applications are listed. In this application, the laminate 10 is often exposed (for example, 1 hour or longer) under high temperature conditions (for example, 400 ° C. or higher).
  • the display device panel includes an LCD, an OLED, an electronic paper, a plasma display panel, a field emission panel, a quantum dot LED panel, a MEMS (MICRO ELECTRO mechanical system) shutter panel, and the like.
  • the glass substrate with a member for electronic devices (glass substrate with a member) containing a glass substrate and the member for electronic devices is manufactured using the laminated body mentioned above.
  • the manufacturing method of this glass substrate with a member is not specifically limited, From the point which is excellent in the productivity of an electronic device, the member for electronic devices is formed on the glass substrate in the said laminated body, and the laminated body with a member for electronic devices is manufactured.
  • the obtained laminated body with a member for an electronic device is separated into a glass substrate with a member and a support plate with a resin layer with the glass substrate side interface of the resin layer or the inside of the resin layer as a peeling surface, and then the glass substrate with a member A method of cleaning the release surface is preferred.
  • the step of forming a member for an electronic device on the glass substrate in the laminate and manufacturing the laminate with the member for an electronic device is a member forming step, and the glass substrate side interface of the resin layer from the laminate with the member for an electronic device
  • the process of separating the resin layer inside into the glass substrate with a member and the support plate with the resin layer as a separation surface is referred to as a separation step, and the step of cleaning the separation surface of the glass substrate with a member as a cleaning treatment step.
  • the materials and procedures used in each process are described in detail below.
  • a member formation process is a process of forming the member for electronic devices on the glass substrate 16 in the laminated body 10 obtained in the said lamination process. More specifically, as shown in FIG. 2C, the electronic device member 20 is formed on the second main surface 16b (exposed surface) of the glass substrate 16 to obtain the laminate 22 with the electronic device member. .
  • the electronic device member 20 used in this step will be described in detail, and the procedure of the subsequent steps will be described in detail.
  • the electronic device member 20 is a member that is formed on the glass substrate 16 in the laminate 10 and constitutes at least a part of the electronic device. More specifically, as the electronic device member 20, a member used for an electronic component such as a display panel, a solar cell, a thin film secondary battery, or a semiconductor wafer having a circuit formed on the surface (for example, Display member, solar cell member, thin film secondary battery member, electronic component circuit).
  • a silicon type includes a transparent electrode such as tin oxide of a positive electrode, a silicon layer represented by p layer / i layer / n layer, a metal of a negative electrode, and the like. And various members corresponding to the dye-sensitized type, the quantum dot type, and the like.
  • a transparent electrode such as a metal or a metal oxide of a positive electrode and a negative electrode, a lithium compound of an electrolyte layer, a metal of a current collecting layer, a resin as a sealing layer, etc.
  • various members corresponding to nickel hydrogen type, polymer type, ceramic electrolyte type and the like can be mentioned.
  • a circuit for an electronic component in a CCD or CMOS, a metal of a conductive part, a silicon oxide or a silicon nitride of an insulating part, and the like, various sensors such as a pressure sensor and an acceleration sensor, a rigid printed board, a flexible printed board And various members corresponding to a rigid flexible printed circuit board.
  • the manufacturing method of the laminated body 22 with the member for electronic devices mentioned above is not specifically limited, The 2nd main surface of the glass substrate 16 of the laminated body 10 by a conventionally well-known method according to the kind of structural member of the member for electronic devices.
  • the electronic device member 20 is formed on the surface of 16b.
  • the electronic device member 20 is not all of the members finally formed on the second main surface 16b of the glass substrate 16 (hereinafter referred to as “all members”), but a part of all members (hereinafter referred to as “parts”). May be referred to as a member.
  • the glass substrate with a partial member peeled from the resin layer 14 can be used as a glass substrate with all members (corresponding to an electronic device described later) in the subsequent steps.
  • the other electronic device member may be formed in the peeling surface (1st main surface 16a) in the glass substrate with all the members peeled from the resin layer 14.
  • FIG. Moreover, an electronic device can also be manufactured by assembling a laminate with all members and then peeling the support plate 12 from the laminate with all members. Furthermore, it can also assemble using two laminated bodies with all members, and can peel the 2 support plates 12 from the laminated body with all members, and can manufacture the glass substrate with a member which has two glass substrates. .
  • the organic EL structure is formed on the surface of the laminate 10 opposite to the resin layer 14 side of the glass substrate 16 (corresponding to the second main surface 16b of the glass substrate 16).
  • Forming a transparent electrode depositing a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, etc. on the surface on which the transparent electrode is formed, forming a back electrode, sealing plate
  • Various layer formation and processing such as sealing using, are performed. Specific examples of the layer formation and processing include film formation processing, vapor deposition processing, sealing plate adhesion processing, and the like.
  • a TFT-LCD when manufacturing a TFT-LCD, it is formed on the second main surface 16b of the glass substrate 16 of the laminate 10 by a general film forming method such as a CVD method and a sputtering method using a resist solution.
  • a general film forming method such as a CVD method and a sputtering method using a resist solution.
  • Various processes such as a CF forming process for forming a color filter (CF) and a laminating process for laminating a laminated body with TFT obtained in the TFT forming process and a laminated body with CF obtained in the CF forming process are used.
  • CF color filter
  • laminating process for laminating a laminated body with TFT obtained in the TFT forming process and
  • the TFT and the CF are formed on the second main surface 16b of the glass substrate 16 by using a well-known photolithography technique, etching technique, or the like. At this time, a resist solution is used as a coating solution for pattern formation.
  • a cleaning method known dry cleaning or wet cleaning can be used.
  • the thin film transistor forming surface of the laminated body with TFT and the color filter forming surface of the laminated body with CF are opposed to each other, and are bonded using a sealant (for example, an ultraviolet curable sealant for cell formation).
  • a sealant for example, an ultraviolet curable sealant for cell formation.
  • a liquid crystal material is injected into a cell formed by the laminate with TFT and the laminate with CF.
  • the method for injecting the liquid crystal material include a reduced pressure injection method and a drop injection method.
  • the separation step is a glass in which the electronic device member 20 is laminated from the laminate 22 with the electronic device member obtained in the member forming step, using the interface between the resin layer 14 and the glass substrate 16 or the resin layer 14 as a release surface.
  • This is a step of separating the substrate 16 (the glass substrate with a member) and the support plate 12 to obtain the member-equipped glass substrate 24 including the electronic device member 20 and the glass substrate 16.
  • the resin may or may not adhere to the first main surface 16a of the separated glass substrate 24 with a member.
  • the peeling surface is the interface between the first main surface 16a of the glass substrate 16 and the resin layer 14, the resin does not adhere to the first main surface 16a of the glass substrate 24 with a member.
  • the peeling surface is inside the resin layer 14 (that is, when peeling occurs due to cohesive failure of the resin layer), the resin adheres to the first main surface 16a of the glass substrate 24 with a member.
  • interfacial peeling and cohesive fracture peeling occur partially, a portion where the resin is attached to the first main surface 16a of the glass substrate with member 24 and a portion where the resin is not attached are generated.
  • the support plate 12 adheres to the surface where the resin layer 14 of the separated support plate 12 was present.
  • the peeling surface is the interface between the first main surface 16a of the glass substrate 16 and the resin layer 14
  • the support plate 12 is provided with a resin having substantially the same structure as the support plate 18 with the resin layer.
  • the support plate has a resin attached to almost the entire surface in contact with the resin layer 14, and there are few surfaces to which no resin is attached.
  • FIG. 2D shows a case where the resin layer 14 is coherently broken, and a part of the resin of the resin layer 14 is attached to the surface of the glass substrate 16 in contact with the resin layer 14.
  • the method for peeling the glass substrate 16 and the support plate 12 is not particularly limited. Specifically, for example, a sharp blade-like object is inserted into the interface between the glass substrate 16 and the resin layer 14 and given a trigger for peeling, and then the peeling is performed by spraying a mixed fluid of water and compressed air. can do.
  • the electronic device member-attached laminate 22 is placed on the surface plate so that the support plate 12 is on the upper side and the electronic device member 20 side is on the lower side, and the electronic device member 20 side is vacuum-adsorbed on the surface plate. (In the case where support plates are laminated on both surfaces, the steps are sequentially performed). In this state, the blade is first inserted into the glass substrate 16-resin layer 14 interface.
  • the support plate 12 side is sucked 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.
  • an air layer is formed on the interface between the resin layer 14 and the glass substrate 16 or on the cohesive failure surface of the resin layer 14, and the air layer spreads over the entire interface or cohesive failure surface, so that the support plate 12 can be easily peeled off. it can.
  • the support plate 12 can be laminated
  • the support plate 12 to which the resin layer is attached is used as the support plate 18 with the resin layer, and newly
  • the laminated body 10 can be manufactured similarly to the above. Further, in the case of the support plate 12 separated by cohesive failure of the resin layer, the attached resin is removed to form a support plate 12 to which no resin is attached, and the support plate 12 to which this resin is not attached is used.
  • the laminated body 10 can be newly manufactured similarly to the above. As a manufacturing method of this new laminated body 10, the manufacturing method of this invention mentioned above is preferable.
  • the cleaning treatment step is a step of performing a cleaning treatment on the peeling surface (first main surface 16a) of the glass substrate 16 in the member-attached glass substrate 24 obtained in the separation step.
  • This step it is possible to remove impurities such as resin and resin layer adhering to the release surface, metal pieces and dust generated in the member forming step adhering to the release surface, and improving the cleanliness of the release surface. Can be maintained.
  • the tackiness of a retardation film, a polarizing film or the like attached to the release surface of the glass substrate 16 is improved. More specifically, by performing this step, as shown in FIG. 2E, a part of the resin layer adhering to the surface of the glass substrate 16 in FIG. 2D is removed. .
  • the cleaning treatment method is not particularly limited as long as the resin or dust attached to the release surface can be removed.
  • a method of thermally decomposing the deposit there are a method of thermally decomposing the deposit, a method of removing impurities on the peeled surface by plasma irradiation or light irradiation (for example, UV irradiation treatment), and a cleaning method using a solvent.
  • a cleaning method using a solvent is preferable in terms of more excellent impurity removability.
  • an optimal solvent is appropriately selected depending on the type of resin constituting the resin layer to be used.
  • the cleaning treatment is preferably performed using a chemical solution containing a solvent having an sp value, that is, a solubility parameter of 7 to 15 (unit: cal 1/2 cm ⁇ 3/2 ). More specifically, it is preferable to use a chemical solution containing methanol, ethanol, propanol, acetone, xylene, hexane, isoparaffin and the like. Furthermore, it is preferable to use a cleaning solution containing an alcohol-based cleaning solution (for example, methanol, ethanol, propanol) from the viewpoint of environmental load. These solvents are used alone or in combination. In addition, you may implement sealing and a masking process so that the member 20 for electronic devices may not contact a solvent as needed. It is also desirable to carry out a solvent removal process such as air blowing or heat drying.
  • the above-described method for manufacturing the glass substrate 24 with a member is suitable for manufacturing a small display device used for a mobile terminal such as a mobile phone or a PDA.
  • the display device is mainly an LCD or an OLED, and the LCD includes a TN type, STN type, FE type, TFT type, MIM type, IPS type, VA type, and the like.
  • the present invention can be applied to both passive drive type and active drive type display devices.
  • a panel for a display device having a glass substrate and a member for a display device a solar cell having a glass substrate and a member for a solar cell, a glass substrate and a member for a thin film secondary battery.
  • a thin film secondary battery an electronic component having a glass substrate and an electronic device member.
  • the display device panel include a liquid crystal panel, an organic EL panel, a plasma display panel, a field emission panel, and the like.
  • a glass plate made of non-alkali borosilicate glass (length 200 mm, width 200 mm, plate thickness 0.3 mm, linear expansion coefficient 38 ⁇ 10 ⁇ 7 / The product name “AN100” manufactured by Asahi Glass Co., Ltd. was used. Further, as the support plate, a glass plate made of non-alkali borosilicate glass (240 mm long, 240 mm wide, 0.4 mm thick, linear expansion coefficient 38 ⁇ 10 ⁇ 7 / ° C., trade name “AN100” manufactured by Asahi Glass Co., Ltd.) It was used.
  • the obtained reaction solution was diluted by adding 150 parts by mass of toluene, two layers were separated. The lower sodium hydroxide aqueous solution layer was removed with a separatory funnel. After washing with water until the pH of the upper toluene layer became 7 or less, it was filtered with a membrane filter having a pore diameter of 0.5 micrometers. The organic solvent was removed from the obtained liquid by heating under reduced pressure at 70 ° C. to obtain a curable silicone resin (S1).
  • the obtained curable silicone resin (S1) had a weight average molecular weight (in terms of polystyrene) of 55000 by GPC (gel permeation chromatography).
  • Curable silicone resins (S2) to (S5) and production of each liquid material
  • the curable silicone resins (S2) to (S5) are shown in Table 1 in the same manner as in Production Example 1. Manufactured at a composition ratio. Subsequently, the curable silicone resins (S2) to (S5) obtained were dissolved in 1-methoxy-2-propanol acetate to prepare liquid materials each containing the curable silicone resins (S2) to (S5).
  • silanol group means whether or not silanol groups are contained in the curable silicone resins (S1) to (S5).
  • mol% of the (B-2) unit was calculated as “0”.
  • a support plate having a thickness of 0.4 mm was cleaned with pure water, and further cleaned by UV cleaning.
  • a liquid material containing the curable silicone resin (S1) was applied onto the first main surface of the support plate using a spin coater (coating amount 30 g / m 2 ).
  • this was heat-cured at 180 ° C. for 10 minutes in the air to remove the solvent in the composition layer on the support plate. Thereafter, it was further heat-cured at 450 ° C. for 60 minutes in the air to form a resin layer having a thickness of 2 ⁇ m on the first main surface of the support plate.
  • the glass substrate and the resin layer surface of the support plate are bonded together by vacuum press at room temperature, and then heat treatment is performed at 350 ° C. for 10 minutes, and the end of the support plate is cut and removed to the same dimensions as the glass substrate.
  • the laminate A was obtained by chamfering. In the obtained laminate A, the support plate and the glass substrate were in close contact with the resin layer without generating bubbles, no distorted defects, and good smoothness.
  • the laminate A was heated at 450 ° C. for 60 minutes in the atmosphere and cooled to room temperature.
  • changes in appearance such as separation of the support plate and glass substrate of the laminate A, foaming and whitening of the resin layer were recognized. I could't.
  • glass The vacuum suction pad was adsorbed on the surface of the substrate and the support plate that were not the peeling surfaces, and an external force was applied in the direction in which the glass substrate and the support plate were separated from each other, thereby separating the glass substrate and the support plate without damaging them.
  • the cutter was inserted while spraying a static eliminating fluid on the interface from an ionizer (manufactured by Keyence Corporation). Specifically, the vacuum suction pad was pulled up while spraying a static eliminating fluid continuously from the ionizer toward the formed gap.
  • the main part of the resin layer is separated from the glass substrate together with the support plate, and as a result, the peel strength (y) at the interface between the support plate layer and the resin layer is determined as the peel strength at the interface between the resin layer and the glass substrate (x Or higher than the cohesive fracture strength (z) of the resin layer.
  • the separated surface of the separated glass substrate was cleaned by brushing with an alcohol solution (manufactured by Nippon Alcohol Sales Co., Neocor R7) for 1 minute, and then air blown to clean it.
  • the alcohol solution contains 86.6% by mass of ethanol, 9.5% by mass of normal propyl alcohol (NPA), 2.6% by mass of methanol, and 1.5% by mass of isopropyl alcohol (IPA).
  • NPA normal propyl alcohol
  • IPA isopropyl alcohol
  • Example 2 In the same manner as in Example 1, a 1.5 ⁇ m thick resin layer made of a heat-cured product of the curable silicone resin (S2) was formed on the first main surface of the support plate. Subsequently, a layered product B was obtained in the same manner as in Example 1. In the obtained laminate B, the support plate and the glass substrate were in close contact with the resin layer without generating bubbles, no distortion defects, and good smoothness. Next, when the laminate B was subjected to the same heat treatment as in Example 1, no change in appearance such as separation of the support plate of the laminate B and the glass substrate, foaming or whitening of the resin layer was observed. And the laminated body B was isolate
  • Example 3 In the same manner as in Example 1, a 2 ⁇ m thick resin layer made of a heat-cured product of the curable silicone resin (S3) was formed on the first main surface of the support plate. Subsequently, a laminate C was obtained in the same manner as in Example 1. In the obtained laminate C, the support plate and the glass substrate were in close contact with the resin layer without generating bubbles, no distorted defects, and good smoothness. Next, when the laminate C was subjected to the same heat treatment as in Example 1, no change in appearance such as separation of the support plate of the laminate C and the glass substrate, foaming or whitening of the resin layer was observed. And the laminated body C was isolate
  • Example 4 an OLED is manufactured using the laminate A obtained in Example 1. First, silicon nitride, silicon oxide, and amorphous silicon are formed in this order on the second main surface of the glass substrate in the laminate A by plasma CVD. Next, low concentration boron is injected into the amorphous silicon layer by an ion doping apparatus, and a dehydrogenation process is performed by heating at 450 ° C. for 60 minutes in a nitrogen atmosphere. Next, the amorphous silicon layer is crystallized by a laser annealing apparatus.
  • low concentration phosphorus is implanted into the amorphous silicon layer by an etching and ion doping apparatus using a photolithography method, thereby forming N-type and P-type TFT areas.
  • a silicon oxide film is formed on the second main surface side of the glass substrate by a plasma CVD method to form a gate insulating film, then molybdenum is formed by a sputtering method, and etching is performed using a photolithography method.
  • a gate electrode is formed.
  • high concentration boron and phosphorus are implanted into desired areas of the N-type and P-type by photolithography and an ion doping apparatus, thereby forming a source area and a drain area.
  • an interlayer insulating film is formed on the second main surface side of the glass substrate by silicon oxide film formation by plasma CVD, and a TFT electrode is formed by aluminum film formation by sputtering and etching using photolithography.
  • a passivation layer is formed by film formation of nitrogen silicon by a plasma CVD method.
  • an ultraviolet curable resin is applied to the second main surface side of the glass substrate, and a planarization layer and a contact hole are formed by photolithography.
  • a film of indium tin oxide is formed by a sputtering method, and a pixel electrode is formed by etching using a photolithography method.
  • a laminate A (hereinafter referred to as panel A) having the organic EL structure on the glass substrate is an electronic device of the present invention. It is a laminated body with a member for use (panel for display apparatuses with a support plate). Subsequently, after the panel A sealing body side is vacuum-adsorbed on the surface plate, a stainless steel knife having a thickness of 0.1 mm is inserted into the interface between the glass substrate and the resin layer at the corner of panel A, and the glass substrate Gives the interface between the resin layer and the resin layer.
  • a suction pad is raised.
  • the blade is inserted while spraying a static eliminating fluid on the interface from an ionizer (manufactured by Keyence Corporation).
  • the vacuum suction pad is pulled up while the static elimination fluid is continuously sprayed from the ionizer toward the formed gap.
  • the separation surface of the glass substrate separated by the same method as in Example 1 was cleaned, the separated glass substrate was cut using a laser cutter or a scribe-break method, and divided into a plurality of cells.
  • the glass substrate on which the EL structure is formed and the counter substrate are assembled, and a module forming process is performed to manufacture an OLED.
  • the OLED obtained in this way does not have a problem in characteristics.
  • Example 5 an LCD is manufactured using the laminate A obtained in Example 1.
  • two laminates A are prepared, and silicon nitride, silicon oxide, and amorphous silicon are formed in this order on the second main surface of the glass substrate in one laminate A1 by plasma CVD.
  • low concentration boron is injected into the amorphous silicon layer by an ion doping apparatus, and a dehydrogenation process is performed by heating at 450 ° C. for 60 minutes in a nitrogen atmosphere.
  • the amorphous silicon layer is crystallized by a laser annealing apparatus.
  • low concentration phosphorus is implanted into the amorphous silicon layer by an etching and ion doping apparatus using a photolithography method, thereby forming N-type and P-type TFT areas.
  • a silicon oxide film is formed on the second main surface side of the glass substrate by a plasma CVD method and a gate insulating film is formed, molybdenum is formed by a sputtering method, and the gate is etched by photolithography. An electrode is formed.
  • high concentration boron and phosphorus are implanted into desired areas of the N-type and P-type by photolithography and an ion doping apparatus, thereby forming a source area and a drain area.
  • an interlayer insulating film is formed on the second main surface side of the glass substrate by silicon oxide film formation by plasma CVD, and a TFT electrode is formed by aluminum film formation by sputtering and etching using photolithography.
  • a passivation layer is formed by film formation of nitrogen silicon by a plasma CVD method.
  • an ultraviolet curable resin is applied to the second main surface side of the glass substrate, and a planarization layer and a contact hole are formed by photolithography.
  • a film of indium tin oxide is formed by a sputtering method, and a pixel electrode is formed by etching using a photolithography method.
  • the other laminate A2 is heat-treated at 450 ° C. for 60 minutes in an air atmosphere.
  • a chromium film is formed on the second main surface of the glass substrate in the laminate A by a sputtering method, and a light-shielding layer is formed by etching using a photolithography method.
  • a color resist is applied to the second main surface side of the glass substrate by a die coating method, and a color filter layer is formed by a photolithography method and heat curing.
  • a film of indium tin oxide is formed by a sputtering method to form a counter electrode.
  • an ultraviolet curable resin liquid is applied to the second main surface side of the glass substrate by a die coating method, and columnar spacers are formed by a photolithography method and thermal curing.
  • a polyimide resin solution is applied by a roll coating method, an alignment layer is formed by thermosetting, and rubbing is performed.
  • the sealing resin liquid is drawn in a frame shape by the dispenser method, and after the liquid crystal is dropped in the frame by the dispenser method, two laminates A are used by using the laminate A1 in which the pixel electrodes are formed as described above.
  • the second principal surface sides of the glass substrates are bonded together, and an LCD panel is obtained by ultraviolet curing and thermal curing.
  • the second main surface of the laminate A1 is vacuum-adsorbed on a surface plate, and a stainless steel knife having a thickness of 0.1 mm is inserted into the interface between the glass substrate and the resin layer at the corner of the laminate A2, and the glass substrate
  • a stainless steel knife having a thickness of 0.1 mm is inserted into the interface between the glass substrate and the resin layer at the corner of the laminate A2, and the glass substrate
  • the blade is inserted while spraying a static eliminating fluid on the interface from an ionizer (manufactured by Keyence Corporation).
  • the vacuum suction pad is pulled up while the static elimination fluid is continuously sprayed from the ionizer toward the formed gap.
  • the second main surface of the glass substrate on which the color filter is formed on the first main surface is vacuum-adsorbed on the surface plate, and a thickness of 0. 0 is formed at the interface between the glass substrate and the resin layer at the corner portion of the laminate A1.
  • a 1 mm stainless steel blade is inserted to give a trigger for peeling between the first main surface of the glass substrate and the peelable surface of the resin layer.
  • sucking the 2nd main surface of the support substrate of laminated body A1 with a vacuum suction pad a suction pad is raised.
  • only the LCD cell is left on the surface plate, and the support plate to which the resin layer is fixed can be peeled off.
  • the peeled surface is cleaned by the same method as in Example 1.
  • a plurality of LCD cells composed of a glass substrate having a thickness of 0.1 mm are obtained.
  • Example 6 an OLED is manufactured using the laminate A obtained in Example 1.
  • a film of molybdenum is formed on the second main surface of the glass substrate in the stacked body A by a sputtering method, and a gate electrode is formed by etching using a photolithography method.
  • a silicon nitride film is further formed on the second main surface side of the glass substrate by a plasma CVD method to form a gate insulating film, and then an indium gallium zinc oxide film is formed by a sputtering method to perform a photolithography method.
  • An oxide semiconductor layer is formed by the etching used.
  • a silicon nitride film is further formed on the second main surface side of the glass substrate by plasma CVD to form a channel protective layer, and then molybdenum is formed by sputtering and etching using a photolithography method is performed. Thus, a source electrode and a drain electrode are formed. Next, heat treatment is performed in the atmosphere at 450 ° C. for 60 minutes. Next, a silicon nitride film is further formed on the second main surface side of the glass substrate by a plasma CVD method to form a passivation layer, followed by an indium tin oxide film formed by a sputtering method and etching using a photolithography method. Thus, a pixel electrode is formed.
  • a laminate A (hereinafter referred to as panel A) having the organic EL structure on the glass substrate is an electronic device of the present invention. It is a laminated body with a member for use (panel for display apparatuses with a support plate). Subsequently, after the panel A sealing body side is vacuum-adsorbed on the surface plate, a stainless steel knife having a thickness of 0.1 mm is inserted into the interface between the glass substrate and the resin layer at the corner of panel A, and the glass substrate Gives the interface between the resin layer and the resin layer.
  • a suction pad is raised.
  • the blade is inserted while spraying a static eliminating fluid on the interface from an ionizer (manufactured by Keyence Corporation).
  • the vacuum suction pad is pulled up while the static elimination fluid is continuously sprayed from the ionizer toward the formed gap.
  • the separation surface of the glass substrate separated by the same method as in Example 1 was cleaned, the separated glass substrate was cut using a laser cutter or a scribe-break method, and divided into a plurality of cells.
  • the glass substrate on which the EL structure is formed and the counter substrate are assembled, and a module forming process is performed to manufacture an OLED.
  • the OLED obtained in this way does not have a problem in characteristics.
  • ⁇ Comparative Example 1> In the same manner as in Example 1, a 1 ⁇ m-thick resin layer made of a heat-cured product of the curable silicone resin (S4) was formed on the first main surface of the support plate. Subsequently, when the glass substrate and the resin layer surface of the support plate were vacuum-pressed at room temperature in the same manner as in Example 1, the resin layer was hard and partially laminated on the glass substrate and the resin layer surface of the support plate. The part which was not seen was seen. Then, when heat processing were performed for 10 minutes at 350 degreeC, it isolate
  • ⁇ Comparative example 2> In the same manner as in Example 1, a 1 ⁇ m thick resin layer made of a heat-cured product of the curable silicone resin (S5) was formed on the first main surface of the support plate. The surface of the resin layer was so flat that unevenness was confirmed by visual observation. Subsequently, when the glass substrate and the resin layer surface of the support plate were vacuum-pressed at room temperature in the same manner as in Example 1, the glass substrate and the entire resin layer surface of the support plate were separated to form a laminate. There wasn't.
  • ⁇ Comparative Example 3> In the same manner as in Example 1, a 1 ⁇ m-thick resin layer made of a heat-cured product of the curable silicone resin (S6) was formed on the first main surface of the support plate. Subsequently, when the glass substrate and the resin layer surface of the support plate were vacuum-pressed at room temperature in the same manner as in Example 1, the resin layer was hard and partially laminated on the glass substrate and the resin layer surface of the support plate. The part which was not seen was seen. Then, when heat processing were performed for 10 minutes at 350 degreeC, it isolate
  • the surface of the glass substrate (length 200 mm, width 200 mm, thickness 0.3 mm) to be brought into contact with the silicone resin layer is cleaned by pure water cleaning, UV cleaning, etc.
  • the surface of the support plate where the silicone resin layer is formed was cleaned by pure water cleaning, UV cleaning, etc.
  • the surface of the support plate where the silicone resin layer is formed was cleaned by pure water cleaning, UV cleaning, etc.
  • the surface of the support plate where the silicone resin layer is formed and glass
  • the substrate was bonded with a vacuum press at room temperature to obtain a glass laminate P having an addition polymerization type silicone resin layer.
  • the 2nd main surface of the glass substrate in the laminated body P it formed into a film in order of the silicon nitride, the silicon oxide, and the amorphous silicon by plasma CVD method.
  • heat treatment was performed at 450 ° C. for 60 minutes in a nitrogen atmosphere to perform dehydrogenation treatment.
  • Examples 4 to 6 are laminates having the resin layer of the present invention, no influence on the device characteristics is observed even when the electronic device is formed at a high temperature. This is presumably because there was no influence of volatile components in the resin layer of the laminate.
  • Comparative Example 4 which is not a resin layer of the present invention, foaming is observed when an electronic device is formed at a high temperature, and it is considered that a volatile component is generated. Moreover, the resin adhering to the glass substrate cannot be removed.

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Abstract

La présente invention porte sur un stratifié comprenant une couche de plaque de support, une couche de résine et une couche de substrat de verre dans cet ordre, la résistance au pelage (y) sur l'interface entre la couche de plaque de support et la couche de résine étant supérieure à la résistance au pelage (x) sur l'interface entre la couche de résine et le substrat de verre ou à la résistance à la rupture cohésive (z) de la couche de résine, une résine contenue dans la couche de résine étant une résine de silicone réticulée, la résine de silicone réticulée contenant une unité organosiloxy (A-1) représentée par la formule (1) et une unité organosiloxy (B-1) représentée par la formule (2), le rapport du total de la somme de la teneur du composant (A-1) et de la teneur du composant (B-1) (à savoir, (A-1) + (B-1)) à la teneur totale de toutes les unités organosiloxy étant de 70 à 100 % en moles, et le rapport de la teneur du composant (A-1) au total de la somme de la teneur du composant (A-1) et de la teneur du composant (B-1) étant de 15 à 50 % en moles dans la résine de silicone réticulée. (Dans la formule (1), R1 représente un atome d'hydrogène ou un groupe alkyle ayant 1 à 4 atomes de carbone. Dans la formule (2), R6 et R7 représentent indépendamment un groupe alkyle ayant 1 à 4 atomes de carbone).
PCT/JP2012/076641 2011-10-18 2012-10-15 Stratifié, procédé de fabrication de stratifié et procédé de fabrication d'un substrat de verre ayant un élément pour des dispositifs électroniques attachés à celui-ci WO2013058217A1 (fr)

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KR1020147010179A KR101973826B1 (ko) 2011-10-18 2012-10-15 적층체, 적층체의 제조 방법 및 전자 디바이스용 부재가 부착된 유리 기판의 제조 방법
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US9340443B2 (en) 2012-12-13 2016-05-17 Corning Incorporated Bulk annealing of glass sheets
JP2017030324A (ja) * 2015-08-06 2017-02-09 旭硝子株式会社 ガラス積層体およびその製造方法
US9889635B2 (en) 2012-12-13 2018-02-13 Corning Incorporated Facilitated processing for controlling bonding between sheet and carrier
US10014177B2 (en) 2012-12-13 2018-07-03 Corning Incorporated Methods for processing electronic devices
US10046542B2 (en) 2014-01-27 2018-08-14 Corning Incorporated Articles and methods for controlled bonding of thin sheets with carriers
US10086584B2 (en) 2012-12-13 2018-10-02 Corning Incorporated Glass articles and methods for controlled bonding of glass sheets with carriers
US10510576B2 (en) 2013-10-14 2019-12-17 Corning Incorporated Carrier-bonding methods and articles for semiconductor and interposer processing
US10543662B2 (en) 2012-02-08 2020-01-28 Corning Incorporated Device modified substrate article and methods for making
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US11097509B2 (en) 2016-08-30 2021-08-24 Corning Incorporated Siloxane plasma polymers for sheet bonding
US11167532B2 (en) 2015-05-19 2021-11-09 Corning Incorporated Articles and methods for bonding sheets with carriers
US11192340B2 (en) 2014-04-09 2021-12-07 Corning Incorporated Device modified substrate article and methods for making
US11331692B2 (en) 2017-12-15 2022-05-17 Corning Incorporated Methods for treating a substrate and method for making articles comprising bonded sheets
US11535553B2 (en) 2016-08-31 2022-12-27 Corning Incorporated Articles of controllably bonded sheets and methods for making same
US11905201B2 (en) 2015-06-26 2024-02-20 Corning Incorporated Methods and articles including a sheet and a carrier
US11999135B2 (en) 2017-08-18 2024-06-04 Corning Incorporated Temporary bonding using polycationic polymers
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US10014177B2 (en) 2012-12-13 2018-07-03 Corning Incorporated Methods for processing electronic devices
US10086584B2 (en) 2012-12-13 2018-10-02 Corning Incorporated Glass articles and methods for controlled bonding of glass sheets with carriers
US9340443B2 (en) 2012-12-13 2016-05-17 Corning Incorporated Bulk annealing of glass sheets
US10538452B2 (en) 2012-12-13 2020-01-21 Corning Incorporated Bulk annealing of glass sheets
US9889635B2 (en) 2012-12-13 2018-02-13 Corning Incorporated Facilitated processing for controlling bonding between sheet and carrier
US10510576B2 (en) 2013-10-14 2019-12-17 Corning Incorporated Carrier-bonding methods and articles for semiconductor and interposer processing
JP2015116694A (ja) * 2013-12-17 2015-06-25 旭硝子株式会社 樹脂層付き支持基板の製造方法、ガラス積層体の製造方法、電子デバイスの製造方法
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US11123954B2 (en) 2014-01-27 2021-09-21 Corning Incorporated Articles and methods for controlled bonding of thin sheets with carriers
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US11192340B2 (en) 2014-04-09 2021-12-07 Corning Incorporated Device modified substrate article and methods for making
US11167532B2 (en) 2015-05-19 2021-11-09 Corning Incorporated Articles and methods for bonding sheets with carriers
US11660841B2 (en) 2015-05-19 2023-05-30 Corning Incorporated Articles and methods for bonding sheets with carriers
US11905201B2 (en) 2015-06-26 2024-02-20 Corning Incorporated Methods and articles including a sheet and a carrier
KR20170017729A (ko) 2015-08-06 2017-02-15 아사히 가라스 가부시키가이샤 유리 적층체 및 그의 제조 방법
JP2017030324A (ja) * 2015-08-06 2017-02-09 旭硝子株式会社 ガラス積層体およびその製造方法
KR102526047B1 (ko) * 2015-08-06 2023-04-27 에이지씨 가부시키가이샤 유리 적층체 및 그의 제조 방법
US11097509B2 (en) 2016-08-30 2021-08-24 Corning Incorporated Siloxane plasma polymers for sheet bonding
US11535553B2 (en) 2016-08-31 2022-12-27 Corning Incorporated Articles of controllably bonded sheets and methods for making same
US11999135B2 (en) 2017-08-18 2024-06-04 Corning Incorporated Temporary bonding using polycationic polymers
US11331692B2 (en) 2017-12-15 2022-05-17 Corning Incorporated Methods for treating a substrate and method for making articles comprising bonded sheets
CN111629899A (zh) * 2018-01-17 2020-09-04 Ａｇｃ株式会社 层叠体、层叠体的制造方法和电子设备的制造方法
US12122138B2 (en) 2021-08-03 2024-10-22 Corning Incorporated Siloxane plasma polymers for sheet bonding

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KR20140079783A (ko) 2014-06-27
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TW201318843A (zh) 2013-05-16
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KR101973826B1 (ko) 2019-08-26
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