CN102883879B - Process for producing laminate, and laminate - Google Patents

Process for producing laminate, and laminate Download PDF

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Publication number
CN102883879B
CN102883879B CN201180023392.8A CN201180023392A CN102883879B CN 102883879 B CN102883879 B CN 102883879B CN 201180023392 A CN201180023392 A CN 201180023392A CN 102883879 B CN102883879 B CN 102883879B
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China
Prior art keywords
substrate
resin bed
duplexer
gripper shoe
silicone oil
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CN201180023392.8A
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CN102883879A (en
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江畑研一
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AGC Inc
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Asahi Glass Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/283—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/286—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polysulphones; polysulfides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B9/045—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/546—Flexural strength; Flexion stiffness
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/732—Dimensional properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • B32B2457/12—Photovoltaic modules
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
    • B32B2457/202—LCD, i.e. liquid crystal displays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
    • B32B2457/206—Organic displays, e.g. OLED

Abstract

Provided is a process for producing a laminate which comprises a substrate, a support plate, and a resin layer interposed therebetween, the process comprising the step of forming the resin layer on the support plate and the step of bringing the resin layer into close contact with the substrate so that the substrate is separable from the resin layer. The process may include, before the contact step, a step in which at least one of the surfaces of the substrate and resin layer that are to be close contacted with each other is treated beforehand with a silicone oil or a silane coupling agent. Alternatively, the resin layer is formed from a resin which contains a silicone oil or silane coupling agent in the step of resin layer formation and, thereafter, the substrate and the resin layer are superposed and close contacted in the contact step.

Description

The manufacture method of duplexer and duplexer
Technical field
The present invention relates to manufacture method and the duplexer of duplexer.
Background technology
In recent years, carrying out the slimming of the devices (electronic equipment) such as solar cell (PV), liquid crystal panel (LCD), organic EL panel (OLED), lightweight, carrying out the thin plate of the substrate for these devices.On the other hand, when causing the intensity of substrate not enough because of thin plate, in the manufacturing process of device, the treatability of substrate can reduce.
Therefore, all the time, extensively following methods is adopted: on the substrate thicker than final thickness after forming apparatus component (such as, thin film transistor (TFT)), utilize chemical etching process by substrate thin plate.But, in the method, such as, by the thickness of 1 plate base by 0.7mm thin plate to 0.2mm or 0.1mm time, the more than half of material of original substrate is pruned by etching solution, therefore from the view point of productivity ratio, raw-material service efficiency, is not preferred.
In addition, in the thin plate method of the above-mentioned substrate based on chemical etching, when substrate surface exists fine scar, be that starting point forms fine pit (etch pit) sometimes with scar because of etch processes, become optic defect.
Recently, in order to tackle above-mentioned problem, propose following methods: the duplexer preparing to be laminated with substrate and reinforcement plate, on the substrate of duplexer after forming apparatus component, from strippable substrate reinforcement plate (for example, referring to patent document 1).Reinforcement plate has glass plate and the resin bed be fixed on this glass plate, and resin bed and substrate fit tightly with strippable form.Reinforcement plate, can be stacked with new substrate after strippable substrate, thus recycle as duplexer.
Prior art document
Patent document
Patent document 1: No. 07/018028th, International Publication
Summary of the invention
the problem that invention will solve
But for the duplexer of above-mentioned existing structure, during by reinforcement plate from strippable substrate, the resin bed meeting cohesion failure of reinforcement plate sometimes, on the substrate causing a part for resin bed to be attached to as product side.This is presumably because the condition because of the heating in the manufacturing process of device, chemical liquid process, cause resin bed deterioration sometimes, the intensity that fits tightly of resin bed and substrate rises sometimes.
The present invention carries out in view of above-mentioned problem, its object is to, and provides manufacture method and the duplexer that can suppress the duplexer of resin bed cohesion failure when peeling off resin bed and substrate.
for the scheme of dealing with problems
To achieve these goals, the manufacture method of duplexer of the present invention is the manufacture method of following duplexer:
It is for manufacturing the method for the duplexer having substrate and gripper shoe and be present in the resin bed between them, there is following operation: aforementioned resin layer be formed in the operation in aforementioned gripper shoe and make aforementioned resin layer fit tightly the operation in aforesaid base plate with strippable form
Wherein, before being included in the aforementioned operation fitted tightly to the aforesaid base plate surface that will fit tightly and at least one party on aforementioned resin layer surface in advance by the operation that silicone oil or silane coupler process, or,
In the operation forming aforementioned resin layer, form aforementioned resin layer by the resin comprising silicone oil or silane coupler, then, in the aforementioned operation fitted tightly, make aforesaid base plate and aforementioned resin ply and fit tightly.
In the manufacture method of duplexer of the present invention, preferably, be coated with to the aforesaid base plate surface that will fit tightly and at least one party on aforementioned resin layer surface silicone oil or silane coupler operation and
The operation of process when silicone oil being carried out during coating silicone oil to operation and the silane-coating coupling agent of low molecule quantification treatment, silane coupler being reacted,
Thereafter, in the aforementioned operation fitted tightly, make aforesaid base plate and aforementioned resin ply and fit tightly.In addition, preferably, the aforesaid base plate surface silicone oil that fit tightly or silane coupler implement surface treatment, and the water contact angle being applied with the substrate surface of aforementioned processing is more than 90 °.
In the manufacture method of duplexer of the present invention, preferably, aforementioned resin layer is being formed in the operation in aforementioned gripper shoe, is forming cured resin composition layer on aforementioned gripper shoe surface, then make this hardening resin composition be solidified to form aforementioned resin layer.
In addition, in the manufacture method of duplexer of the present invention, preferably, aforementioned resin layer is formed by silicones.
And then in the manufacture method of duplexer of the present invention, preferably, aforementioned resin layer is formed by the reaction solidfied material of olefinic organic based polysiloxane and organic hydrogen polysiloxanes.
In addition, duplexer of the present invention is following duplexer:
Its resin bed that there is substrate and gripper shoe and be present between them, aforementioned resin layer and aforesaid base plate fit tightly with strippable form, the mode of the peel strength that aforementioned resin layer is greater than between aforementioned resin layer and aforesaid base plate with the peel strength between them in aforementioned gripper shoe is fixed
The aforesaid base plate surface fitted tightly and at least one party on aforementioned resin layer surface are by being formed with the surface of silicone oil or silane coupler process in advance, or aforementioned resin layer is the resin bed formed by the resin comprising silicone oil or silane coupler.
In duplexer of the present invention, preferably, the substrate surface fitted tightly in aforementioned resin layer surface uses silicone oil or silane coupler to implement surface-treated surface.In addition, preferably, the aforementioned water contact angle implementing surface-treated substrate surface is more than 90 °.
In addition, in duplexer of the present invention, preferably, aforementioned resin layer is formed by silicones.
And then in duplexer of the present invention, preferably, aforementioned resin layer is formed by the reaction solidfied material of olefinic organic based polysiloxane and organic hydrogen polysiloxanes.
the effect of invention
According to the present invention, manufacture method and the duplexer that can suppress the duplexer of resin bed cohesion failure when peeling off resin bed and substrate can be provided.
Accompanying drawing explanation
Fig. 1 is the partial side view of an example of duplexer of the present invention.
Detailed description of the invention
Below, be described for implementing embodiments of the present invention with reference to accompanying drawing, but the present invention is by the restriction of following embodiment, various distortion and displacement can be applied to following embodiment not exceeding in scope of the present invention.
It should be noted that, in the present invention, resin bed is fixed and refers to that the peel strength between resin bed and gripper shoe is greater than the state of the peel strength between resin bed and substrate on the supporting plate.
(the first embodiment)
Fig. 1 is the partial side view of an example of duplexer of the present invention.As shown in Figure 1, for there is the duplexer of substrate 20 and gripper shoe 31 and the resin bed between them 32 in duplexer 10.Resin bed 32 is fixed in gripper shoe 31, and fits tightly the first interarea 201 in substrate 20 with strippable form.Gripper shoe 31 and resin bed 32, in the operation manufacturing the devices (electronic equipment) such as liquid crystal panel, work as the reinforcement plate 30 strengthening substrate 20.
Use this duplexer 10 until the midway of manufacturing process of device.That is, this duplexer 10 is used until form the device components such as thin film transistor (TFT) on the base plate 20.Thereafter, reinforcement plate 30 is peeled off from substrate 20, can not become the component of constituent apparatus.The reinforcement plate 30 peeled off from substrate 20 can be stacked with new substrate 20, thus recycle as duplexer 10.Below, each formation is described in detail.
First, substrate 20 is described.
Substrate 20 forming apparatus component and constituent apparatus on the second interarea 202.Herein, device component refers to the component at least partially of constituent apparatus.As the object lesson of device component, thin film transistor (TFT) (TFT), colour filter (CF) can be listed.As device, solar cell (PV), liquid crystal panel (LCD), organic EL panel (OLED) etc. can be exemplified.
The kind of substrate 20 can be common substrate, such as, can be silicon wafer, glass substrate, resin substrate or metal substrate such as stainless steel (SUS) substrate, copper base etc.Among them, preferred glass substrate.This is because the chemical proofing of glass substrate, resistance to excellent moisture permeability, and percent thermal shrinkage is low.As the index of percent thermal shrinkage, use the linear expansion coefficient specified in JIS R 3102-1995.
When the linear expansion coefficient of substrate 20 is large, the most heat tracing process of the manufacturing process due to device, therefore easily produces various unfavorable condition.Such as, when forming TFT on the base plate 20, if cool the substrate 20 being formed with TFT under heating, then have and cause the position of TFT to depart from excessive worry because of the thermal contraction of substrate 20.
Glass substrate is by frit melting and melten glass is configured as tabular and obtains.This manufacturing process can be usual way, such as, can use float glass process, fusion method, slot draw method, Fourcault process (Fourcault process), Lu Baifa (Lubbers process) etc.In addition, especially the glass substrate of thinner thickness can (horizontal sheet process) be shaped and obtain by the following method: by being temporarily configured as the glass heats of tabular to the temperature that can be shaped, stretching and make its thinning by means such as extensions.
The glass of glass substrate is not particularly limited, preferred alkali-free glass, Pyrex, soda-lime glass, high silica glass, chemically reinforced glass, other take silica as the oxide based glass of main component.As oxide based glass, be preferably the glass of 40 ~ 90 quality % in the content of the silica of oxide conversion.
As the glass of glass substrate, adopt and be suitable for the kind of device, the glass of its manufacturing process.Such as, because the stripping of alkali metal component easily impacts liquid crystal, therefore the glass substrate of liquid crystal panel is formed by the glass being substantially free of alkali metal component (alkali-free glass).Like this, the glass of glass substrate is suitably selected based on the kind of applied device and its manufacturing process.
The thickness of glass substrate is not particularly limited, from slimming and/or the light-weighted viewpoint of glass substrate, is usually less than 0.8mm, be preferably below 0.3mm, more preferably below 0.15mm.When more than 0.8mm, the slimming of glass substrate and/or light-weighted requirement cannot be met.And when below 0.3mm, good flexibility can be given to glass substrate.When below 0.15mm, glass substrate can be coiled into tubular.In addition, from being easy to manufacture glass substrate, being easy to the reasons such as process glass substrate, the thickness of glass substrate is preferably more than 0.03mm.
The kind of the resin of resin substrate is not particularly limited.Specifically, pet resin, polycarbonate resin, polyimide resin, fluororesin, polyamide, Nomex resin, polyethersulfone resin, polyether ketone resin, polyether-ether-ketone resin, PEN resin, polyacrylics, various liquid crystal polymer resin, cyclic olefin resins, silicones etc. can be exemplified.Wherein, resin substrate can be transparent, also can be opaque.In addition, resin substrate can also be the resin substrate that surface is formed with the functional layers such as protective layer.
It should be noted that, substrate 20 can be formed by more than 2 layers, and in this case, the material forming each layer can be same material, also can be not same material.In addition, in this case, " thickness of substrate 20 " means the gross thickness of all layers in substrate.From slimming and/or the light-weighted viewpoint of substrate, the thickness of substrate 20 is usually less than 1.0mm, is preferably below 0.5mm, more preferably below 0.3mm.In addition, from the reason being easy to manufacture substrate and be easy to treatment substrate etc., more than 0.01mm is preferably.
Then, gripper shoe 31 is described.
Gripper shoe 31 and resin bed 32 acting in conjunction, support and strengthen substrate 20, preventing the distortion of substrate 20, damage, breakage etc. in the manufacturing process of device.In addition, one of object of gripper shoe 31 is used also to be, when the substrate 20 using the existing substrate of Thickness Ratio thin, make the duplexer 10 identical with the thickness of existing substrate, thus manufacturing technology, the manufacturing equipment of the substrate being suitable for existing thickness can be used in the manufacturing process of device.
As gripper shoe 31, such as, can use the metallic plates etc. such as glass plate, resin plate or stainless steel (SUS) plate.In the manufacturing process of device with in heat treated situation, gripper shoe 31 is preferably formed with the material that the difference of the linear expansion coefficient with substrate 20 is little, is more preferably formed with the material identical with substrate 20.When substrate 20 is glass substrate, gripper shoe 31 is preferably glass plate.It is particularly preferably the glass plate formed by the glass material identical with glass substrate.
The thickness of gripper shoe 31 can be thicker than substrate 20, also can be thinner than substrate 20.Preferably, the thickness of gripper shoe 31 is selected according to the thickness of the thickness of substrate 20, the thickness of resin bed 32 and duplexer 10.Such as, the manufacturing process of existing device is the patten's design of the substrate processing thickness 0.5mm, when the thickness of substrate 20 and the thickness sum of resin bed 32 are 0.1mm, the thickness of gripper shoe 31 is set to 0.4mm.The thickness of gripper shoe 31 is preferably 0.08 ~ 5.0mm under normal conditions, is more preferably 0.2 ~ 5.0mm, more preferably 0.2 ~ 1.0mm.
When gripper shoe 31 is glass plate, from the reason being easy to process, being difficult to break etc., the thickness of glass plate is preferably more than 0.08mm.In addition, when hope is peeled off after device component is formed, have the flexible and reason of such rigidity of not breaking of appropriateness, the thickness of glass plate is preferably below 1.0mm.
Substrate 20 is preferably 500 × 10 with the difference of the average coefficient of linear expansion of gripper shoe 31 at 25 ~ 300 DEG C (hreinafter referred to as " average coefficient of linear expansion ") -7/ DEG C below, be more preferably 300 × 10 -7/ DEG C below, more preferably 200 × 10 -7/ DEG C below.When difference is excessive, there is following possibility: when carrying out heating cooling in the manufacturing process of device, the violent warpage of duplexer 10 or substrate 20 are peeled off with reinforcement plate 30.When the material of substrate 20 is identical with the material of gripper shoe 31, the generation of this problem can be suppressed.
Then, resin bed 32 is described.
Resin bed 32 is fixed in gripper shoe 31, in addition, fits tightly in substrate 20 with strippable form.Resin bed 32 prevents from departing from until the position of the substrate 20 carried out till strip operation, and is easily peeled off from substrate 20 by strip operation, prevents substrate 20 grade damaged due to strip operation.
The size of resin bed 32 is not particularly limited.The size of resin bed 32 can be larger than substrate 20, gripper shoe 31, also can be less than it.
Preferably, surperficial below the 321(of the substrate side of resin bed 32, also referred to as " fitting tightly face 321 ") be attached at surperficial below the 201(of substrate 20 by resulting from the power of the Van der Waals force between molecular solids, also referred to as " fitting tightly face 201 "), instead of by as common adhesive have bonding force attaching.This is because can easily peel off.In the present invention, the character that can easily peel off of this resin layer surface is called fissility.
On the other hand, the adhesion on the surface of resin bed 32 pairs of gripper shoes 31 is relatively higher than the adhesion on the surface 201 of resin bed 32 pairs of substrates 20.Therefore, the peel strength between resin bed 32 and gripper shoe 31 is higher than the peel strength between resin bed 32 and substrate 20.In the present invention, the combination of resin layer surface to substrate surface is called and fits tightly, will be called fixing to the combination on gripper shoe surface.Preferably combine with bonding force, bonding force between resin bed 32 and gripper shoe 31.But being not limited to these modes, as long as relatively higher to the adhesion fitting tightly face 201 than resin bed 32, then also can attaching by resulting from the power of above-mentioned Van der Waals force between resin bed 32 and gripper shoe 31.
The thickness of resin bed 32 is not particularly limited, is preferably 1 ~ 100 μm, is more preferably 5 ~ 30 μm, more preferably 7 ~ 20 μm.This is because when the thickness of resin bed 32 is this scope, resin bed 32 and fitting tightly of substrate 20 become abundant.In addition, this is because, even if entrained air bubbles, foreign matter between resin bed 32 and substrate 20, substrate 20 also can be suppressed to produce deformation defect.In addition, when the thickness of resin bed 32 is blocked up, needing time and materials to form resin bed, is therefore uneconomic.
It should be noted that, resin bed 32 can be formed by more than 2 layers.In this case, " thickness of resin bed 32 " means the gross thickness of all layers in resin bed.
In addition, when resin bed 32 is formed by more than 2 layers, the kind forming the resin of each layer can be different.
Resin bed 32 preferably by glass transition point lower than room temperature (about 25 DEG C) or do not have the material of glass transition point to be formed.This is because can become non-adhesive resin bed, more easily peel off with substrate 20, simultaneously also become abundant with fitting tightly of substrate 20.
In addition, resin bed 32 mostly heats in the manufacturing process of device, therefore preferably has heat resistance.
In addition, when the elastic modelling quantity of resin bed 32 is too high, there is the tendency with the close fitting step-down of substrate 20.On the other hand, when the elastic modelling quantity of resin bed 32 is too low, fissility can step-down.
The kind of the resin forming resin bed 32 is not particularly limited.Such as, acrylic resin, vistanex, polyurethane resin and silicones can be listed.Also several mixed with resin can be used.Wherein preferred silicones.This is because the heat resistance of silicones, fissility are excellent.In addition also because when gripper shoe 31 is glass plate, be easy to fix on a glass by the condensation reaction of the silanol base with glass pane surface.Silicone layer is under the state between gripper shoe 31 and substrate 20, even if such as in an atmosphere with about 200 DEG C process 1 hours, fissility also substantially can not be deteriorated, is also preferred from this point.
Resin bed 32 is preferably formed by the silicones (solidfied material) for peeling paper in silicones.The resin bed 32 that the hardening resin composition of formation peeling paper silicones is solidified to form on the surface of gripper shoe 31 has excellent fissility, is therefore preferred.In addition, because flexibility is high, even if the therefore foreign matter such as entrained air bubbles, dust between resin bed 32 and substrate 20, the generation of the deformation defect of substrate 20 also can be suppressed.
The curable silicone forming such peeling paper silicones is according to its curing mechanism, and can be divided into condensation reaction type organosilicon, addition reaction-type organosilicon, ultraviolet hardening organosilicon and electron ray curing type organosilicon, any one all can use.Preferred addition reaction-type organosilicon among these.This is because the degree of the easy degree of curing reaction, fissility when forming resin bed 32 is good, heat resistance is also high.
Addition reaction-type organosilicon is the solidification compound comprising host and crosslinking agent, solidify under the existence of the catalyst such as platinum group catalyst.The organosilyl solidification of addition reaction-type is promoted by heating.The organosilyl host of addition reaction-type is formed by the straight-chain organopolysiloxane with bonding thiazolinyl on the silicon atoms (vinyl etc.) (that is, olefinic organic based polysiloxane), and vinyl etc. become crosslinking points.The organosilyl crosslinking agent of addition reaction-type is formed by the straight-chain organopolysiloxane (that is, organic hydrogen polysiloxanes) with bonding hydrogen atom on the silicon atoms (silicon hydrogen base), and silicon hydrogen base etc. becomes crosslinking points.
In addition, the curable silicone forming peeling paper silicones has solvent-borne type, emulsion-type and no-solvent type form, and arbitrary type all can use.Preferred no-solvent type among these.This is because the aspect of productivity ratio, security, environmental characteristics is excellent.In addition, also because when not being included in solidification when forming resin bed 32 being heating and curing, ultraviolet curing or electron ray curing time produce the solvent of foaming, therefore bubble is difficult in resin bed 32 residual.
In addition, as the curable silicone forming peeling paper silicones, specifically, commercially available trade name can be listed or model is KNS-320A, KS-847(is organosilicon company of SHIN-ETSU HANTOTAI and manufactures), organosilicon company of TPR6700(GE Toshiba manufactures), the combination of vinyl organosilicon " 8500 " (Arakawa Chemical Industries, Ltd.'s manufacture) and methylhydrogen polysiloxanes " 12031 " (Arakawa Chemical Industries, Ltd. manufactures), the combination of vinyl organosilicon " 11364 " (Arakawa Chemical Industries, Ltd.'s manufacture) and methylhydrogen polysiloxanes " 12031 " (Arakawa Chemical Industries, Ltd. manufactures), the combination etc. of vinyl organosilicon " 11365 " (Arakawa Chemical Industries, Ltd.'s manufacture) and methylhydrogen polysiloxanes " 12031 " (Arakawa Chemical Industries, Ltd. manufactures).
Wherein, KNS-320A, KS-847 and TPR6700 are the curable silicones in advance containing host and crosslinking agent.
In addition, the silicones composition preferably had in silicone layer forming resin bed 32 is difficult to the character of moving to substrate 20, i.e. low organosilicon animal migration.
The method be fixed in gripper shoe 31 by resin bed 32 is not particularly limited, include, for example out the method be fixed on by the resin of film-form on the surface of gripper shoe 31.Specifically, can list: in order to give, to the surface of gripper shoe 31, surface modification treatment (prime treatment) be carried out to the high bed knife (high-peeling strength) on the surface of film, resin bed 32 is fixed on the method in gripper shoe 31.Such as, the chemical method (prime treatment) of the lifting chemistry bed knife as silane coupler can be exemplified, the physical method of the increase surface active groups as processed in flame (frame), the mechanical processing method etc. being increased attachment by the roughness increasing surface that blasting treatment is such.
In addition, also by being such as formed into the layer of the hardening resin composition of resin bed 32 on the surface in gripper shoe 31, then this hardening resin composition can be solidified to form the method for resin bed 32, form the resin bed 32 be fixed in gripper shoe 31 thus.As the method for layer forming hardening resin composition in gripper shoe 31 on the surface, include, for example out the method be coated on by hardening resin composition in gripper shoe 31.As coating process, spraying process can be listed, mould is coated with method, spin-coating method, dip coating, rolling method, stick coating method, silk screen print method, gravure coating process.Suitably can select from these methods according to the kind of resin combination.
In addition, when being coated in gripper shoe 31 by the hardening resin composition forming resin bed 32, its coating weight is preferably 1 ~ 100g/m 2, be more preferably 5 ~ 20g/m 2.
Such as, when forming resin bed 32 by the organosilyl hardening resin composition of addition reaction-type, the hardening resin composition formed by mixture by olefinic organic based polysiloxane, organic hydrogen polysiloxanes and catalyst is coated in gripper shoe 31 by known methods such as above-mentioned spraying processes, makes thereafter it be heating and curing.The condition that is heating and curing is different according to the compounding amount of catalyst, such as, in total amount 100 mass parts relative to olefinic organic based polysiloxane and organic hydrogen polysiloxanes, during compounding 2 mass parts platinum group catalyst, in an atmosphere with 50 DEG C ~ 250 DEG C, preferably react with 100 DEG C ~ 200 DEG C.In addition, reaction time is now set to 5 ~ 60 minutes, is preferably set to 10 ~ 30 minutes.
By making hardening resin composition be heating and curing, during curing reaction, silicones and gripper shoe 31 carry out chemical bond, and/or by anchor effect (anchor effect), silicone layer are combined with gripper shoe 31.By their effect, silicone layer is stably fixed in gripper shoe 31.It should be noted that, when being formed the resin bed that the resin beyond by silicones is formed by hardening resin composition, also can form fixing resin bed on the supporting plate by method same as described above.
Making resin bed 32 fit tightly method on the base plate 20 with strippable form can for known method.Such as, can to list under atmospheric pressure environment after the overlapping substrate 20 in fissility surface of resin bed 32, use the method for roller, press crimping resin bed 32 and substrate 20.By crimping with roller, press, resin bed 32 and substrate 20 fit tightly more, are therefore preferred.In addition, by utilizing the crimping of roller or press, can remove the bubble be mixed between resin bed 32 and substrate 20 relatively easily, be therefore preferred.
If utilize vacuum layer platen press, Vacuum Pressure method for making crimp, then more preferably can suppress being mixed into of bubble, guarantee closely sealed well, because of but preferred.Carry out crimping also tool under vacuo to have the following advantages: even if also can not grow up due to heating at the situation bubble of remaining small bubble, not easily cause the deformation defect of substrate 20.
When resin bed 32 is fitted tightly on the base plate 20 with strippable form, preferably, washing resin layer 32 and substrate 20 contact with each other the surface of side fully, carry out stacked under the environment that cleanliness factor is high.Even if be mixed into foreign matter between resin bed 32 and substrate 20, therefore can not impact the flatness on the surface of substrate 20 because resin bed 32 can be out of shape, but cleanliness factor its flatness higher being better, is therefore preferred.
It should be noted that, the order of the operation be fixed on by resin bed 32 in gripper shoe 31 with the operation making resin bed 32 fit tightly on the base plate 20 with strippable form is not particularly limited, such as, can carries out approximately simultaneously.
In the present invention, fit tightly face 201 and process with silicone oil or silane coupler in advance with at least one party fitting tightly face 321, or resin bed 32 is formed by the resin comprising silicone oil or silane coupler.First embodiment is wherein the former surface treatment.By carrying out surface treatment with silicone oil or silane coupler to fitting tightly face 201 in advance with at least one party fitting tightly face 321 before fitting tightly, the density of the polar group existed in the face of fitting tightly 201,321 suitably can be regulated thus.Wherein, in present embodiment, surface treatment can be carried out to the face that fits tightly 201 of substrate 20 side in advance, also can carry out surface treatment to the face that fits tightly 321 of resin bed 32 side in advance, surface treatment can also be carried out to the face that fits tightly 201,321 of both sides in advance.In addition, by being formed resin bed 32(second embodiment by the resin comprising silicone oil or silane coupler), also similarly suitably can regulate the density of the polar group existed in the face of fitting tightly 321.
Herein, the polar group that the surface as glass substrate exists, include, for example out hydroxyl (-OH) etc.In addition, the polar group that the surface as resin bed exists, include, for example out carbonyl (-CO), carboxyl (-COOH) etc.These polar groups are hydrophilic radical.
Whether appropriate to judge the density of the polar group existed in the face that fits tightly 201,321 of substrate 20 and resin bed 32 by measuring the water contact angle becoming the surface in the face of fitting tightly 201,321 before fitting tightly.The density of the hydrophilic polar group usually having surface to exist is higher, and water contact angle becomes less tendency.Herein, water contact angle refers to the contact angle specified in JIS R 3257-1999.
Carry out surface-treated to fit tightly the water contact angle of face 201,321 before fitting tightly and be preferably more than 90 °, be more preferably 90 ~ 120 °, more preferably 90 ~ 110 °.When both water contact angle of the face that fits tightly 201,321 before fitting tightly all are less than 90 °, the density of the polar group of the surface existence of substrate 20, resin bed 32 is too high.Therefore, in the manufacturing process of device, when the temperature of duplexer 10 is more than 250 DEG C, substrate 20 is promoted with the chemical bond of resin bed 32, substrate 20 and resin bed 32(reinforcement plate 30) become and be difficult to be separated.
Water contact angle before fitting tightly is the face that fits tightly 201 that the surface of more than 90 ° is preferably substrate 20.If the water contact angle fitting tightly face 201 is more than 90 °, even if then fit tightly the water contact angle of face 321 before fitting tightly lower than 90 °, as long as the hydrophily of resin is not high especially, resin bed 32 and substrate 20 easily can be peeled off.When particularly resin bed 32 is the hydrophobic resins such as silicones, even if fit tightly the water contact angle of face 321 before fitting tightly lower than 90 °, also can easily peel off.
Trickle concaveconvex structure can be pre-formed on the face that fits tightly 201 of substrate 20 by the surface treatment before fitting tightly.In this case, by the anchor effect of concaveconvex structure, the face that fits tightly 201 of substrate 20 is fitted tightly with sufficient adhesion with the face that fits tightly 321 of resin bed 32, can easily process duplexer 10.Wherein, when forming fine concaveconvex structure by surface treatment, there is the tendency increased in water contact angle, water contact angle can more than 120 ° sometimes.
Carry out surface-treated surface and be preferably fully clean face, be preferably the face after just washing.When cleanliness factor (activity degree) is too low, uniform surface treatment cannot be carried out.As washing methods, the usual way of the washing for glass surface, resin surface can be used.
Surface-treated surface is not carried out it is desirable that protect in advance with protective films such as masks.This is because the face being attached with surface-treated material is difficult to forming apparatus component in the manufacturing process of device by mistake.
May be used singly or in combin as the silicone oil of surface-treated material, silane coupler.When combinationally using, after can carrying out surface treatment with silane coupler, recycle silicon oil carries out surface treatment, and after also can carrying out surface treatment with silicone oil, recycle silicon alkane coupling agent carries out surface treatment.
The kind of silicone oil is not particularly limited, can exemplify the straight chain silicone oil (straight silicone oil) such as dimethicone, methyl phenyl silicone oil, methyl hydrogen silicone oil, side chain or end have imported the modified silicon oil of alkyl, hydrogen base, epoxy radicals, amino, carboxyl, polyether-based, halogen group etc.As object lesson, can list methylhydrogen polysiloxanes, dimethyl polysiloxane, methyl phenyl silicone, diphenylpolysiloxane etc., heat resistance increases according to the order of above-mentioned record, and what heat resistance was the highest is diphenylpolysiloxane.These silicone oil are generally used for glass substrate, carried out the water-proofing treatment on the surface of the substrates such as the metal substrate of prime treatment.
Surface treatment method based on silicone oil can be usual way.For being only merely coated with the process of silicone oil, owing to there being the worry that silicone oil is low with the combination degree on processed surface, cannot give full play to treatment effect, be therefore preferably combined in process on processed surface at the after-applied silicone oil that makes of coating silicone oil.Think and make the silicone oil process be combined on processed surface be process strand as cut off silicone oil, the part cut off is combined in processed surface upper (below this process being called that the low molecule of silicone oil quantizes).
As the surface treatment method based on silicone oil, preferably, silicone oil is coated on the face that fits tightly 321 of the face that fits tightly 201 of substrate 20, resin bed 32, and carries out the method for low-molecular-weight.By the treatment conditions etc. regulating the coating weight of silicone oil, low molecule quantizes, the density optimization of the polar group that the face that fits tightly 321 of the face that fits tightly 201 of substrate 20, resin bed 32 can be existed.Thereby, it is possible to suppress peel off resin bed 32 and substrate 20 time resin bed 32 cohesion failure.
The coating process of silicone oil can be usual way.Such as, according to the kind of silicone oil, coating weight etc., can be coated with method, spin-coating method, dip coating, rolling method, stick coating method, silk screen print method, gravure coating process etc. suitably select from spraying process, mould.As coating fluid, it is desirable that silicone oil is diluted to the solution of below 1 quality % by use hexane, heptane, dimethylbenzene equal solvent.During more than 1 quality %, the processing time that low molecule quantizes is long.In addition, it is desirable that use the solution being diluted to more than 0.01 quality %.During lower than 0.01 quality %, the optimization of the density of polar group can become insufficient.
The method that silicone oil low molecule quantizes can be used usual way, such as, have the method by light decomposes, the siloxane bond of silicone oil is cut off in thermal decomposition.Light utilizes the ultraviolet irradiated from low pressure mercury lamp, xenon arc lamp etc. in decomposing, also may be combined with the ozone using and produced by the Ultraviolet radiation in air.Thermal decomposition can be carried out with batch furnace, conveyor furnace etc., also can utilize plasma, arc discharge etc.When carrying out thermal decomposition with batch furnace, conveyor furnace, although according to the kind of the silicone oil of above-mentioned coating fluid, concentration and different, it is desirable that process at 250 DEG C ~ 400 DEG C.During lower than 250 DEG C, organosilyl low molecule quantizes to become insufficient, and during more than 400 DEG C, organosilyl silication becomes remarkable, becomes insufficient as low molecule quantification treatment.
If the siloxane bond of silicone oil is cut off, then the density of the hydrophobic functional groups such as methyl uprises, and the density of the hydrophilic polar group existed in the face that fits tightly 201 of substrate 20, the face that fits tightly 321 of resin bed 32 reduces.Wherein, if the siloxane bond of silicone oil is excessively cut off, then the tendency that the density of hydrophilic polar group increases again is had.
The kind of silane coupler is not particularly limited, such as, preferably can use more than one being selected from following compound: HMDS (HMDS), APTES, N-(2-amino-ethyl)-3-TSL 8330, N-{N-(2-amino-ethyl)-2-amino-ethyl the amino silicone alkanes such as-3-TSL 8330,3-anilino-propyl trimethoxy silicane; 3-glycidoxypropyltrime,hoxysilane, 2-(3,4-epoxycyclohexyl) the epoxy radicals silicone hydride class such as ethyl trimethoxy silane; The chlorosilane of 3-r-chloropropyl trimethoxyl silane and so on, silicon fluoride class; The hydrosulphonyl silanes such as 3-sulfydryl trimethoxy silane; Vinyltrimethoxy silane, N-2-(N-vinyl benzyl-2-amino-ethyl) the vinyl silanes class such as-3-TSL 8330; The silicon Acrylote alkanes such as 3-methacryloxypropyl trimethoxy silane.
Surface treatment method based on silane coupler can be usual way.Such as, the face that fits tightly 201 of substrate 20, the face that fits tightly 321 of resin bed 32 are exposed in the atmosphere comprising the gas gasified by silane coupler, the hydrophilic polar group existed are replaced as the method etc. of the hydrophobic functional groups such as methyl in the face that fits tightly 321 of the face that fits tightly 201 of substrate 20, resin bed 32.By regulating the concentration, temperature, processing time etc. of the silane coupler in atmosphere, can by the density optimization of the polar group of existence in the face that fits tightly 321 of the face that fits tightly 201 of substrate 20, resin bed 32.Thereby, it is possible to suppress peel off resin bed 32 and substrate 20 time resin bed 32 cohesion failure.
In addition, fit tightly face 201,321 after the midway of the manufacturing process of device is peeled off mutually, the state before surface treatment can be returned to by the process of regulation.Such as applied can be decomposed by light based on the surface-treated face of silicone oil or silane coupler, thermal decomposition returned to the state before surface treatment.Thus, if the surface 201 of such as substrate 20 is returned to the state before surface treatment, then can improve to attaching intensity time surperficial 201 optical film adhered (such as, polarizing film).In addition, if pay attention to re-workability, then also can with surface 201 optical film adhered of the state after surface treatment directly to substrate 20.
(the second embodiment)
The formation of the duplexer of present embodiment is roughly the same with Fig. 1, therefore omits diagram.
In the present embodiment, resin bed 32 is formed by the resin comprising silicone oil or silane coupler.Preferably, resin bed 32 is solidified to form by making the hardening resin composition comprising silicone oil or silane coupler.Hardening resin composition is not particularly limited, such as, can uses the hardening resin composition forming peeling paper silicones.Wherein, for the face that fits tightly 201,321 of substrate 20 and resin bed 32, before fitting tightly, also above-mentioned surface treatment can not be applied.
Silicone oil, silane coupler can be used alone or combinationally use, and preferably use silicone oil, the silane coupler without the functional group of reacting with the composition of hardening resin composition respectively.Such as, when forming resin bed 32 by the organosilyl hardening resin composition of aforementioned addition reaction-type, as silicone oil, silane coupler, use silicone oil, the silane coupler without the functional group's (such as, vinyl, silicon hydrogen base) becoming crosslinking points.In addition, when forming resin bed 32 by the organosilyl hardening resin composition of condensation reaction type, use that do not have can the silicone oil of functional group's (hydrolization group, silanol base etc.) of cocondensation.
In this resin bed 32, silicone oil is uncrosslinked when the solidification of above-mentioned hardening resin composition, but comprises dispersedly wherein.In addition, the silane coupler condensation when the solidification of above-mentioned hardening resin composition usually, and be included in the form of the condensation product of silane coupler in the resin solidified.Therefore, the condensation product of silicone oil or silane coupler is comprised in the face that fits tightly 321 of resin bed 32 dispersedly.
Such as, when comprising silicone oil in the face that fits tightly 321 of resin bed 32, in the manufacturing process of device, if the temperature of duplexer 10 uprises, then silicone oil can quantize by low molecule.Its result, two density fitting tightly the hydrophilic polar group existed in face 201,321 reduce, and the density of the hydrophobic functional groups such as methyl increases.
In addition, when comprising silane coupler condensation product in the face that fits tightly 321 of resin bed 32, two fit tightly the hydrophilic polar group existed in face 201,321 and are replaced by hydrophobic functional groups such as methyl.
Therefore, by regulating the content, the kind that become silicone oil or the silane coupler comprised in the hardening resin composition of resin bed 32, two can be fitted tightly the density optimization of the polar group existed in face 201,321.
Therefore, in present embodiment, the cohesion failure of resin bed 32 when also can suppress to peel off resin bed 32 and substrate 20 in the same manner as the first embodiment.In addition, carry out because the operation that quantized by silicone oil low molecule merges with the operation for other objects, in addition, due to not by the operation of silane coupler gasification, therefore can reduce process number.
It is desirable that the content forming silicone oil and the silane coupler comprised in the hardening resin composition of resin bed 32 is 0.1 ~ 5 quality % relative to the solid constituent of the hardening resin composition comprising them.During lower than 0.1 quality %, sufficient effect cannot be obtained.On the other hand, during more than 5 quality %, the heat resistance of resin bed 32 becomes too low.
When the second embodiment, the face that fits tightly 201 of substrate 20 also can not apply the surface treatment in foregoing first embodiment.When substrate 20 is glass substrate, because its surface is the surface that hydrophily is high, therefore fit tightly the surface treatment that face 201 also can apply in foregoing first embodiment in advance before fitting tightly.
Embodiment
Below, specifically describe the present invention further by embodiment etc., but the present invention is not by the restriction of these examples.
[embodiment 1]
Substrate and gripper shoe all use the glass plate (Asahi Glass Co., Ltd manufactures, AN100, alkali-free glass) of the long 720mm × wide 600mm obtained by float glass process.Wherein, the thickness of substrate is set to 0.4mm, the thickness of gripper shoe is set to 0.3mm.The average coefficient of linear expansion of substrate and gripper shoe is respectively 38 × 10 -7/ DEG C.
(making of reinforcement plate)
Gripper shoe is carried out pure water, UV washing, make the clean surface of gripper shoe.Thereafter, serigraphy is utilized to be coated with hardening resin composition (coating weight 30g/m on the one side of gripper shoe 2).
Hardening resin composition uses the mixture of the solvent-free addition reaction-type organosilicon of 100 mass parts (organosilicon company of SHIN-ETSU HANTOTAI manufactures, KNS-320A) and 2 mass parts platinum group catalysts (organosilicon company of SHIN-ETSU HANTOTAI manufactures, CAT-PL-56).
Above-mentioned solvent-free addition reaction-type organosilicon comprises the straight-chain olefinic organic based polysiloxane (host) with bonding vinyl on the silicon atoms and methyl and has bonding hydrogen atom on the silicon atoms and the straight-chain organic hydrogen polysiloxanes (crosslinking agent) of methyl.
Within 30 minutes, make it solidify with 180 DEG C of heating in an atmosphere in coating mixture on the supporting plate, thus centre is on the supporting plate formed and the silicone layer of fixed length 705mm × wide 595mm × thickness 20 μm.
(surface treatment of substrate)
Substrate is carried out pure water, UV washing, make the clean surface of substrate.Thereafter, the second interarea of the one side as substrate applies on the basis of mask, on the first interarea of opposition side, sprayed silicon oil content is the n-heptane solution also drying of 0.5 quality %.Silicone oil uses dimethyl polysiloxane (Dow Corning Toray Co., Ltd. manufactures, SH200).Then, in order to the low molecule carrying out silicone oil quantizes, and 2 minutes UV treatment based on low pressure mercury lamp are carried out in atmosphere.
Thereafter, use contact angle instrument (KRUSS company manufactures, DROP SHAPE ANALYSIS SYSTEM DSA 10Mk2), measuring the water contact angle of the first interarea of substrate, is 100 °.
(making of duplexer)
After UV treatment, to the overlapping silicone layer of the first interarea of substrate, by vacuum pressing, substrate and silicone layer are at room temperature fitted tightly, thus obtain the duplexer that formed by substrate and reinforcement plate.
(heat resistant test of duplexer)
By this duplexer at oxysome volume concentrations be in the nitrogen atmosphere of below 1000ppm, heat 1 hour at 350 DEG C.Thereafter, after cooling to room temperature, peel off cutter to inserting between substrate and silicone layer, limit keeps substrate-side smooth, while make the deflection deformation successively near insertion position of silicone layer side, thus peels off substrate and silicone layer.
According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing thing of the appearance of the substrate after stripping from silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 100 °.
[embodiment 2]
Substrate and gripper shoe use the glass plate identical with embodiment 1 respectively.
(making of reinforcement plate)
In embodiment 2, as hardening resin composition, two ends are used to have the straight-chain olefinic organic based polysiloxane (vinyl organosilicon of vinyl, Arakawa Chemical Industries, Ltd. manufactures, 8500), there is in molecule polymethyl hydrogen siloxane (Arakawa Chemical Industries, Ltd. manufactures, 12031) and platinum group catalyst (Arakawa Chemical Industries, Ltd.'s manufacture of silicon hydrogen base, CAT 12070) mixture, in addition, operate similarly to Example 1, make reinforcement plate.
Herein, regulate the mixing ratio of straight-chain olefinic organic based polysiloxane and methylhydrogen polysiloxanes, make the mol ratio of vinyl and silicon hydrogen base be 1:1.In addition, relative to total amount 100 mass parts of straight-chain olefinic organic based polysiloxane and methylhydrogen polysiloxanes, platinum group catalyst is set to 5 mass parts.
(surface treatment of substrate)
In embodiment 2, in order to the low molecule of silicone oil quantizes, carry out, based on the plasma treatment of normal pressure remote plasma unit (Sekisui Fine Chemical Co., Ltd. manufactures, RT series), in addition, operating similarly to Example 1, carrying out the surface treatment of substrate.
Herein, the treatment conditions of plasma treatment are set to: export 3kw, nitrogen/air mass flow ratio=600slm/750sccm, transporting velocity 5m/ minute.The surface temperature of substrate during irradiation plasma is less than 50 DEG C.The water contact angle of the first interarea of the substrate after surface treatment is 95 °.
(making of duplexer)
After surface treatment, operate similarly to Example 1, obtain the duplexer formed by substrate and reinforcement plate.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, peel off substrate and silicone layer similarly to Example 1.According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing thing of the appearance of the substrate after stripping from silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 100 °.
[embodiment 3]
Substrate and gripper shoe use the glass plate identical with embodiment 1 respectively.
(making of reinforcement plate)
In embodiment 3, operate similarly to Example 2, make reinforcement plate.
(surface treatment of substrate)
In embodiment 3, in order to the low molecule of silicone oil quantizes, carry out heating for 10 minutes with 400 DEG C in an atmosphere, in addition, operated similarly to Example 1, carry out the surface treatment of substrate.The water contact angle of the first interarea of the substrate after surface treatment is 105 °.
(making of duplexer)
After surface treatment, operate similarly to Example 1, obtain the duplexer formed by substrate and reinforcement plate.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, peel off substrate and silicone layer similarly to Example 1.According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing thing of the appearance of the substrate after stripping from silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 105 °.
[embodiment 4]
Substrate and gripper shoe use the glass plate identical with embodiment 1 respectively.
(making of reinforcement plate)
In embodiment 4, operate similarly to Example 2, make reinforcement plate.
(surface treatment of substrate)
In embodiment 4, in order to the low molecule of silicone oil quantizes, the first interarea sprayed silicon oil content to substrate is the n-heptane solution of 0.1 quality % and makes it dry, carries out heating for 10 minutes in an atmosphere with 250 DEG C, in addition, the surface treatment of substrate is carried out similarly to Example 1.The water contact angle of the first interarea of the substrate after surface treatment is 98 °.
(making of duplexer)
After surface treatment, operate similarly to Example 1, obtain the duplexer formed by substrate and reinforcement plate.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, peel off substrate and silicone layer similarly to Example 1.According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing thing of the appearance of the substrate after stripping from silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 98 °.
[embodiment 5]
Substrate and gripper shoe use the glass plate (Asahi Glass Co., Ltd manufactures, AS, soda-lime glass) of the long 720mm × wide 600mm obtained by float glass process respectively.Wherein, the thickness of substrate is set to 0.4mm, the thickness of gripper shoe is set to 0.3mm.The average coefficient of linear expansion of substrate and gripper shoe is respectively 85 × 10 -7/ DEG C.
(making of reinforcement plate)
In embodiment 5, operate similarly to Example 2, make reinforcement plate.
(surface treatment of substrate)
In embodiment 5, in order to the low molecule of silicone oil quantizes, on the first interarea of substrate, sprayed silicon oil content is the n-heptane solution of 0.5 quality % and dry, in an atmosphere, carries out heating for 10 minutes at 350 DEG C, in addition, the surface treatment of substrate is carried out similarly to Example 1.The water contact angle of the first interarea of the substrate after surface treatment is 102 °.
(making of duplexer)
After surface treatment, operate similarly to Example 1, obtain the duplexer formed by substrate and reinforcement plate.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, peel off substrate and silicone layer similarly to Example 1.According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing thing of the appearance of the substrate after stripping from silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 102 °.
[embodiment 6]
Substrate and gripper shoe use glass plate identical with embodiment 5 except chemical enhanced respectively.
(making of reinforcement plate)
In embodiment 6, operate similarly to Example 2, make reinforcement plate.
(surface treatment of substrate)
In embodiment 6, in order to the low molecule of silicone oil quantizes, carry out the surface treatment of substrate similarly to Example 5.The water contact angle of the first interarea of the substrate after surface treatment is 102 °.
(making of duplexer)
After surface treatment, obtain the duplexer formed by substrate and reinforcement plate similarly to Example 1.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, peel off substrate and silicone layer similarly to Example 1.According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing thing of the appearance of the substrate after stripping from silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 102 °.
[embodiment 7]
Substrate and gripper shoe use the glass plate identical with embodiment 1 respectively.
(making of reinforcement plate)
Gripper shoe is carried out pure water, UV washing, make the clean surface of gripper shoe.Thereafter, utilize serigraphy on the one side of gripper shoe, be coated with mixture (the coating weight 30g/m of 99.5 mass parts hardening resin compositions and 0.5 mass parts silicone oil 2).Herein, hardening resin composition uses the composition identical with embodiment 2, and silicone oil uses dimethyl polysiloxane (Dow Corning Toray Co., Ltd. manufactures, SH200).
By coating mixture on the supporting plate in an atmosphere, at 180 DEG C heating within 30 minutes, make it solidify, thus centre is on the supporting plate formed and the silicone layer of fixed length 705mm × wide 595mm × thickness 20 μm.
(making of duplexer)
After making reinforcement plate, to the stacked silicone layer in the surface after the washing of substrate, at room temperature by vacuum pressing, substrate and silicone layer are fitted tightly, thus obtain the duplexer that formed by substrate and reinforcement plate.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, peel off substrate and silicone layer similarly to Example 1.According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing of the appearance of the substrate after stripping from the resin of silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 102 °.
[embodiment 8]
Substrate and gripper shoe use the polyimide resin plate (Du Pont-Toray Co., Ltd. manufactures, Kapton 200HV) of long 720mm × wide 600mm respectively.Wherein, the thickness of substrate is set to 0.05mm, the thickness of gripper shoe is set to 0.5mm.
(making of reinforcement plate)
In embodiment 8, operate similarly to Example 2, make reinforcement plate.
(surface treatment of substrate)
In embodiment 8, operate similarly to Example 2, carry out the surface treatment of substrate.The water contact angle of the first interarea of the substrate after surface treatment is 100 °.
(making of duplexer)
After surface treatment, to the overlapping silicone layer of the first interarea of substrate, at room temperature by vacuum pressing, substrate and silicone layer are fitted tightly, thus obtain the duplexer that formed by substrate and reinforcement plate.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, peel off substrate and silicone layer similarly to Example 1.According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing thing of the appearance of the substrate after stripping from silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 100 °.
[embodiment 9]
Substrate and gripper shoe use the glass plate identical with embodiment 1 respectively.
(making of reinforcement plate)
In embodiment 9, operate similarly to Example 2, make reinforcement plate.
(surface treatment of substrate)
Substrate is carried out pure water, UV washing, make the clean surface of substrate.Thereafter, after second interarea of the one side as substrate applies mask, first interarea of opposition side is maintained in the atmosphere of saturation state at the gas making silane coupler (Dow Corning Toray Co., Ltd. manufactures, Z6040) gasify and exposes 10 minutes.The surface temperature of substrate during exposure is 25 DEG C.The water contact angle of the first interarea of the substrate after exposure is 100 °.
(making of duplexer)
After based on the surface treatment of silane coupler, to the overlapping silicone layer of the first interarea of substrate, at room temperature by vacuum pressing, substrate and silicone layer are fitted tightly, thus obtain the duplexer that formed by substrate and reinforcement plate.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, peel off substrate and silicone layer in the same manner as embodiment 1.According to the observation of light microscope, have no the silicone layer after stripping and occur cohesion failure, have no the transfer printing thing of the appearance of the substrate after stripping from silicone layer.In addition, the water contact angle of the first interarea of the substrate after stripping is 100 °.
[comparative example 1]
Substrate and gripper shoe use the glass plate identical with embodiment 1 respectively.
(making of duplexer)
In comparative example 1, operate similarly to Example 2, make reinforcement plate, first interarea of substrate is carried out pure water and UV washing and purifying after, overlapping silicone layer on the first interarea of substrate, at room temperature by vacuum pressing, substrate and silicone layer are fitted tightly, thus obtain the duplexer that formed by substrate and reinforcement plate.In addition, the water contact angle before the fitting tightly of the face that fits tightly (the first interarea) of substrate is 7 °.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, when peeling off substrate and silicone layer similarly to Example 1, there is cohesion failure in silicone layer, a part for silicone layer is attached to substrate-side.
[comparative example 2]
Substrate and gripper shoe use the glass plate identical with embodiment 1 respectively.
(making of reinforcement plate)
In comparative example 2, operate similarly to Example 2, make reinforcement plate.
(making of duplexer)
Make reinforcement plate similarly to Example 2, first interarea of substrate is carried out pure water and purifying after, to the overlapping silicone layer of the first interarea of substrate, at room temperature by vacuum pressing, substrate and silicone layer are fitted tightly, thus obtain the duplexer that formed by substrate and reinforcement plate.In addition, the water contact angle before the fitting tightly of the first interarea of substrate is 40 °.
(heat resistant test of duplexer)
After being heated similarly to Example 1 by this duplexer, when peeling off substrate and silicone layer similarly to Example 1, there is cohesion failure in silicone layer, a part for silicone layer is attached to substrate-side.
Understand the present invention in detail with reference to specific embodiment, but under the premise without departing from the spirit and scope of the present invention, can apply various correction, change, this is apparent to those skilled in the art.
The application applied for based on May 11st, 2010, Japanese patent application 2010-108952, is incorporated herein its content as reference.
description of reference numerals
10 duplexers
20 substrates
201 fit tightly face (the first interarea)
202 second interareas
30 reinforcement plates
31 gripper shoes
32 resin beds
321 fit tightly face

Claims (8)

1. the manufacture method of a duplexer, it is for manufacturing the method for the duplexer having substrate and gripper shoe and be present in the resin bed between them, the method has following operation: described resin bed be formed in the operation in described gripper shoe and make described resin bed fit tightly the operation in described substrate with strippable form
Also there is following operation:
At least one party to the described substrate surface that will fit tightly and described resin layer surface be coated with silicone oil or silane coupler operation and
The operation of process when described silicone oil being carried out during coating silicone oil to operation, the silane-coating coupling agent of low molecule quantification treatment, described silane coupler being reacted,
Thereafter, in the described operation fitted tightly, make described substrate and described resin bed overlapping and fit tightly.
2. the manufacture method of duplexer according to claim 1, wherein, the described substrate surface silicone oil that fit tightly or silane coupler implement surface treatment, and the water contact angle being applied with the substrate surface of described process is more than 90 °.
3. the manufacture method of duplexer according to claim 1 and 2, wherein, described resin bed is being formed in the operation in described gripper shoe, is forming cured resin composition layer on described gripper shoe surface, then make this hardening resin composition be solidified to form described resin bed.
4. the manufacture method of duplexer according to claim 1 and 2, wherein, described resin bed is formed by silicones.
5. the manufacture method of duplexer according to claim 1 and 2, wherein, described resin bed is formed by the reaction solidfied material of olefinic organic based polysiloxane and organic hydrogen polysiloxanes.
6. a duplexer, its resin bed that there is substrate and gripper shoe and be present between them, described resin bed and described substrate fit tightly with strippable form, the mode of the peel strength that described resin bed is greater than between described resin bed and described substrate with the peel strength between them in described gripper shoe is fixed
The described substrate surface fitted tightly and at least one party of described resin layer surface are by being formed with the surface of silicone oil or silane coupler process in advance, described in implement surface-treated substrate surface water contact angle be more than 90 °.
7. duplexer according to claim 6, wherein, described resin bed is formed by silicones.
8. duplexer according to claim 6, wherein, described resin bed is formed by the reaction solidfied material of olefinic organic based polysiloxane and organic hydrogen polysiloxanes.
CN201180023392.8A 2010-05-11 2011-04-28 Process for producing laminate, and laminate Active CN102883879B (en)

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JP2010108952 2010-05-11
PCT/JP2011/060448 WO2011142280A1 (en) 2010-05-11 2011-04-28 Process for producing laminate, and laminate

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JP5835214B2 (en) 2015-12-24
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CN104085168A (en) 2014-10-08
JPWO2011142280A1 (en) 2013-07-22

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