CN103435257B - Glass film layers lamination and manufacture method thereof - Google Patents
Glass film layers lamination and manufacture method thereof Download PDFInfo
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- CN103435257B CN103435257B CN201310347051.7A CN201310347051A CN103435257B CN 103435257 B CN103435257 B CN 103435257B CN 201310347051 A CN201310347051 A CN 201310347051A CN 103435257 B CN103435257 B CN 103435257B
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- glass substrate
- glassy membrane
- support glass
- membrane
- lamination
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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
-
- 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
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65G—TRANSPORT OR STORAGE DEVICES, e.g. CONVEYORS FOR LOADING OR TIPPING, SHOP CONVEYOR SYSTEMS OR PNEUMATIC TUBE CONVEYORS
- B65G49/00—Conveying systems characterised by their application for specified purposes not otherwise provided for
- B65G49/05—Conveying systems characterised by their application for specified purposes not otherwise provided for for fragile or damageable materials or articles
- B65G49/06—Conveying systems characterised by their application for specified purposes not otherwise provided for for fragile or damageable materials or articles for fragile sheets, e.g. glass
- B65G49/061—Lifting, gripping, or carrying means, for one or more sheets forming independent means of transport, e.g. suction cups, transport frames
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B35/00—Transporting of glass products during their manufacture, e.g. hot glass lenses, prisms
- C03B35/14—Transporting hot glass sheets or ribbons, e.g. by heat-resistant conveyor belts or bands
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Ceramic Engineering (AREA)
- Joining Of Glass To Other Materials (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides a kind of glass film layers lamination and manufacture method thereof, this plywood comprises stacked support glass substrate and glassy membrane, the edge of described glassy membrane is positioned in the lamination surface of described support glass substrate, have sealing ply between all sides of described glassy membrane and the lamination surface of described support glass substrate, the difference of the surfaceness of the part that the lamination surface of described support glass substrate and the lamination surface of described glassy membrane contact with each other is more than or equal to 1.0nm.Scheme provided by the invention, the contact surface of layer glass is provided with the extremely strong seal area of bonding force and the extremely weak stacked district of uneven surface of bonding force, by seal area, stably can manufactures association process; By the stacked district of uneven surface, be easy to peel off glassy membrane, prevent because bonding force cross strong and cause glassy membrane to peel off time breakage, prevent because of bonding force cross weak and cause manufacture association process time the coming off of glassy membrane.
Description
Technical field
The present invention relates to glass film technology, particularly relate to a kind of glass film layers lamination and manufacture method thereof, be particularly useful for liquid-crystal display or organic EL(electro-luminescence, electroluminescent) glassy membrane that uses in the cover glass or pharmaceuticals encapsulation etc. of the equipment such as glass substrate or organic EL illuminating of the equipment such as flat-panel monitor or solar cell, lithium ion battery, digital signage, touch panel, electronic book of indicating meter etc.
Background technology
Popularize liquid-crystal display in recent years, the flat-panel display devices such as OLED display, further slimming is required to these flat-panel display devices, special in OLED display, require by folding or reel and easily carry, and not only can also be used for curved surface for plane, in addition, on the bodywork surface of motor vehicle or the roof of buildings, post, the surface that outer wall etc. have the object of curved surface forms solar cell, or form the words of organic EL illuminating, its purposes can become extensively, thus, further thin plate and high pliability are required for substrate used in such devices or cover plate.
The twinkler used in OLED display is deteriorated owing to contacting with the gas of oxygen or water vapour etc., thus, higher gas-barrier property is required for the substrate used in OLED display, therefore expect to use glass substrate, but, the glass used in substrate is due to different from resin molding and do not tolerate tensile stress, therefore pliability is low, breakage can be produced when applying tensile stress by curved glass substrate to glass baseplate surface, needing to carry out ultra thin plate to give pliability to glass substrate, proposing the glassy membrane that thickness is less than 200 μm.
For the glass substrate used in the electron device of flat-panel monitor or solar cell etc., the manufacture association process of the various electron device such as membrane process or clean of nesa coating etc. can be carried out, manufacture association process to refer to be coated with the various films such as nesa coating on glass, when making glass surface possess flat-panel monitor or solar cell electron device corresponding function, the association manufacturing process that must experience, membrane process listed in such as literary composition or clean, but, when carrying out the glass substrate membranization used in these electron devices, because glass is hard brittle material, therefore will breakage be produced because of STRESS VARIATION slightly, when carrying out the process that above-mentioned various electron devices are associated, very difficulty, in addition, because the glassy membrane of thickness below 200 μm is rich flexible, be difficult to position when carrying out manufacture association process.
Name be called " glass film laminate " application number be 201180010413.2 patent documentations one and name be called " glass film laminate " application number be 201080021282.3 patent documentation two all describe a kind of by support glass substrate and glassy membrane by the stacked glass film laminate be combined into, for improving the treatability of glassy membrane, even if adopt the sheet glass not having intensity or rigidity in monomer, also existing glass liquid crystal display device manufacturing line can be shared to manufacture liquid crystal display device, glass substrate can be peeled off after operation terminates, in addition, owing to using supporting mass, therefore also easily position during association process.
But, realizing the further ultra thin plate of sheet glass, carry out ultra thin plate when changing into as glassy membrane, even above-mentioned glass film laminate, also be difficult to glassy membrane to be peeled off from support glass substrate after electron device makes, when glassy membrane is peeled off from support glass substrate, peel off from the corner part of glassy membrane, but, in the glass film laminate recorded in patent documentation one, breakage or shortcoming is easily produced when peeling off glassy membrane, especially, when glassy membrane and support glass substrate are adhered, this problem is particularly remarkable, in order to solve this problem, also contemplate and make glassy membrane outstanding stacked from a support glass substrate part, but also there is the problem of the glassy membrane breakage of exposing from support glass substrate.
The scheme of patent documentation one, when carrying out film forming process, clean to the surface of glassy membrane, because support glass substrate and glassy membrane are bonding well, therefore, it is possible to location when processing without any problems, operation; But when peeling off after treatment, glassy membrane is then crossed due to bonding force and bent by force and significantly, there is glassy membrane when peeling off and damaged defect occurs.
The scheme of patent documentation two, by carrying out the milled processed based on aluminum oxide and oxidation decorations to the contact surface of support glass substrate, after thus the surface roughness Ra of contact surface being adjusted to 2.2nm equably, by the contact surface layer laminated glass film at support glass substrate, produce glass film layers lamination.For glass film layers lamination in patent documentation two, when carrying out clean, film forming process to the surface of glassy membrane, there is the situation that bonding force is insufficient, there is the defect that cannot well position and operate when glassy membrane is peeled off from support glass substrate when processing.
Summary of the invention
The invention provides a kind of glass film layers lamination and manufacture method thereof; for overcoming defect of the prior art; by support glass substrate for glassy membrane provides provide protection; easily glassy membrane peeled off from support glass substrate and make glassy membrane injury-free, and ensureing good location and operation.
The invention provides a kind of glass film layers lamination, comprise stacked support glass substrate and glassy membrane, the edge of described glassy membrane is positioned in the lamination surface of described support glass substrate, have sealing ply between all sides of described glassy membrane and the lamination surface of described support glass substrate, the difference of the surfaceness of the part that the lamination surface of described support glass substrate and the lamination surface of described glassy membrane contact with each other is more than or equal to 1.0nm.
The invention provides a kind of manufacture method of above-mentioned glass film layers lamination, comprise the following steps:
Step 1, is laminated in glassy membrane on support glass substrate; And the difference of the surfaceness of support glass substrate and glassy membrane contact surface is more than or equal to 1.0nm; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of described support glass substrate and glassy membrane is less than 15 × 10
-7/ DEG C;
Step 2, all sides of glassy membrane and the lamination surface of support glass substrate apply sealing material; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of any one in described sealing material and described support glass substrate and glassy membrane is less than 100 × 10
-7/ DEG C;
Step 3, heats the subassembly of above-mentioned glassy membrane and support glass substrate, makes sealing material solidify to form sealing ply.
Glass film layers lamination provided by the invention and manufacture method thereof, when carrying out clean, film forming process to the surface of glassy membrane, because support glass substrate and glassy membrane are bonding well by sealing ply, therefore, it is possible to carry out associating location when manufacturing process, operation without any problems; When being peeled off from support glass substrate by glassy membrane, wipe sealing ply off, can peel off well from uneven surface, the difference of the lamination surface surfaceness contacted with support glass substrate due to glassy membrane is comparatively large, and therefore glassy membrane breakage can not occur.
The contact surface of glassy membrane and supporting glass substrate is provided with the extremely strong seal area of bonding force and is namely provided with the region of sealing ply and the extremely weak vacuum suck district of bonding force and the region between sealing ply and vacuum chamber, therefore by the region that bonding force is extremely strong, can stably implement to manufacture association process under making glassy membrane be laminated in the suprabasil state of supporting glass securely; In addition, owing to having the extremely weak region of bonding force, therefore, it is possible to easily the extremely weak region of glassy membrane from bonding force is peeled off after manufacturing association process, thus, can prevent the bonding force because of supporting glass substrate and glassy membrane cross on the whole strong and glassy membrane that is that cause is peeled off time breakage, and the improper stripping of glassy membrane when can prevent the manufacture association process caused because bonding force is excessively weak on the whole comes off.
Accompanying drawing explanation
The front view of the glass film layers lamination that Fig. 1 provides for the embodiment of the present invention one;
Fig. 2 is along A-A to sectional view in Fig. 1;
The front view of the glass film layers lamination that Fig. 3 provides for the embodiment of the present invention two;
Fig. 4 is along B-B to sectional view in Fig. 3;
Fig. 5 is the front view of support glass substrate in Fig. 3;
Fig. 6 is the structural representation after glassy membrane is taken away by the glass film layers lamination in Fig. 3;
Fig. 7 is the close-up schematic view in Fig. 4;
The sectional view of the glass film layers lamination that Fig. 8 provides for the invention process three.
Embodiment
As shown in Figure 1 and Figure 2, the invention provides a kind of glass film layers lamination, comprise stacked support glass substrate 1 and glassy membrane 2, the edge of glassy membrane 2 is positioned in the lamination surface of support glass substrate 1,
Have sealing ply 3 between all sides of glassy membrane 2 and the lamination surface of support glass substrate, the difference of the surfaceness of the part that the lamination surface of support glass substrate 1 and the lamination surface of glassy membrane 2 contact with each other is more than or equal to 1.0nm.
The manufacture method of the glass film layers lamination of the present embodiment comprises the following steps:
Step 1, is laminated in glassy membrane 2 on support glass substrate 1; And support glass substrate 1 is more than or equal to 1.0nm with the difference of the surfaceness of glassy membrane 2 contact surface; When temperature changes between 25 ~ 300 DEG C, support glass substrate 1 is less than 15 × 10 with the difference of the thermal expansivity of glassy membrane 2
-7/ DEG C;
Step 2, all sides of glassy membrane 2 and the lamination surface of support glass substrate 1 apply sealing material; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of any one in sealing material and support glass substrate and glassy membrane is all less than 100 × 10
-7/ DEG C; The difference of the thermal expansivity of sealing material and support glass substrate is less than 100 × 10
-7/ DEG C, and the difference of the thermal expansivity of sealing material and glassy membrane is less than 100 × 10
-7/ DEG C;
Step 3, heats the subassembly of above-mentioned glassy membrane and support glass substrate, makes sealing material solidify to form sealing ply.
Providing a kind of concrete manufacture method below, is that the transparent sheet glass of the rectangular shape of 500 μm uses as supporting glass using lengthwise 300mm, width 300mm, thickness.A jiao of supporting glass be provided with vertical 3mm, horizontal 3mm the otch 11 of right-angle triangle as plane of orientation.As the glassy membrane be layered on support glass substrate, employ lengthwise 298mm, width 298mm, thickness is the glassy membrane of 100 μm.Support glass substrate and glassy membrane employ the non-alkali glass of Nippon Electric Glass Co., Ltd, and (ProductName: OA-10G, thermal expansivity at 30 ~ 380 DEG C are 38 × 10
-7/ DEG C).To be shaped support glass substrate and glassy membrane by overflow downdraw.The contact surface of support glass substrate applies the fluorspar acid solution of 1%, by this has been roughened process.Coating fluorspar acid solution carried out clean, using fluoric acid treated side as uneven surface after 30 seconds.The surface roughness Ra of the lamination surface on support glass substrate is 1.5nm.The surface roughness Ra of the lamination surface of glassy membrane is 0.2nm.Afterwards, laminated glass film on the contact surface of support glass substrate, coating sintering sealing material, thus obtain the glass film layers lamination of embodiment.For the glass film layers lamination obtained, when carrying out clean, film forming process to the surface of glassy membrane, due to bonding well by sealing ply between support glass substrate with glassy membrane, therefore, it is possible to location when processing without any problems, operation.Because the difference of the surfaceness of two lamination surface is more than or equal to 1.0nm, the bonding force between two surface in contacts is more weak, and when peeling off glassy membrane from support glass substrate thus, can peel off well from uneven surface, glassy membrane breakage can not occur.
The manufacture method of the present embodiment glass film layers lamination is relative to the scheme of patent documentation one, and carry out roughened process to the contact surface of support glass substrate, the surface roughness Ra of the contact surface of support glass substrate and glassy membrane is 0.2nm.The composition of support glass substrate and glassy membrane is not restricted, such as, can use the glass of the various composition such as glass (i.e. soda-lime glass), non-alkali glass containing alkalimetal oxide.The shape of support glass substrate is not restricted, but is preferably rectangle.Wherein, at this, " rectangle " also comprises and is essentially substantially rectangular, cut away the shape at one of them angle, cut away the inclined-plane 11 behind this angle for location, convenient operation.Compatibly use when the lens of the glass substrate that the present invention can use at equipment such as making the flat-panel monitor such as liquid-crystal display or OLED display, solar cell and organic EL illuminating.
Providing several embodiment below, first, is 38 × 10 to long 720mm, wide 600mm, thickness of slab 0.4mm, thermal expansivity
-7/ DEG C support glass substrate (Asahi Glass Co., Ltd manufacture, AN100) and corresponding glassy membrane carry out pure water cleaning, UV cleaning and surface is become clean.By stacked for both sides glass; Then, utilize silk screen printing to take width as 0.6mm and in frame shape, category of glass seal, sealing materials be printed on the circumference of glassy membrane; Then, with 430 DEG C, 10 minutes are heated to layer glass in an atmosphere, sintered glass class seal, sealing materials.
Screen process press can also be utilized by solvent-free addition reaction-type organosilicon (organosilicon company of SHIN-ETSU HANTOTAI manufactures, KNS-320A, viscosity: 0.40Pas)) mixture of 100 mass parts and platinum class catalyzer (organosilicon company of SHIN-ETSU HANTOTAI manufactures, CAT-PL-56) two mass parts is coated on the circumference of glassy membrane and is laminated on support glass substrate by glassy membrane.Then, with 180 DEG C, 30 minutes are heated to support glass substrate in an atmosphere, make the mixture solidified of solvent-free addition reaction-type organosilicon and platinum class catalyzer, obtain encapsulated with silicone resin material.Then, in an atmosphere with 450 DEG C to glass film layers lamination heat treated one hour.
In addition, for the glass laminated class prepared in addition, under a reduced pressure (1.0 × 10
-5pa) from room temperature to 450 DEG C, gas is not produced from glass film layers lamination.Then, as the resin for the formation of sealing ply, employ and at two ends, there is the straight-chain polysiloxane (Arakawa Chemical Industries, Ltd. manufacture, trade(brand)name " 8500 ") of vinyl and there is the methyl hydrogen siloxane (Arakawa Chemical Industries, Ltd. manufactures, trade(brand)name " 12031 ") of hydrogen silyl in molecule.Then, by it, (Arakawa Chemical Industries, Ltd. manufactures, trade(brand)name " CAT12070 ") mixes mutually with platinum class catalyzer, pentane is utilized to dilute further, prepare the mixture that solids component accounts for 50%, by extrusion coated in glassy membrane side, it within 30 minutes, is made to be solidified to form encapsulated with silicone resin material with 250 DEG C of heating in an atmosphere.At this, the mode becoming 1:1 with the mol ratio of hydrogen silyl and vinyl adjusts the ratio of mixture of straight-chain polysiloxane and methyl hydrogen siloxane.The platinum class catalyzer of five mass parts is added relative to total 100 mass parts of straight-chain polysiloxane and methyl hydrogen siloxane.
Usually, if glass plies gathered into folds, in lamination surface, glass surface is bonded to each other and with bonding force close contact to a certain degree, thinks that this bonding force is produced by the Van der Waals force etc. between the generation of silanol base (Si-OH) chemical bond that hydrogen combines or dehydrating condensation locally causes each other being present in two glass surfaces, two glass surfaces.The difference of the surfaceness of preferred support glass substrate and glassy membrane contact surface is greater than 1.0nm.If the surfaceness average deviation of two lamination surface is more than 1.0nm, then the substantial contact area on two surfaces is too small, therefore can not make two face close contacts with sufficient bonding force, is easy to peel off.
Preferably, temperature is 25 DEG C ~ 300 DEG C time, and the difference of the thermal expansivity of support glass substrate and glassy membrane is 15 × 10
-7/ DEG C below.Temperature is 25 DEG C ~ 300 DEG C time, and the difference of the thermal expansivity of sealing material and support glass substrate is 100 × 10
-7/ DEG C below, the difference of the thermal expansivity of sealing material and glassy membrane is 100 × 10
-7/ DEG C below.
The thermal expansivity of support glass substrate can be identical in fact with glassy membrane, also can be different.If identical in fact, then when heat-treating duplexer of the present invention, glassy membrane or support glass substrate not easily produce warpage.The difference of the thermal expansivity of glassy membrane and support glass substrate is preferably 300 × 10
-7/ DEG C below, be more preferably 100 × 10
-7/ DEG C below, more preferably 15 × 10
-7/ DEG C below.Glassy membrane and support glass substrate can be the glass of identical material.In this case, the difference of the thermal expansivity of two glass is 0.The composition of support glass substrate such as can be identical with alkali glass, non-alkali glass.Wherein, the preferred non-alkali glass because percent thermal shrinkage is less.
In addition, manufacture the method for glassy membrane and support glass substrate and be restricted especially, known method can be adopted.Such as, after obtaining melten glass in the known glass raw material of fusing, drawing method, traction method again etc. under utilizing float glass process, scorification, crystal pulling method, discharge orifice is configured as tabular, can obtain glassy membrane and support glass substrate.Wherein category of glass seal, sealing materials can be lead glass, borate glass, zinc glass, vanadate glass, tellurate glass, stibnate glass etc., if consider relative to glassy membrane and seal (binding property), its reliability (adhesion reliability, stopping property) of support glass substrate and the impact property etc. for environment, human body, preferred tin-phosphoric acid class glass, bismuth class glass.
Above-mentioned sealing material be acrylic resin, polyolefin resin, polyurethane based resin, silicone based resin, polyamide-based resin, polyimide based resin, polyether-ether-ketone resinoid, polyphenylene ether group resin, poly (arylene ether) system resin, redix, silicone elastomer, silicone elastomer, fluorosilicone elastomerics or Perfluoroelastomer.Category of glass sealing material is the glass of melt temperature between 300 ~ 750 DEG C.
As the resin for forming sealing material, be not restricted especially as mentioned above, but based on excellent heat resistance and relative to the excellent such reason of the rippability of glassy membrane, preferred silicone resin.In addition, even if process the also deteriorated hardly aspect of 1 hours, rippability based on such as about 400 DEG C, also preferred silicone resin.
The melt temperature of the category of glass seal, sealing materials of acquisition like this is preferably 400 DEG C ~ 750 DEG C, is more preferably 500 DEG C ~ 700 DEG C/DEG C.And, be preferably 20 × 10 containing the thermal expansivity after category of glass seal, sealing materials sintering
-7~ 250 × 10
-7/ DEG C.
As the known method used when being coated with sealing material, extrusion coated method, print roll coating method, bar shaped coating method, silk screen print method, gravure coating process etc. can be listed, suitably can select according to the kind of sealing material.Such as, the known methods such as extrusion coated method are utilized to be coated on the surface of support glass substrate by the resin combination containing organosilicon (host), linking agent and catalyzer, carrying out heating afterwards makes it solidify, and the dimethyl of this organosilicon (host) containing straight-chain in molecule gathers silica a heatable brick bed.By being heating and curing, the surface chemistries ground of resin and support glass substrate combines.
The condition that is heating and curing is also different because of the use level difference of catalyzer.Such as, when total amount 100 mass parts relative to host and linking agent has coordinated the platinum class catalyzer of two mass parts, preferably in an atmosphere to react with 50 DEG C ~ 300 DEG C, more preferably reacted with 100 DEG C ~ 250 DEG C.In addition, the reaction times is preferably 5 minutes ~ 60 minutes, is more preferably 10 minutes ~ 30 minutes.
In order to be set to by sealing ply, there is the metastatic silicone resin of low organosilicon, preferably be cured reaction in the mode not remaining unreacted silicone ingredients in silicone resin as far as possible.If temperature of reaction as above and reaction times, then can make not remain unreacted silicone ingredients in silicone resin, so preferably.When long compared with the above-mentioned reaction times or temperature of reaction is too high, carry out the oxygenolysis of silicone resin simultaneously and generate low-molecular-weight silicone ingredients, organosilicon transitivity likely increases.From in order to make the angle that the rippability after heat treated is good, it is also preferred for being cured reaction in the mode not remaining unreacted silicone ingredients in silicone resin as far as possible.
In addition, when making glass film layers be stacked on support glass substrate, silicone resin combines with the surface of support glass substrate by means of anchoring effect, is fixed more firmly.As the sintering of category of glass sealing material, specifically, the sintering undertaken by process furnace, the sintering etc. undertaken by laser radiation can such as be listed.
Sealing ply 3 comprises the polyimide of aromatic diamines and the aromatic tetracarboxylic acid's acid anhydride class polycondensation making to have benzoxazole structure.Preferred sealing ply only comprises above-mentioned polyimide.Above-mentioned " polycondensation " is carried out as follows, first, in a solvent, by Diamines and tetracarboxylic anhydride class for open loop polyaddition reaction, obtains polyamic acid solution, then, by this polyamic acid solution, after forming base film etc. as required, carries out dehydrating condensation (imidization).As long as the solvent used when making Diamines and tetracarboxylic anhydride Type of Collective obtain polyamic acid makes the material all dissolved as the monomer of raw material and the polyamic acid of generation just be not particularly limited, preferred polar organic solvent, such as, can list: METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO), hempa acid amide, ethyl cellosolve acetate, diethylene glycol dimethyl ether etc.These solvents can be used alone or used in combination.The usage quantity of solvent is the amount being enough to the monomer as raw material is dissolved, and as concrete usage quantity, the mass percent that can list monomer total mass shared in the solution being dissolved with monomer is generally 5 ~ 40%, preferably 10 ~ 30%.Condition for the polyreaction (hereinafter also referred to as " polyreaction ") obtaining polyamic acid uses known condition, as concrete example, can list in organic solvent 0 ~ 80 DEG C temperature range continuously stirring and/or mixing 10 minutes ~ 30 hours.Also polyreaction can be made as required to carry out stage by stage or elevate the temperature or reduce.In this situation, the order of addition of two kinds of monomers is not particularly limited, and preferably in the solution of aromatic diamines, adds aromatic tetracarboxylic acid's acid anhydride class.The mass percent of polyamic acid shared by the polyamic acid solution obtained by polyreaction is preferably 5 ~ 50%, is more preferably 10 ~ 30%, the viscosity of above-mentioned solution is in the mensuration utilizing cloth viscometer to carry out (25 DEG C), be preferably 10 ~ 2000Pas from the viewpoint of the stability of liquor charging, be more preferably 100 ~ 1000Pas.Carrying out vacuum defoamation in the polymerization, is effective for the organic solvent solution of the polyamic acid manufacturing high-quality.In addition, a small amount of end-capping reagent can be added before polymerization in aromatic diamines and control polymerization.As end-capping reagent, the compound that maleic anhydride etc. has carbon-carbon double bond can be listed.Usage quantity during use maleic anhydride preferably every 1 mole of aromatic diamines is 0.001 ~ 1.0 mole.
Above-described embodiment is applicable to electricity field, and the thickness of support glass substrate is between 0.08mm to 1.3mm, and the thickness of glassy membrane is between 0.01mm to 1.1mm.
Above-described embodiment has following three kinds of preferred implementations:
Embodiment one
As shown in Figure 1 and Figure 2, glass film layers laminate structure: roughened process is carried out to the lamination surface of support glass substrate or the lamination surface of glassy membrane, the difference of the surfaceness of two lamination surface is increased, be easy to peel off, but preferred version carries out roughened process to the lamination surface of support glass substrate, because its opposing glass film is thicker, be easy to roughened process.
The manufacture method of glass film layers lamination is as follows:
Step 1A, carries out roughened process to the lamination surface 12 of support glass substrate;
Step 1B, is compound in glassy membrane 2 in the lamination surface 12 of support glass substrate; And the difference of the surfaceness of support glass substrate and glassy membrane contact surface is more than or equal to 1.0nm; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of support glass substrate and glassy membrane is less than 15 × 10
-7/ DEG C;
Step 2, all sides of glassy membrane and the lamination surface of support glass substrate apply sealing material; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of any one in sealing material and support glass substrate and glassy membrane is less than 100 × 10
-7/ DEG C;
Step 3, heats the subassembly of above-mentioned glassy membrane and support glass substrate, makes sealing material solidify to form sealing ply 3.
Above-mentioned roughened process can be from the etch processes based on fluoric acid, the etch processes based on atmospheric pressure plasma, based thin film formed roughened, based on sandblasting roughened process, based on grinding formed roughened, based on surface modification formed roughened one or more process.
Embodiment two
As shown in fig. 3 to 7, glass film layers laminate structure: the lamination surface of support glass substrate is provided with the seal area of enclosed shape and encloses the vacuum suck district 30 be placed in sealing district, is provided with many grooves communicated with each other 10 in vacuum suck district 30; Jointly form vacuum chamber 20 between groove 10 and glassy membrane 2, seal area has the sealing ply 3 for sealed vacuum chamber 20.
The manufacture method of glass film layers lamination is as follows:
Step 1C, the lamination surface of described support glass substrate divides the seal area in closed and encloses the vacuum suck district 30 of putting with sealing district, the edge shape of seal area and glassy membrane 2 is suitable; When temperature changes between 25 ~ 300 DEG C, support glass substrate 1 is less than 15 × 10 with the difference of the thermal expansivity of glassy membrane 2
-7/ DEG C;
Step 1D, offers many grooves communicated with each other 10 in this vacuum suck district 30;
Step 1E, is compound in glassy membrane in the lamination surface of above-mentioned support glass substrate, and makes glassy membrane cover all above-mentioned grooves completely;
Step 2, all sides of glassy membrane and the lamination surface of support glass substrate apply sealing material; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of any one in sealing material and support glass substrate and glassy membrane is less than 100 × 10
-7/ DEG C;
Step 3, heats the subassembly of above-mentioned glassy membrane and support glass substrate in vacuum environment, makes sealing material solidify to form sealing ply 3.Air in heat-processed further groove can be overflowed by uncured sealing material.
Glass film layers lamination provided by the invention, the contact surface of glassy membrane and supporting glass substrate is provided with the extremely strong sealing area of bonding force and is namely provided with the seal area of sealing ply 3 and the extremely weak lamination area of bonding force and the vacuum suck district 30 between sealing ply 3 and vacuum chamber 20, therefore by the region that bonding force is extremely strong, can stably implement to manufacture association process under making glassy membrane be laminated in the suprabasil state of supporting glass securely; In addition, owing to having the extremely weak region of bonding force, therefore, it is possible to easily the extremely weak region of glassy membrane from bonding force is peeled off after manufacturing association process, thus, can prevent the bonding force because of supporting glass substrate and glassy membrane cross on the whole strong and glassy membrane that is that cause is peeled off time breakage, and the improper stripping of glassy membrane when can prevent the manufacture association process caused because bonding force is excessively weak on the whole comes off.
As the optimal way of embodiment two, the surface of support glass substrate and glassy membrane edge contact is also provided with multiple depression 40, depression 40 is all communicated with by groove 10, is filled with the sealing material for the formation of sealing ply 3 in depression 40.Sealing material is one in bismuth class glass, vanadium class glass, antimony class glass, tellurium class glass, plumbous class glass, phosphate glass or its mixture.Be filled in by sealing material in depression 40, what be convenient to deposit with sealing ply is shaping.
By arranging the structure of discontinuous depression at above-mentioned support glass substrate in the circumference of the one side contacted with above-mentioned glassy membrane, can be more prone to and reliably peel off glassy membrane and support glass substrate, thus, can prevent the bonding force because of support glass substrate and glassy membrane cross on the whole strong and glassy membrane that is that cause is peeled off time breakage, and the improper stripping of glassy membrane when can prevent the manufacture association process caused because bonding force is excessively weak on the whole comes off.Upper strata glassy membrane can be whole piece glass, and also can be that multi-disc rectangular glass is spliced, sealing material be centered around the side of every sheet rectangular glass.
In order to ensure the intensity of support glass substrate, the degree of depth of depression 40 and groove 10 is all less than the half of support glass substrate 1 thickness.
As the preferred implementation of above-described embodiment, groove 10 comprises many continuous grooves and the connecting groove 10c being communicated with continuous groove.The shape of continuous groove and connecting groove can cross polyline shaped etc. for linearity, curve-like, does not limit at this.In the present embodiment, glassy membrane 2 is rectangular, and continuous groove is alternately connected stepped by transverse concave groove 10a with longitudinal fluting 10b from beginning to end, and the both ends of continuous groove form depression 40.Structure is simple, is easy to make.
On the basis of above-described embodiment, for ensureing the intensity of support glass substrate further, the all transverse concave groove 10a length sums be located along the same line are less than the half of the horizontal length of side of glassy membrane, and all longitudinal fluting 10b length sums be located along the same line are less than the half of longitudinal length of side of glassy membrane.In the present embodiment, the widthwise edge of transverse concave groove 10a and glassy membrane be arranged in parallel, and the longitudinal sides parallel of longitudinal fluting 10b and glassy membrane is arranged, and, continuous groove transverse concave groove and transverse concave groove when arranging are located along the same line, and longitudinal fluting and longitudinal fluting are located along the same line.The more weak lamination area glassy membrane of bonding force is more balanced with the bonding force between support glass substrate, and the forming of glass film layers lamination, not easily departs from.
The manufacture method of the plywood preferred version in embodiment two is as follows:
Step 1C, the lamination surface of support glass substrate divides the seal area in closed and encloses the vacuum suck district 30 of putting with sealing district, the edge shape of seal area and glassy membrane is suitable; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of support glass substrate and glassy membrane is less than 15 × 10
-7/ DEG C;
Step 1D, offers many grooves communicated with each other 10 in this vacuum suck district 30; Multiple depression is offered in described seal area, and depression is all communicated with by described groove;
Step 1D ', packing matcrial in depression; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of any one in sealing material and support glass substrate and glassy membrane is less than 100 × 10
-7/ DEG C;
Step 1E, is compound in glassy membrane in the lamination surface of above-mentioned support glass substrate, and makes glassy membrane 2 cover all above-mentioned grooves 10 completely;
Step 2, all sides of glassy membrane and the lamination surface of support glass substrate apply sealing material; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of any one in described sealing material and described support glass substrate and glassy membrane is less than 100 × 10
-7/ DEG C;
Step 3, heats the subassembly of above-mentioned glassy membrane and support glass substrate in vacuum environment, makes sealing material solidify to form sealing ply 3.
Making the air pressure in layer glass be in room temperature to the temperature range of above-mentioned two panels strain point of glass at above-mentioned glass film layers lamination is 10
4~ 10
-5between Pa, stably implement under the state making glassy membrane be laminated on support glass substrate securely further by vacuum adsorption force to manufacture association process.
Glassy membrane and the stacked method of support glass substrate are not restricted especially, if utilize vacuum layer platen press or vacuum-pressure processes to crimp, then can suppress being mixed into of bubble better, guarantee good close contact, so more preferably.By crimping under vacuo, even if when remaining the bubble of trace, bubble also can not increase because of heating, also has the advantage not easily causing the flex failure of glassy membrane such.Glass film layers lamination of the present invention forms preferably by laminated glass film under reduced atmosphere and support glass substrate manufacture.Below, this layered manner is called decompression layered manner.Reduced atmosphere refers to, if by atmospheric level cancellation, then pressure is preferably below-60kPa, is more preferably below-100kPa.In other words, if not by atmospheric level cancellation, then reduced atmosphere is that finger pressure is preferably below 41.3kPa, is more preferably below 1.3kPa.
Embodiment three
As shown in Figure 8, glass film layers laminate structure: the lamination surface of support glass substrate has plated film, plated film is the mineral membrane 4 of thickness between lnm ~ 10000nm, and glassy membrane 2 is stacked and placed on mineral membrane 4, and sealing ply 3 is sealed between mineral membrane 4 and all sides of glassy membrane.
Glass film layers lamination manufacture method,
Step 1F, plated film in the lamination surface of support glass substrate, this film is the mineral membrane 4 of thickness between lnm ~ 10000nm;
Step 1G, is compound in glassy membrane 2 on mineral membrane 4; And support glass substrate 1 is more than or equal to 1.0nm with the difference of the surfaceness of glassy membrane contact surface; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of described support glass substrate and glassy membrane is less than 15 × 10
-7/ DEG C;
Step 2, all sides and mineral membrane 4 of glassy membrane apply sealing material; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of any one in sealing material and support glass substrate and glassy membrane is less than 100 × 10
-7/ DEG C;
Step 3, heats the subassembly of above-mentioned glassy membrane and support glass substrate, makes sealing material solidify to form sealing ply 3.
Support glass substrate can form one deck plated film, and plated film can select thickness to be the mineral membrane of lnm ~ 10000nm.In order to control film forming cost, thickness is more few more favourable, is more preferably lnm ~ 1000nm, most preferably is lnm ~ 200nm.Mineral membrane is by being selected from ITO, Ti, Si, Au, Ag, Al, Cr, Cu, Mg, Ti, SiO, SiO
2, AI
2o
3, MgO, Y
2o
3, La
2o
3, Pr
6o
11, SC
2o
3, WO
3, HfO
2, In
2o
3, ZrO
2, Nd
2o
3, Ta
2o
5, CeO
2, Nb
2o
5, TiO, TiO
2, Ti
3o
5, one in NiO, ZnO or two or more formation.Mineral membrane is more preferably sull.Sull is thermally-stabilised.Therefore, by arranging sull on support glass substrate, even if carry out the process of heat tracing to glass film layers lamination, also can the membrane support glass substrate of Reusability as sull, preferably use SiO, SiO
2, AI
2o
3, MgO, Y
2o
3, La
2o
3, Pr
6o
11, SC
2o
3, WO
3, HfO
2, In
2o
3, ZrO
2, Nd
2o
3, Ta
2o
5, CeO
2, Nb
2o
5, TiO, TiO
2, Ti
3o
5, NiO, ZnO and their combination.
Support glass substrate only forms one deck mineral membrane, but also can form mineral membrane by multilayer.Now, the layer that outermost layer contacts with glassy membrane is preferably sull.As mentioned above, this is because sull is heat-staple.Also can in order to use the two sides of support glass substrate, with the surface of above-mentioned surperficial opposition side on also can form mineral membrane.In addition, also mineral membrane can be formed on the whole surface of support glass substrate.Become film unit can use known method, sputtering method, vapour deposition method, CVD, sol-gel method etc. can be used.In addition, the width in the region for the formation of groove of the downside of glassy membrane circumference, preferably from the outer rim 0.5mm ~ 100mm to the inside of glassy membrane, is more preferably 0.5mm ~ 50mm, more preferably 0.5mm ~ 10mm, is further preferably 0.5mm ~ 1mm.If support glass substrate is comparatively large, then preferably width is also larger.Support glass substrate is more bigger than glassy membrane, during device processes it by protective glass film from edge impact.Such as, this carrier can slightly large 5mm, and carries out precision work, rounding or grinding to its edge, to allow the typical impact stood in equipment making equipment.In addition, support glass substrate can have the geometrical shape different from glassy membrane.In addition, support glass substrate can have surface characteristic or groove, sealing material is bonded or location.When support glass substrate and glassy membrane are bonded together by sealing material, the hardness of combination is compatible with typical treatment facility.
Treatment condition required by later step, the sealing material between support glass substrate and glassy membrane can be such as organic radical tackiness agent, elastomerics or inorganic bond layer.In certain embodiments, advantageously, bonding agent layer is elastomerics, especially inorganic, elastic body, and described elastomeric embodiment comprises silicone elastomer, the intoxicated elastomerics of fluorine silicon and Perfluoroelastomer.Certainly, Perfluoroelastomer is suitable for many application especially well, because hydrogen atom is all substituted by fluorine atom by they, and they realize completely crosslinked ability, this causes low-level degassed and high-caliber thermostability and chemical stability jointly, and such as thermostability is up to 400 DEG C and than silicon and the higher chemical durability of fluorosilicone.According to the composition of functional substrate and carrier substrates, Perfluoroelastomer can present higher than silicone elastomer in conjunction with energy, and this is additional advantage for some application.
Once define the assembly comprising support glass substrate and the glassy membrane engaged by sealing material, then the mode process that the non-planar contact surfaces of glassy membrane can be similar to the single thick support glass substrate for having component thickness.Described process can include, but are not limited to thickness reduction, surface modifications (such as, surface finish, alligatoring, film deposit, etch, through raying, are bonded to additional substrate or film etc.), and makes functional component thereon.Several functions parts can be formed on the non-planar contact surfaces of support glass substrate.Functional component can comprise optical device, mechanical means, electric equipment or their combination or mixing.The non-limiting example of optics comprises: indicating meter, colour filter, slab guide, slab guide parts and equipment, lens, optical amplifier, multiplexer, demultplexer etc.The non-limiting example of mechanical part comprises: MEMS, valve etc.The non-limiting example of electricity parts comprises: transistor, diode, electrical condenser, resistor, inducer, antenna, transceiver, conductor, sensor, optical diode, and their combination and mixing etc.Functional component can be material function layer or its part.Such as, functional layer can be single silicon layer (non-crystalline state, polycrystal or single crystal).Person of ordinary skill in the relevant knows for making treatment condition required by described functional component and material on the non-planar contact surfaces of support glass substrate.During the step forming functional component, assembly can stand the radiation of high temperature, various chemical solution, steam, various energy level and dosage, mechanical vibration, machine washing, brushing, acceleration and deceleration etc.The selected material applying to bonding agent of high expectations, and the bonding strength between bonding agent and two support glass substrate can stand described treatment condition.
The advantage of silicone elastomer is, by changing the consumption of linking agent in solidification process, can regulate their level of adhesion easily.But unreacted linking agent and/or low molecular weight substance may produce unacceptable exhaust level in the manufacturing processed of electronic unit in the finished product.As discussed above, Perfluoroelastomer can not cause exhausting problem usually.
Last it is noted that above each embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to foregoing embodiments to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein some or all of technical characteristic; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.
Claims (9)
1. a glass film layers lamination, comprise stacked support glass substrate and glassy membrane, the edge of described glassy membrane is positioned in the lamination surface of described support glass substrate, it is characterized in that, have sealing ply between all sides of described glassy membrane and the lamination surface of described support glass substrate, the difference of the surfaceness of the part that the lamination surface of described support glass substrate and the lamination surface of described glassy membrane contact with each other is more than or equal to 1.0nm; Wherein, the lamination surface of described support glass substrate is provided with the seal area of enclosed shape and encloses the vacuum suck district be placed in sealing district, is provided with many grooves communicated with each other in described vacuum suck district; Jointly form vacuum chamber between described groove and described glassy membrane, there is in described seal area the described sealing ply for sealing described vacuum chamber; Described seal area is provided with multiple depression, and described depression is all communicated with by described groove, is filled with the sealing material for the formation of described sealing ply in described depression.
2. glass film layers lamination according to claim 1, is characterized in that, the degree of depth of described depression and groove is all less than the half of described support glass substrate thickness.
3. glass film layers lamination according to claim 2, is characterized in that, described groove comprises many continuous grooves and the connecting groove being communicated with described continuous groove.
4. glass film layers lamination according to claim 3, is characterized in that, described glassy membrane is rectangular, and described continuous groove is alternately connected stepped by transverse concave groove with longitudinal fluting from beginning to end, and the both ends of described continuous groove form described depression; The all described transverse concave groove length sum be located along the same line is less than the half of the horizontal length of side of described glassy membrane, and all longitudinal fluting length sums be located along the same line are less than the half of longitudinal length of side of described glassy membrane.
5. glass film layers lamination according to claim 1, it is characterized in that, the lamination surface of described support glass substrate have the mineral membrane of thickness between lnm ~ 10000nm, described glassy membrane is stacked and placed on described mineral membrane, and described sealing ply is sealed between described mineral membrane and all sides of described glassy membrane.
6. a manufacture method for the arbitrary described glass film layers lamination of the claims 1-5, is characterized in that, comprise the following steps:
Step 1, carries out roughened process to the lamination surface of described support glass substrate; Described glassy membrane is compound in the lamination surface of described support glass substrate; And the difference of the surfaceness of support glass substrate and glassy membrane contact surface is more than or equal to 1.0nm; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of described support glass substrate and glassy membrane is less than 15 × 10
-7/ DEG C;
Step 2, all sides of glassy membrane and the lamination surface of support glass substrate apply sealing material; When temperature changes between 25 ~ 300 DEG C, the difference of the thermal expansivity of any one in described sealing material and described support glass substrate and glassy membrane is less than 100 × 10
-7/ DEG C;
Step 3, heats the subassembly of above-mentioned glassy membrane and support glass substrate, makes sealing material solidify to form sealing ply.
7. the manufacture method of glass film layers lamination according to claim 6, is characterized in that, described step 1 comprises the following steps:
Step 1C, the lamination surface of described support glass substrate divides the seal area in closed and encloses the vacuum suck district be placed in sealing district, the edge shape of described seal area and described glassy membrane is suitable;
Step 1D, offers many grooves communicated with each other in this vacuum suck district;
Step 1E, is compound in glassy membrane in the lamination surface of above-mentioned support glass substrate, and makes described glassy membrane cover all above-mentioned grooves completely.
8. the manufacture method of glass film layers lamination according to claim 6, is characterized in that,
Described step 1D also comprises: on described seal area, offer multiple depression, and described depression is all communicated with by described groove;
Also comprise between described step 1D and step 1E:
Step 1D ', packing matcrial in described depression.
9. the manufacture method of glass film layers lamination according to claim 6, is characterized in that, described step 1 comprises the following steps:
Step 1F, plated film in the lamination surface of described support glass substrate, this film is the mineral membrane of thickness between lnm ~ 10000nm;
Step 1G, is compound in described glassy membrane on described mineral membrane;
Step 2 is specially, and all sides and described mineral membrane of glassy membrane apply described sealing material.
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| PCT/CN2014/084041 WO2015018370A1 (en) | 2013-08-09 | 2014-08-08 | Glass film laminate and manufacturing method therefor |
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| CN105093595A (en) * | 2015-09-24 | 2015-11-25 | 京东方科技集团股份有限公司 | Carrying body, preparation method of ultrathin display panel and display device |
| CN105415808B (en) * | 2015-11-05 | 2017-08-18 | 金弼 | A kind of vacuum glass and preparation method thereof |
| CN105271835A (en) * | 2015-11-17 | 2016-01-27 | 湖南普照爱伯乐平板显示器件有限公司 | Attaching method for flexible glass |
| JP2018035008A (en) * | 2016-08-29 | 2018-03-08 | 日本電気硝子株式会社 | Joined body and production method thereof |
| JP7085414B2 (en) * | 2018-06-14 | 2022-06-16 | 住友化学株式会社 | Liquid crystal film manufacturing method and optical laminate manufacturing method |
| CN109461845A (en) * | 2018-10-17 | 2019-03-12 | 武汉华星光电半导体显示技术有限公司 | The production method of flexible substrate, flexible display panels and flexible display panels |
| JP7211914B2 (en) * | 2019-08-29 | 2023-01-24 | 矢崎総業株式会社 | shield connector |
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| EP2511092B1 (en) * | 2010-07-28 | 2015-01-28 | Nippon Electric Glass Co., Ltd. | Glass film laminate |
| CN103435257B (en) * | 2013-08-09 | 2016-04-27 | 刘国正 | Glass film layers lamination and manufacture method thereof |
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