WO2022186338A1 - 合わせガラス、及び合わせガラスの製造方法 - Google Patents
合わせガラス、及び合わせガラスの製造方法 Download PDFInfo
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- WO2022186338A1 WO2022186338A1 PCT/JP2022/009142 JP2022009142W WO2022186338A1 WO 2022186338 A1 WO2022186338 A1 WO 2022186338A1 JP 2022009142 W JP2022009142 W JP 2022009142W WO 2022186338 A1 WO2022186338 A1 WO 2022186338A1
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- adhesive layer
- laminated glass
- layer
- glass substrate
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- 238000004519 manufacturing process Methods 0.000 title claims description 30
- 239000012790 adhesive layer Substances 0.000 claims abstract description 177
- 239000010410 layer Substances 0.000 claims abstract description 144
- 239000011521 glass Substances 0.000 claims abstract description 111
- 239000000758 substrate Substances 0.000 claims description 114
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- 238000000034 method Methods 0.000 description 20
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- 125000000524 functional group Chemical group 0.000 description 5
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- 239000002904 solvent Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000004049 embossing Methods 0.000 description 4
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- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 239000012792 core layer Substances 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
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- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- PRKPGWQEKNEVEU-UHFFFAOYSA-N 4-methyl-n-(3-triethoxysilylpropyl)pentan-2-imine Chemical compound CCO[Si](OCC)(OCC)CCCN=C(C)CC(C)C PRKPGWQEKNEVEU-UHFFFAOYSA-N 0.000 description 1
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- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical class CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
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- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
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- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- QYJYJTDXBIYRHH-UHFFFAOYSA-N trimethoxy-[8-(oxiran-2-ylmethoxy)octyl]silane Chemical compound C(C1CO1)OCCCCCCCC[Si](OC)(OC)OC QYJYJTDXBIYRHH-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60J—WINDOWS, WINDSCREENS, NON-FIXED ROOFS, DOORS, OR SIMILAR DEVICES FOR VEHICLES; REMOVABLE EXTERNAL PROTECTIVE COVERINGS SPECIALLY ADAPTED FOR VEHICLES
- B60J1/00—Windows; Windscreens; Accessories therefor
Definitions
- the present invention relates to laminated glass and a method for manufacturing laminated glass.
- Patent Literature 1 describes a laminated glass in which a half mirror is provided between an inner glass and an outer glass.
- a laminated glass that displays such a HUD image is required to suppress deterioration in the visibility of the displayed HUD image.
- laminated glass is also required to reduce the degree of falling off of fragments when impacted.
- the present invention has been made in view of the above problems, and a laminated glass capable of suppressing a decrease in visibility of a HUD image and reducing the degree of falling off of fragments when receiving an impact, and the laminated glass. It aims at providing the manufacturing method of.
- the laminated glass according to the present disclosure is provided with a first glass substrate, a second glass substrate, and between the first glass substrate and the second glass substrate. and an adhesive layer provided between the second glass substrate and the reflective layer for bonding the second glass substrate and the reflective layer, wherein the adhesive layer has a thickness of 2 ⁇ m or more and 25 ⁇ m or less and contains siloxane bonds.
- a method for manufacturing laminated glass according to the present disclosure uses a resin material and a silane compound to form an adhesive layer having a thickness of 30 ⁇ m or less and containing a siloxane bond. and laminating the first glass substrate, the reflective layer, the adhesive layer, and the second glass substrate to form a laminated glass.
- the present invention it is possible to reduce the degree of falling off of fragments when receiving an impact while suppressing deterioration in the visibility of the HUD image.
- FIG. 1 is a schematic diagram of a laminated glass according to this embodiment.
- FIG. 2 is a schematic cross-sectional view of the laminated glass according to this embodiment.
- FIG. 3 is a diagram for explaining the bubble residual rate.
- FIG. 4 is a diagram for explaining a method for manufacturing an adhesive layer.
- FIG. 5 is a schematic diagram showing an adhesive layer before lamination.
- FIG. 6 is a diagram illustrating a method for manufacturing laminated glass.
- FIG. 1 is a schematic diagram of a laminated glass according to this embodiment.
- a laminated glass 1 according to the present embodiment shown in FIG. 1 is mounted on a vehicle.
- the laminated glass 1 is a window member applied to a windshield of a vehicle, in other words, it is used as a front window of the vehicle, in other words, a windshield.
- the inside of a vehicle refers to, for example, a vehicle interior in which a driver's seat is provided.
- the application of the laminated glass 1 is not limited to the windshield of the vehicle, and can be applied to other parts of the vehicle.
- the upper edge of the laminated glass 1 will be referred to as upper edge portion 1a, the lower edge as lower edge portion 1b, one side edge as side edge portion 1c, and the other side edge as side edge portion 1d.
- the upper edge portion 1a is an edge portion positioned vertically upward when the laminated glass 1 is mounted on a vehicle.
- the lower edge portion 1b is an edge portion located on the lower side in the vertical direction when the laminated glass 1 is mounted on a vehicle.
- the side edge portion 1c is an edge portion positioned on one side when the laminated glass 1 is mounted on a vehicle.
- the side edge portion 1d is an edge portion located on the other side when the laminated glass 1 is mounted on a vehicle.
- the direction from the lower edge portion 1b to the upper edge portion 1a is defined as the Y direction (longitudinal direction), and the direction from the side edge portion 1c to the side edge portion 1d is defined as The X direction (horizontal direction).
- the X direction and the Y direction are orthogonal.
- the direction orthogonal to the surface of the laminated glass 1, in other words, the thickness direction of the laminated glass 1 is defined as the Z direction.
- the Z direction is, for example, the direction from the outside to the inside of the vehicle when the laminated glass 1 is mounted on the vehicle.
- the X direction and the Y direction are along the surface of the laminated glass 1, for example, when the surface of the laminated glass 1 is curved, they are the directions that contact the surface of the laminated glass 1 at the center point O of the laminated glass 1. may Note that the center point O is the center position of the laminated glass 1 when the laminated glass 1 is viewed from the Z direction.
- the laminated glass 1 has a light transmission area A1 and a light shielding area A2.
- the translucent area A1 is an area that occupies the central portion of the laminated glass 1 when viewed from the Z direction, and is an area for ensuring the driver's visual field.
- the translucent area A1 is an area that transmits visible light.
- the light shielding area A2 is an area formed around the light transmitting area A1 when viewed from the Z direction.
- the light shielding area A2 is an area that shields visible light.
- Within the light shielding area A2 there are formed a far-infrared transmission area in which far-infrared rays are transmitted and a far-infrared camera is installed, and a visible light transmission area in which visible light is transmitted and a visible-light camera is installed.
- a HUD area AH is formed in the translucent area A1.
- the HUD area AH is an area irradiated with light from a projection device (not shown), and an area where a HUD image, which is an image projected from the projection device, is displayed.
- the projection device is a device that projects an HUD image onto the laminated glass 1, that is, a projector, for example.
- the projection device is provided at a position overlapping the HUD area AH when viewed from the optical axis direction of the projection device.
- the HUD area AH is formed on the X direction side of the center point O, and is formed on the side edge portion 1d side and the lower edge portion 1b side of the center point O in the example of FIG.
- the position and size of the HUD area AH are arbitrary, and may be formed closer to the side edge 1c than the center point O, for example. Also, a plurality of HUD areas AH may be formed.
- the HUD area AH is an eye box based on SAE-J1757-2 (2016), and when the mirror that constitutes the HUD placed in the vehicle is rotated, the light from the mirror that constitutes the HUD hits the windshield. It can also be said that it is the range to be irradiated.
- the laminated glass 1 preferably has a curvature radius of 20000 mm or less in the Y direction (longitudinal direction), more preferably 4000 mm or more. More preferably, the laminated glass 1 has a curvature radius of 6000 mm or more and 20000 mm or less in the Y direction.
- the laminated glass 1 preferably has a radius of curvature in the X direction (horizontal direction) of 10000 mm or less, and preferably has a radius of curvature in the X direction of 1000 mm or more. More preferably, the laminated glass 1 has a radius of curvature in the X direction of 1500 mm or more and 6000 mm or less.
- the Y-direction curvature radius refers to the curvature radius of a curve extending in the Y-direction along the surface of the laminated glass 1
- the X-direction curvature radius refers to the X-direction curvature along the surface of the laminated glass 1.
- the radius of curvature of a curve it is preferable that the radius of curvature of the laminated glass 1 is within the range of the radius of curvature over the entire area.
- the radius of curvature is obtained by measuring the shape of the laminated glass 1 at a predetermined pitch, for example, a pitch of 20 mm, and converting it into the radius of curvature in the Y or X direction.
- the length of the laminated glass 1 in the Y direction is preferably 200 mm or more and 2500 mm or less, and more preferably 200 mm or more and 2000 mm or less. It is preferably 200 mm or more and 1500 mm or less, more preferably.
- the length in the Y direction of the laminated glass 1 refers to the length in the Y direction at the longest point.
- the length of the laminated glass 1 in the X direction that is, the length along the X direction from the side edge 1c to the side edge 1d is preferably 200 mm or more and 2500 mm or less, and is 200 mm or more and 2300 mm or less. , and more preferably 200 mm or more and 2000 mm or less.
- the length in the X direction of the laminated glass 1 here refers to the length in the X direction at the longest point.
- FIG. 2 is a schematic cross-sectional view of the laminated glass according to this embodiment.
- FIG. 2 is a cross-sectional view when the laminated glass 1 is viewed from the Y direction.
- the laminated glass 1 has a first glass substrate 12 , a second glass substrate 14 , a reflective layer 16 , an intermediate layer 18 , an adhesive layer 20 and a light shielding layer 22 .
- the laminated glass 1 has a first glass substrate 12, an intermediate layer 18, a reflective layer 16, an adhesive layer 20, a second glass substrate 14, and a light shielding layer 22 laminated in this order in the Z direction.
- the laminated glass 1 displays a HUD image by reflecting the light from the projection device on the reflective layer 16 formed in the HUD area AH.
- the first glass substrate 12 is an exterior glass substrate.
- the first glass substrate 12 for example, soda-lime glass, aluminosilicate, or organic glass can be used, but the material is not limited to these.
- the thickness D1 of the first glass substrate 12 is preferably 1.8 mm or more and 3.0 mm or less, more preferably 1.9 mm or more and 2.3 mm or less. By setting the thickness D1 of the first glass substrate 12 within this range, it is possible to prevent an increase in weight and a decrease in moldability while appropriately maintaining resistance to stepping stones and the like.
- the thickness D1 is the length in the Z direction of the first glass substrate 12, and hereinafter, unless otherwise specified, the thickness indicates the length in the Z direction.
- the second glass substrate 14 is a glass substrate inside the vehicle.
- the second glass substrate 14 for example, soda-lime glass, aluminosilicate, or organic glass can be used like the first glass substrate 12, but the material is not limited to these.
- the thickness D2 of the second glass substrate 14 is preferably 0.3 mm or more and 2.3 mm or less, more preferably 0.4 mm or more and 2.0 mm or less. When the thickness of the second glass substrate 14 is 0.3 mm or more, it is easy to handle during manufacture and assembly. When the thickness D2 of the second glass substrate 14 is within this range, it does not become thicker than the thickness D1 of the first glass substrate 12, and the first glass substrate 12 and the second glass after bending into a curved shape. Mismatches are less likely to occur when the substrate 1 is laminated, and followability to the adhesive layer can be appropriately maintained.
- the reflective layer 16 is provided between the first glass substrate 12 and the second glass substrate 14 in the Z direction.
- the reflective layer 16 is a layer that reflects light emitted from the projection device to the HUD area AH. Reflective layer 16 is transparent to visible light. In this embodiment, since P-polarized light is emitted from the projection device, the reflective layer 16 can be said to be a P-polarized reflective film that reflects P-polarized light.
- the reflective layer 16 is formed, for example, by laminating a plurality of members such as polymers having different refractive indices in the Z direction.
- the reflective layer 16 preferably has a reflectance of 5% or more and 30% or less for P-polarized light at an incident angle of Brewster's angle when the reflective layer 16 is enclosed in the laminated glass 1 . If the reflectance of P-polarized light is 5% or more, the HUD image can be properly viewed.
- the reflective layer 16 is not limited to being a P-polarized reflective film, and may be, for example, a hologram film, a scattering type transparent screen, a high reflection film for a HUD, or the like.
- the reflective layer 16 includes a first layer (e.g., a quarter-wave plate) that converts incident P-polarized light into circularly polarized light, and a second layer (e.g., a cholesteric liquid crystal layer) that selectively reflects the circularly polarized light.
- the first layer may convert the circularly polarized light reflected by the second layer into P-polarized light and emit the P-polarized light.
- the thickness D3 of the reflective layer 16 is preferably 25 ⁇ m or more and 200 ⁇ m or less, more preferably 40 ⁇ m or more and 100 ⁇ m or less. When the thickness D3 is within this range, it is possible to properly reflect the light from the projection device and properly transmit the outside light.
- the reflective layer 16 is provided over the entire area of the laminated glass 1 when viewed from the Z direction, but may be provided only in the HUD area AH, for example. That is, the reflective layer 16 may be formed at least in the HUD area AH in the entire area of the laminated glass 1 .
- the intermediate layer 18 is provided between the first glass substrate 12 and the reflective layer 16 in the Z direction.
- the intermediate layer 18 bonds the first glass substrate 12 and the reflective layer 16 by bonding the first glass substrate 12 on the vehicle exterior surface and the reflective layer 16 on the vehicle interior surface.
- the intermediate layer 18 is made of PVB (Poly Vinyl Butyral), that is, polyvinyl butyral resin.
- Polyvinyl butyral resin is a thermoplastic resin obtained, for example, by reacting polyvinyl alcohol with n-butyraldehyde.
- the thickness D4 of the intermediate layer 18 is thicker than the thickness D5 of the adhesive layer 20, which will be described later.
- the thickness D4 of the intermediate layer 18 is preferably 0.3 mm or more and 15 mm or less, more preferably 0.3 mm or more and 3 mm or less, and even more preferably 0.7 mm or more and 1 mm or less.
- the intermediate layer 18 is not limited to being made of polyvinyl butyral resin, and may be made of any material such as EVA (Ethylene Vinyl Acetate, ethylene-vinyl acetate copolymer), COP (Cyclo Olefin Polymer, cycloolefin polymer). may be configured.
- EVA Ethylene Vinyl Acetate, ethylene-vinyl acetate copolymer
- COP Cyclo Olefin Polymer
- cycloolefin polymer Cyclo Olefin Polymer
- the intermediate layer 18 may have a coating that has a function of absorbing ultraviolet rays or infrared rays.
- a portion of the intermediate layer 18 corresponding to the upper edge portion 1a of the laminated glass 1 may be colored.
- the intermediate layer 18 may have three or more layers, such as sound insulation PVB in which a layer having a sound insulation function is sandwiched between PVB layers.
- the thickness of the core layer located in the center in the thickness direction is preferably 70 ⁇ m or more and 130 ⁇ m or less, more preferably 80 ⁇ m or more and 120 ⁇ m or less, and still more preferably 90 ⁇ m or more and 110 ⁇ m or less. is. By setting the core layer to this thickness, it is possible to prevent the sound insulation function of the intermediate layer 18 from deteriorating.
- the adhesive layer 20 is provided between the second glass substrate 14 and the reflective layer 16 in the Z direction.
- the adhesive layer 20 has a function of adhering the reflective layer 16 and the second glass substrate 14 by adhering to the reflective layer 16 on the vehicle-exterior surface and adhering to the second glass substrate 14 on the vehicle-interior surface.
- the adhesive layer 20 is made of resin.
- the adhesive layer 20 is made of polyvinyl butyral resin.
- the adhesive layer 20 is not limited to being made of polyvinyl butyral resin, and may be made of any resin material such as EVA or COP.
- embossing can be appropriately performed so as to suppress the remaining air bubbles when laminated glass is formed by bonding the glass substrate with the adhesive layer 20.
- penetration resistance and adhesiveness can be ensured.
- the adhesive layer 20 and the intermediate layer 18 are provided across the entire area with the reflective layer 16 therebetween.
- the adhesive layer 20 and the intermediate layer 18 may be bonded together and integrated in the area where the reflective layer 16 is not formed.
- the adhesive layer 20 may exist only in a portion where the reflective layer 16 is present. It may have a configuration in which it is in direct contact with the base 14 .
- the adhesive layer 20 contains a reaction product generated by the reaction of a silane compound (silane coupling agent). That is, the adhesive layer 20 contains a resin (polyvinyl butyral resin in this embodiment) and a reaction product of a silane compound. In this embodiment, the adhesive layer 20 contains a reaction product of a silane compound in a resin layer. However, the adhesive layer 20 is not limited to this, and the resin layer and the reaction product layer of the silane compound may be separately formed. In this case, the adhesive layer 20 has a resin layer positioned on the reflective layer 16 side (vehicle outer side), and a layer of a silane compound reaction product positioned between the resin layer and the second glass substrate 14 .
- the silane compound is hydrolyzed to produce a silanol compound having a silanol group (Si--OH group).
- This silanol compound undergoes a condensation reaction and is bonded to the surface of the second glass substrate 14 with a siloxane bond (Si—O bond).
- the functional groups contained in the silanol compound are bonded to the resin contained in the adhesive layer 20, the reflective layer 16, and the intermediate layer 18.
- the adhesive layer 20 contains siloxane bonds. That is, the adhesive layer 20 is adhered to the surface of the second glass substrate 14 by siloxane bonding. This makes it possible to appropriately improve the adhesiveness with the second glass substrate 14 and reduce the degree of falling off of fragments when receiving an impact.
- the siloxane bond contained in the adhesive layer 20 corresponds to the reaction product produced by the reaction of the silane compound.
- the adhesive layer 20 preferably contains a functional group that bonds with the resin contained in the adhesive layer 20 and organic substances such as the reflective layer 16 and the intermediate layer 18 .
- the adhesive layer 20 preferably contains at least one of an amino group and an epoxy group, and more preferably contains both an amino group and an epoxy group, as functional groups.
- the adhesive layer 20 contains at least one of an amino group and an epoxy group as a functional group, thereby appropriately improving adhesion to the resin contained in the adhesive layer 20, the reflective layer 16, the intermediate layer 18, and the like, thereby reducing impact. It is possible to reduce the degree of falling off of fragments when receiving.
- This functional group also corresponds to a reaction product produced by the reaction of the silane compound.
- the adhesive layer 20 contains a silane compound or a silanol group, since not all react normally, the unreacted silane compound can be captured by using GC-MS and LC-MS. is added.
- the adhesive layer 20 preferably does not have a bond between silicon and a methyl group. Since the adhesive layer 20 does not have a bond between silicon and a methyl group, it is possible to appropriately improve adhesiveness and reduce the degree of falling off of fragments when receiving an impact.
- the adhesive layer 20 preferably contains Si derived from the silane compound, and the amount of Si detected when the adhesive layer 20 is quantitatively measured is, for example, in terms of mass ratio to Si contained in the added silane compound. It is assumed to be about 60% or more and 100% or less.
- the adhesive layer 20 preferably has a Si content of 0.10% by mass or more and 3.2% by mass or less with respect to the content of all the elements contained in the adhesive layer 20, and 0.2% by mass. % or more and 1.0 mass % or less, and more preferably 0.5 mass % or more and 0.6 mass % or less.
- the Si content can be measured by, for example, an XPS (X-ray Photoelectron Spectroscopy) method to calculate the elemental composition ratio, and the content of the silane compound can be estimated from the elemental ratio.
- the adhesive layer 20 preferably has N derived from aminosilane, and the amount of N detected when the adhesive layer 20 is quantitatively measured is, for example, 60% by mass of the N contained in the added aminosilane. It is assumed that it is more than 100% or less.
- the adhesive layer 20 preferably has a N content of 0.05% by mass or more and 1.5% by mass or less with respect to the content of all elements contained in the adhesive layer 20, and 0.10% by mass. % or more and 0.50 mass % or less, more preferably 0.20 mass % or more and 0.40 mass % or less.
- the N content is measured using CHN elemental analysis.
- CHN elemental analysis The principle of CHN elemental analysis is to burn and pyrolyze a weighed organic sample with oxygen, convert carbon, hydrogen, and nitrogen into nitrogen gas, water, and carbon dioxide, and use a TCD (thermal conductivity detector) to detect nitrogen. Detect gas.
- the adhesive layer 20 preferably has epoxy groups derived from epoxysilane, and the amount of epoxy groups detected when the adhesive layer 20 is quantitatively measured is, for example, the mass of the epoxy groups contained in the added aminosilane. It is assumed that the ratio is about 60% or more and 100% or less.
- the adhesive layer 20 preferably has an epoxy group content of 0.05% by mass or more and 1.5% by mass or less with respect to the content of all elements contained in the adhesive layer 20, and preferably 0.10% by mass or more. It is more preferably 0.50% by mass or more, and even more preferably 0.20% by mass or more and 0.40% by mass or less. When the content of the epoxy group is within this range, the epoxy group can be sufficiently contained and the adhesiveness can be appropriately improved.
- the thickness D5 of the adhesive layer 20 is 2 ⁇ m or more and 25 ⁇ m or less, preferably 4 ⁇ m or more and 25 ⁇ m or less, and more preferably 4 ⁇ m or more and 20 ⁇ m or less. By setting the thickness D5 within this range, it is possible to suppress deterioration in the visibility of the HUD image, which is called orange peel, and also to suppress deterioration in adhesion to the second glass substrate 14 and the reflective layer 16 .
- the thickness D5 here refers to the thickness of the adhesive layer 20 when laminated on the laminated glass 1 . As will be described later, the adhesive layer 20 may be laminated with unevenness formed on its surface. The uneven surface is deformed, and the thickness D5 at the time of lamination falls within the above numerical range.
- the light shielding layer 22 is provided on the surface of the second glass substrate 14 on the interior side of the vehicle.
- the light shielding layer 22 is a layer that shields visible light.
- a ceramic light shielding layer or a light shielding film can be used.
- a ceramic light-shielding layer a ceramic layer made of a conventionally known material such as a black ceramic layer can be used.
- the light-shielding film for example, a light-shielding polyethylene terephthalate (PET) film, a light-shielding polyethylene naphthalate (PEN) film, a light-shielding polymethyl methacrylate (PMMA) film, or the like can be used.
- PET light-shielding polyethylene terephthalate
- PEN light-shielding polyethylene naphthalate
- PMMA light-shielding polymethyl methacrylate
- the light shielding layer 22 is not limited to being provided on the vehicle-interior surface of the second glass substrate 14 , and may be provided on the vehicle-exterior surface of the first glass substrate 12 . It may be formed between the second glass substrate 14 and the second glass substrate 14 .
- the light shielding region A2 is formed by providing the light shielding layer 22 on the laminated glass 1. That is, the light shielding region A2 is the region where the light shielding layer 22 is provided.
- the translucent area A1 is an area where the glass substrates 12 and 14 do not have the light shielding layer 22 .
- FIG. 3 is a diagram for explaining the bubble residual rate.
- the laminated glass 1 configured as described above preferably has a residual bubble rate of 2% or less, more preferably 1% or less, and even more preferably 0%. .
- a decrease in visibility can be suppressed when the air bubble residual ratio falls within this numerical range.
- the bubble residual rate of the HUD area AH falls within this numerical range.
- the bubble residual ratio refers to the degree of residual bubbles in the laminated glass 1 .
- Bubbles are bubbles that exist between the first glass substrate 12 and the second glass substrate 14. For example, air bubbles that cannot be degassed and remain between the adhesive layer 20 and the second glass substrate 14 during the manufacturing process. It is air bubbles.
- each air bubble is 2 mm or less in diameter. If the bubble diameter is 2 mm or less, visibility is less likely to be affected. Furthermore, it is preferable that the diameter of the bubbles is 1 mm or less. If the bubble is not circular when viewed from the Z direction, it may be treated as the diameter of the circumscribed circle of the bubble. Further, in this embodiment, a region in which the adhesive layer 20 does not become transparent and appears cloudy due to poor adhesion between the adhesive layer 20 and the second glass substrate 14 is regarded as a collection of small bubbles. In addition, a region where the PVB layer 20 remains uneven and looks like a mela mela is also regarded as a collection of small bubbles.
- the area of such a region is calculated as the area of the air bubble, and the air bubble residual rate is obtained.
- the bubble residual ratio will be explained more specifically.
- a 100 mm square area at an arbitrary position when the surface of the laminated glass 1 is viewed from the Z direction (in a plan view) is defined as an area 1H.
- Light is applied to the laminated glass 1 to confirm the presence of air bubbles in the region 1H when viewed from the Z direction. For example, it may be confirmed by illuminating the laminated glass 1 with a high-intensity lamp and reflecting it with air bubbles, or by shining light from the end surface of the laminated glass 1 and scattering the light by air bubbles.
- the bubble image may be confirmed by irradiating light from the opposite side of the laminated glass 1, or the bubble may be confirmed with a laser microscope.
- a bubble c exists in the first region 1Ha, and no bubble exists in the second region 1Hb that does not overlap with the first region 1Ha.
- the bubble survival rate of the first region 1Ha is obtained by the ratio of the area of all the bubbles c existing in the region 1Ha to the area of the region 1Ha as viewed from the Z direction, and there is no bubble c in the region 1Hb. Therefore, the bubble residual rate becomes zero.
- the laminated glass 1 as a whole has a bubble residual rate within the above range.
- the determination may be made in the HUD area AH.
- the area 1Ha shown in the example of FIG. 3 may overlap the HUD area AH.
- the laminated glass 1 according to this embodiment reflects the light from the projection device with the reflective layer 16 to display the HUD image.
- the inventors have found that when the adhesive layer 20 between the reflective layer 16 and the second glass substrate 14 is thick, a phenomenon called orange peel occurs, in which the visibility of the HUD image is lowered.
- the thickness D5 of the adhesive layer 20 is reduced to 25 ⁇ m or less, thereby suppressing the orange peel and suppressing the deterioration of the visibility of the HUD image. By doing so, it is possible to ensure the adhesiveness of the adhesive layer 20 .
- the adhesive layer 20 according to the present embodiment contains siloxane bonds, the adhesiveness to the second glass substrate 14 can be appropriately improved, and when receiving an impact, the degree of falling off of fragments can be reduced. It becomes possible to
- the adhesive layer 20 is formed using a resin material that is the resin component of the adhesive layer 20 and a silane compound (silane coupling agent). More specifically, in this embodiment, the adhesive layer 20 is formed by adding a resin material and a silane compound to a solvent and reacting the silane compound.
- the solvent is, for example, ethanol, but is not limited to ethanol and may be a liquid of any component.
- the resin material is PVB resin before curing.
- the amount of the resin material to be added is preferably 6% or more and 15% or less by mass relative to the total amount of the solvent, the resin material, and the silane compound.
- the silane compound forms siloxane bonds contained in the adhesive layer 20 by reacting.
- at least one of aminosilane and epoxysilane is preferably used as the silane compound, and both aminosilane and epoxysilane are more preferably used.
- aminosilanes include 3-aminopropyltrimethoxysilane, N-2-(aminoethyl)-3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, and N-phenyl-3-aminopropyltrimethoxysilane.
- epoxysilanes include 3-glycidoxypropyltrimethoxysilane, 8-glycidoxyoctyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, and 3-glycidoxypropyltrimethoxysilane. at least one of ethoxysilanes;
- the amount of the silane compound added is preferably 1% or more and 20% or less, more preferably 2.5% or more and 10% or less, by mass relative to the amount of the resin material added. It is preferably 4% or more and 6% or less.
- the amount of silane compound added here refers to the amount of one type of silane compound added when one type of silane compound is added, and when multiple types of silane compounds are added, , indicates the total addition amount of these plural kinds of silane compounds.
- the amount of aminosilane added is 1% or more and 10% or less, and the amount of epoxysilane added is 1% by mass relative to the amount of resin material added. % or more and 10% or less, more preferably the addition amount of aminosilane is 1% or more and 5% or less, and the addition amount of epoxysilane is 1% or more and 5% or less, and the addition amount of aminosilane is 2%. % or more and 3% or less, and the addition amount of the epoxysilane is more preferably 2% or more and 3% or less. Adhesion can be improved by setting the amounts of aminosilane and epoxysilane added within this range.
- FIG. 4 is a diagram for explaining a method for manufacturing an adhesive layer.
- a coating liquid 20A is prepared.
- the coating liquid 20A contains a resin material, a silane compound, and a solvent. That is, in this manufacturing method, the coating liquid 20A is prepared by adding a resin material and a silane compound to a solvent. The compounding ratio of each component in the coating liquid 20A may be as described above.
- a forming substrate B2 provided on the substrate B1 is prepared. Concavities and convexities (embossing) are formed on the surface B2a of the formation substrate B2 opposite to the substrate B1.
- a coating liquid 20A is applied onto the surface B2a of the formation substrate B2.
- the amount of the coating liquid 20A applied onto the forming substrate B2 is set so that the thickness D5 of the adhesive layer 20 when laminated on the laminated glass 1 falls within the above numerical range.
- the liquid component of the coating liquid 20A is removed by drying as shown in step S12 of FIG. is formed.
- unevenness is formed on the surface 20a on the side in contact with the surface B2a of the formation substrate B2.
- the surface 20b opposite to the surface 20a of the adhesive layer 20 before lamination may not have unevenness and may have any shape.
- FIG. 5 is a schematic diagram showing an adhesive layer before lamination.
- the thickness of the adhesive layer 20 before lamination is defined as a thickness D5a.
- the thickness D5a refers to the thickness of the thickest part of the adhesive layer 20 before lamination. It refers to the length in the Z direction between the protruding parts.
- the thickness D5a is preferably 30 ⁇ m or less, more preferably 25 ⁇ m or less, and even more preferably 10 ⁇ m or less.
- the thickness D5a is preferably 6.2 ⁇ m or more, more preferably 6.4 ⁇ m or more, and even more preferably 6.6 ⁇ m or more.
- the thickness (height) of the uneven portion of the adhesive layer 20 before lamination is defined as a thickness D6a.
- the thickness D6a is between the portion of the surface 20a of the adhesive layer 20 before lamination that protrudes farthest from the surface 20b and the portion of the surface 20a of the adhesive layer 20 before lamination that is closest to the surface 20b. , in the Z direction. That is, it can be said that the thickness D6a is the maximum height (maximum height roughness) Rz of the surface 20a defined in JIS B 0601. In this case, the thickness D6a is preferably 5 ⁇ m or more, more preferably 5.4 ⁇ m or more.
- the thickness D6a is preferably thinner than the thickness D5a of the adhesive layer 20 before lamination.
- the thickness D6a is preferably thinner than the thickness D5a of the adhesive layer 20 before lamination.
- the ratio of the thickness D6a to the thickness D5a is defined as the thickness ratio.
- the thickness ratio is preferably less than 0.95, more preferably 0.82 or less, even more preferably 0.63 or less.
- the thickness ratio is preferably 0.18 or more, more preferably 0.22 or more, and even more preferably 0.27 or more.
- the arithmetic mean roughness Ra defined by JIS B 0601 of the surface 20a of the adhesive layer 20 before lamination is preferably 0.1 ⁇ m or more and 10 ⁇ m or less, more preferably 0.5 ⁇ m or more and 10 ⁇ m or less. , 0.5 ⁇ m or more and 5 ⁇ m or less.
- Ra By setting Ra within this range, unevenness can be appropriately formed over the entire surface 20a, and the bubble residual rate of the laminated glass 1 can be reduced. That is, when the arithmetic mean roughness Ra of the surface 20a of the adhesive layer 20 is 0.1 ⁇ m or more and 10 ⁇ m or less, it is possible to maintain the air release property and suppress the uneven shape from remaining after pressure bonding to the glass substrate.
- the shape and dimensions of the unevenness on the surface 20a of the adhesive layer 20 before lamination follow the shape and dimensions of the unevenness on the surface B2a of the formation substrate B2. Therefore, the thicknesses D5a and D6a of the adhesive layers 20 before lamination and the surface roughness of the surface 20a described above are determined depending on the shape and dimensions of the surface B2a of the formation substrate B2.
- the adhesive layer 20 before lamination is formed by the method described above.
- the method of forming the adhesive layer 20 is not limited to the above.
- the application liquid 20A is not limited to being applied onto the formation substrate B2 as described above, and the adhesive layer 20 before lamination may not be uneven.
- the adhesive layer 20 is formed by mixing the resin material and the silane compound, but the present invention is not limited to this.
- a layer formed from a silane compound and a layer formed from a resin material may be separately formed to form an adhesive layer.
- FIG. 6 is a diagram illustrating a method for manufacturing laminated glass.
- the first glass substrate 12, the intermediate layer 18, the reflective layer 16, the adhesive layer 20 produced as described above, and the second glass substrate 14 are laminated to form the laminated glass 1.
- manufacture Specifically, as shown in step S20 of FIG. 6, the surface 16a of the reflective layer 16 is brought into contact with the surface 20b of the adhesive layer 20 before lamination formed on the surface B2a of the forming substrate B2, Surface 20b and surface 16a are adhered. Thereby, the reflective layer 16 and the adhesive layer 20 are adhered and laminated.
- the temperature is 80° C. or higher, preferably 100° C. or higher, the temperature is 150° C. or lower, preferably 130° C. or lower, the pressure is 0.6 MPa or higher, preferably 1.
- a pressure bonding process is used in which the reflective layer 16 and the adhesive layer 20 are heated and pressurized under conditions of 0 MPa or more and a pressure of 3.0 MPa or less, preferably 1.5 MPa or less.
- step S22 in FIG. 6 the forming substrate B2 is removed from the adhesive layer 20 laminated on the reflective layer 16. As a result, the uneven surface 20a of the adhesive layer 20 is exposed. Any method may be used to remove the formation substrate B2 from the adhesive layer 20 .
- the laminate of the reflective layer 16 and the adhesive layer 20, the first glass substrate 12, the second glass substrate 14, and the intermediate layer 18 are laminated.
- Surfaces 18a and 18b of intermediate layer 18 are uneven.
- the shape and size of the unevenness on the surface 18a and the surface 18b may be arbitrary, but may be the same shape and size as the surface 20a of the adhesive layer 20, for example.
- surface 18a of intermediate layer 18 and surface 16b of reflective layer 16 opposite surface 16a are brought into contact to bond surfaces 18a and 16b together.
- the pressure and temperature conditions for bonding the surfaces 18 a and 16 b may be the same as the conditions for bonding the reflective layer 16 and the adhesive layer 20 .
- the surface 18b of the intermediate layer 18 opposite to the surface 18a is brought into contact with the vehicle-interior surface 12a of the first glass substrate 12 to bond the surfaces 18b and 12a.
- the surface 14b of the second glass substrate 14 on the side opposite to the surface 14a on the vehicle interior side is brought into contact with the surface 20a of the adhesive layer 20 to bond the surfaces 14b and 20a.
- the laminate of the reflective layer 16 and the adhesive layer 20, the first glass substrate 12, the second glass substrate 14, and the intermediate layer 18 are laminated.
- a laminate of an intermediate layer 18, a reflective layer 16 and an adhesive layer 20 is interposed between the first glass substrate 12 and the second glass substrate 14 to form a glass laminate.
- this glass laminate is placed in a rubber bag and bonded at a temperature of about 70° C. to 130° C. in a vacuum of -65 kPa to -100 kPa.
- a pressure bonding process may be performed in which the pressure is 0.6 MPa or more and 1.5 MPa or less and the temperature is 100° C. or more and 150° C. or less.
- the flat plate-shaped first glass substrate 12 and the second glass substrate 14 are respectively bent, and the intermediate layer 18 is formed between the bent first glass substrate 12 and the second glass substrate 14.
- the laminate of the reflective layer 16 and the adhesive layer 20 may be sandwiched between them.
- an adhesive layer 20 may be additionally laminated between the laminate of the reflective layer 16 and the adhesive layer 20 and the second glass substrate 14 .
- step S24 after forming the laminate of the intermediate layer 18, the reflective layer 16, and the adhesive layer 20, the laminate is sandwiched between the first glass substrate 12 and the second glass substrate 14, and laminated. to run.
- the order of stacking each member and the stacking conditions in step S24 are not limited to those described above and may be arbitrary.
- the laminated glass 1 is manufactured as shown in step S26.
- the light shielding layer 22 may be formed, and another layer may be laminated
- the adhesion layer 20 is formed by adding a silane compound while thinning the adhesion layer 20 before lamination. Adhesion can be guaranteed. Moreover, since the unevenness is formed in the adhesive layer 20 before lamination, the air bubble residual rate of the laminated glass 1 can be reduced. It should be noted that, as described above, the process of forming unevenness on the adhesive layer 20 is not essential.
- the laminated glass 1 according to the present embodiment includes the first glass substrate 12, the second glass substrate 14, and the reflective layer 16 provided between the first glass substrate 12 and the second glass substrate 14. and an adhesive layer 20 provided between the second glass substrate 14 and the reflective layer 16 to bond the second glass substrate 14 and the reflective layer 16 together.
- the adhesive layer 20 has a thickness D5 of 2 ⁇ m or more and 25 ⁇ m or less, and includes siloxane bonds.
- the thickness D5 of the adhesive layer 20 is reduced to 25 ⁇ m or less, thereby suppressing orange peel and reducing the visibility of the HUD image. , the adhesiveness of the adhesive layer 20 can be ensured.
- the laminated glass 1 according to the present embodiment includes a siloxane bond in the adhesive layer 20 to improve the adhesiveness between the adhesive layer 20 and the second glass substrate 14, so that when receiving an impact, the glass substrate 1 is broken into pieces. It is possible to reduce the degree of dropout of the
- the adhesive layer 20 preferably contains a polyvinyl butyral resin. That is, the adhesive layer 20 preferably contains a polyvinyl butyral resin and a siloxane bond. By forming the adhesive layer 20 with polyvinyl butyral resin, it is possible to more appropriately reduce the degree of falling off of fragments when receiving an impact.
- the adhesive layer 20 preferably has a Si content of 0.10% by mass or more and 3.2% by mass or less with respect to the content of all the elements contained in the adhesive layer 20 .
- the adhesive layer 20 contains a sufficient amount of siloxane bonds, and can more appropriately reduce the degree of falling off of fragments when receiving an impact.
- the adhesive layer 20 preferably has a N content of 0.05% by mass or more and 1.5% by mass or less with respect to the content of all the elements contained in the adhesive layer 20 .
- N 0.05% by mass or more and 1.5% by mass or less with respect to the content of all the elements contained in the adhesive layer 20 .
- the adhesive layer 20 preferably has an epoxy group content of 0.05% by mass or more and 1.5% by mass or less with respect to the content of all the elements contained in the adhesive layer 20 .
- the content of the epoxy group is within this range, the epoxy group can be sufficiently contained and the adhesiveness can be appropriately improved.
- the laminated glass 1 preferably further includes an intermediate layer 18 provided between the first glass substrate 12 and the reflective layer 16 and made of polyvinyl butyral resin.
- the intermediate layer 18 is thicker than the adhesive layer 20 .
- the thickness D5 of the adhesive layer 20 is preferably 4 ⁇ m or more and 25 ⁇ m or less, and more preferably 4 ⁇ m or more and 20 ⁇ m or less. As a result, deterioration in the visibility of the HUD image can be more suitably suppressed.
- the method for manufacturing laminated glass according to the present embodiment includes the steps of forming an adhesive layer 20 having a thickness D5a of 30 ⁇ m or less and containing a siloxane bond using a resin material and a silane compound; forming the laminated glass 1 by laminating the reflective layer 16, the adhesive layer 20 and the second glass substrate 14 in this order.
- this manufacturing method by setting the thickness D5a to 30 ⁇ m or less, it is possible to reduce the thickness of the adhesive layer 20 after lamination, thereby suppressing deterioration in the visibility of the HUD image.
- the adhesive layer 20 is formed using a silane compound, the adhesiveness between the adhesive layer 20 and the second glass substrate 14 is improved, and when receiving an impact, the fragments are prevented from falling off. It is possible to reduce the degree.
- Example 2 Examples are described below.
- laminated glass was produced by varying the thickness of the adhesive layer after lamination, the material of the silane compound used to form the adhesive layer, and the content of the silane compound, and evaluated by image clarity and a falling ball test. gone.
- the laminated glass was laminated in order of a first glass substrate, an intermediate layer, a reflective layer, an adhesive layer, and a second glass substrate.
- the amount of the silane compound used for forming the adhesive layer is disclosed. It is assumed that the silanol compound is contained in a proportion of less than 10%.
- Example 1 In Example 1, PVB was used as the resin material, and the added amount of epoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd.: KBM403) was 2.5% by mass, and aminosilane (manufactured by Shin-Etsu Silicone Co., Ltd.) was added to the amount of PVB added as the resin material. : KBM903) was added in an amount of 2.5% by mass to form an adhesive layer. Then, a laminated glass was produced so that the thickness of the adhesive layer after lamination was 2 ⁇ m. In Example 1, the thickness of the first glass substrate and the thickness of the second glass substrate were both 2.0 mm, the intermediate layer was PVB and had a thickness of 0.76 mm, and the reflective layer had a thickness of 75 ⁇ m to 100 ⁇ m. rice field.
- epoxysilane manufactured by Shin-Etsu Silicone Co., Ltd.: KBM403
- aminosilane manufactured by Shin-Etsu Silicone Co., Ltd.
- Example 2 In Example 2, a laminated glass was manufactured in the same manner as in Example 1, except that the thickness of the adhesive layer after lamination was 4 ⁇ m.
- Example 3 a laminated glass was produced in the same manner as in Example 1, except that the thickness of the adhesive layer after lamination was 8 ⁇ m.
- Example 4 a laminated glass was manufactured in the same manner as in Example 1, except that the thickness of the adhesive layer after lamination was 25 ⁇ m.
- Example 5 a laminated glass was produced in the same manner as in Example 1, except that the thickness of the adhesive layer after lamination was 30 ⁇ m.
- Example 6 the adhesive layer was formed so that the added amount of epoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd.: KBM403) was 5% by mass with respect to the added amount of PVB as the resin material. Then, a laminated glass was produced so that the thickness of the adhesive layer after lamination was 4 ⁇ m.
- epoxysilane manufactured by Shin-Etsu Silicone Co., Ltd.: KBM403
- Example 7 the adhesive layer was formed so that the added amount of epoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd.: KBM403) was 10% by mass with respect to the added amount of PVB as the resin material. Then, a laminated glass was produced so that the thickness of the adhesive layer after lamination was 4 ⁇ m.
- epoxysilane manufactured by Shin-Etsu Silicone Co., Ltd.: KBM403
- Example 8 the adhesive layer was formed so that the amount of aminosilane (manufactured by Shin-Etsu Silicone Co., Ltd.: KBM903) added was 5% by mass with respect to the amount of PVB added as the resin material. Then, a laminated glass was produced so that the thickness of the adhesive layer after lamination was 4 ⁇ m.
- KBM903 aminosilane
- Example 9 a laminated glass was manufactured by forming an adhesive layer using PVB as a resin material so that the thickness of the adhesive layer after lamination was 4 ⁇ m. No silane compound was added to the adhesive layer.
- Example 10 a laminated glass was manufactured by forming an adhesive layer using PVB as a resin material so that the thickness of the adhesive layer after lamination was 30 ⁇ m. No silane compound was added to the adhesive layer.
- Table 1 shows the conditions and evaluation results of Examples 1 to 10.
- samples with double circles or circles in the falling ball test and circles in the image definition were regarded as acceptable.
- those that satisfied at least one of the falling ball test and the image sharpness were rejected.
- Examples 1 to 4 and 6 to 8 correspond to Examples, and Examples 5, 9 and 10 correspond to Comparative Examples.
- Examples 1 to 10 it can be seen that a decrease in image definition can be suppressed by setting the thickness of the adhesive layer to 2 ⁇ m or more and 25 ⁇ m or less.
- the addition of a silane compound forms a siloxane bond to improve adhesion, and can reduce the degree of falling off of fragments when receiving an impact.
- the use of epoxysilane and aminosilane as silane compounds can further reduce the degree of falling off of fragments.
- the embodiment of the present invention has been described above, the embodiment is not limited by the content of this embodiment.
- the components described above include those that can be easily assumed by those skilled in the art, those that are substantially the same, and those within the so-called equivalent range.
- the components described above can be combined as appropriate.
- various omissions, replacements, or modifications of components can be made without departing from the gist of the above-described embodiments.
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Abstract
Description
図1は、本実施形態に係る合わせガラスの模式図である。図1に示す本実施形態に係る合わせガラス1は、車両に搭載される。合わせガラス1は、車両のフロントガラスに適用される窓部材であり、言い換えると、車両のフロントウィンドウ、言い換えれば風防ガラスとして用いられている。車両の内部(車内)とは、例えばドライバーの運転席が設けられる車室内を指す。ただし、合わせガラス1の用途は車両のフロントガラスに限られず任意であり、車両の他の箇所などにも適用可能である。以下、合わせガラス1の上縁を、上縁部1aとし、下縁を、下縁部1bとし、一方の側縁を、側縁部1cとし、他方の側縁を、側縁部1dとする。上縁部1aは、合わせガラス1を車両に搭載した際に、鉛直方向上側に位置する縁部分である。下縁部1bは、合わせガラス1を車両に搭載した際に、鉛直方向下側に位置する縁部分である。側縁部1cは、合わせガラス1を車両に搭載した際に、一方の側方側に位置する縁部分である。側縁部1dは、合わせガラス1を車両に搭載した際に、他方の側方側に位置する縁部分である。
第1ガラス基体12は、車外側のガラス基体である。第1ガラス基体12としては、例えばソーダライムガラス、アルミノシリケート、有機ガラスを用いることができるが、これに限定されない。第1ガラス基体12の厚さD1は、1.8mm以上3.0mm以下であることが好ましく、1.9mm以上2.3mm以下であることがより好ましい。第1ガラス基体12の厚さD1がこの範囲になることで、飛び石等に対する耐性能を適切に保ちつつ、重量が増加して、成形性が低下することを抑制できる。厚さD1は、第1ガラス基体12のZ方向における長さであり、以降においても、特に断りがない限り、厚さとはZ方向における長さを指す。
反射層16は、Z方向において第1ガラス基体12と第2ガラス基体14との間に設けられている。反射層16は、投影装置からHUD領域AHに照射される光を反射する層である。反射層16は、可視光に対しては透明である。本実施形態においては、投影装置からP偏光の光が照射されるため、反射層16は、P偏光の光を反射するP偏光反射フィルムであるといえる。反射層16は、例えば、屈折率が異なるポリマーなどの部材をZ方向に複数積層して形成される。反射層16は、反射層16が合わせガラス1内に封入された状態において、入射角がブリュースター角でのP偏光の反射率が5%以上30%以下であることが好ましい。P偏光の反射率が5%以上であれば、HUD像を適切に視認することができる。なお、反射層16は、P偏光反射フィルムであることに限られず、例えば、ホログラムフィルム、散乱型透明スクリーン、HUD向け増反射フィルムなどであってもよい。また例えば、反射層16は、入射したP偏光を円偏光に変換する第1層(例えば1/4波長板)と、円偏光を選択的に反射する第2層(例えばコレステリック液晶層)とを備えて、第1層が、第2層で反射された円偏光をP偏光に変換して出射する構成であってもよい。
中間層18は、Z方向において第1ガラス基体12と反射層16との間に設けられる。中間層18は、車外側の表面で第1ガラス基体12と接着し、車内側の表面で反射層16と接着することで、第1ガラス基体12と反射層16とを接着する。中間層18は、PVB(Poly Vinyl Butyral)、すなわちポリビニルブチラール樹脂で形成される。ポリビニルブチラール樹脂は、例えばポリビニルアルコールとn-ブチルアルデヒドとを反応させて得られる、熱可塑性樹脂である。
接着層20は、Z方向において第2ガラス基体14と反射層16との間に設けられる。接着層20は、車外側の表面で反射層16と接着し、車内側の表面で第2ガラス基体14と接着することで、反射層16と第2ガラス基体14とを接着する機能を有する。
遮光層22は、第2ガラス基体14の車内側の表面に設けられている。遮光層22は、可視光を遮蔽する層である。遮光層22としては、例えばセラミックス遮光層や遮光フィルムを用いることができる。セラミックス遮光層としては、例えば黒色セラミックス層等の従来公知の材料からなるセラミックス層を用いることができる。遮光フィルムとしては、例えば遮光ポリエチレンテレフタレート(PET)フィルム、遮光ポリエチレンナフタレート(PEN)フィルム、遮光ポリメチルメタクリレート(PMMA)フィルム等を用いることができる。なお、遮光層22は、第2ガラス基体14の車内側の表面に設けられることに限られず、第1ガラス基体12の車外側の表面に設けられていてもよいし、第1ガラス基体12と第2ガラス基体14との間に形成されてもよい。
図3は、気泡残存率について説明する図である。以上のような構成の合わせガラス1は、気泡残存率が2%以下であることが好ましく、気泡残存率が1%以下であることがより好ましく、気泡残存率が0%であることが更に好ましい。気泡残存率がこの数値範囲となることで、視認性の低下を抑制できる。特にHUD領域AHの気泡残存率がこの数値範囲になることが好ましい。気泡残存率とは、合わせガラス1の気泡の残存度合いを指す。気泡とは、第1ガラス基体12と第2ガラス基体14との間に存在する気泡であり、例えば、接着層20と第2ガラス基体14との間に製造工程中に脱気できずに残った気泡である。さらに気泡単体の大きさは直径2mm以下であることが好ましい。気泡の直径が2mm以下であれば、視認性に影響を与えにくい。さらに気泡の直径が1mm以下であることが好ましい。なお、Z方向から見て気泡が円形でない場合には気泡の外接円の直径として扱ってよい。
また本実施形態では、接着層20と第2のガラス基体14との接着不良により接着層20が透明化せずに白濁して見える領域を小さな気泡の集合とみなす。また、PVB層20の凹凸が残ってメラメラに見える領域も小さな気泡の集合とみなす。このような領域の面積を算出して気泡の面積とし、気泡残存率を求める。
気泡残存率についてより具体的に説明する。図3に示すように、合わせガラス1の表面をZ方向から見た(平面視で)任意の位置の100mm角の領域を、領域1Hとする。合わせガラス1に光を当てて、Z方向から見て領域1H内の気泡の存在を確認する。例えば、高輝度ランプで合わせガラス1を照らして気泡で反射させて確認してもよく、また合わせガラス1の端面から光を入れ、気泡で光を散乱させて確認することでもよい。また、光を合わせガラス1の反対側から照射させて気泡の像を確認してもよく、レーザー顕微鏡で気泡を確認してもよい。例えば、図3において、第1領域1Haに気泡cが存在し、第1領域1Haとは重複しない第2領域1Hbには気泡は存在していない。この場合において、第1領域1Haの気泡残存率は、Z方向から見た、領域1Haの面積に対する領域1Haに存在する全ての気泡cの面積の比率で求められ、領域1Hbについては気泡cがないため、気泡残存率はゼロとなる。なお、領域1Hは、任意の領域であるので、合わせガラス1は、全体において、気泡残存率が上記の範囲となる。ただし、表面1Hは、必ず合わせガラス1の全体を測定する必要はなく、合わせガラス1全体で気泡が最も多く残存している100mm角の領域のみを、表面1Hとしても測定してもよい。また、HUD領域AHで判断してもよい。例えば 、図3の例に示す領域1HaがHUD領域AHに重なっていてもよい。
次に、以上説明した合わせガラス1の製造方法について説明する。本製造方法においては、接着層20の樹脂成分の材料となる樹脂材料と、シラン化合物(シランカップリング剤)とを用いて、接着層20を形成する。より詳しくは、本実施形態では、溶媒に、樹脂材料とシラン化合物を添加し、シラン化合物を反応させて、接着層20を形成する。溶媒は、例えばエタノールであるが、エタノールに限られず、任意の成分の液体であってよい。接着層20がPVBである場合には、樹脂材料は、硬化前のPVB樹脂である。樹脂材料の添加量は、溶媒と樹脂材料とシラン化合物との合計量に対して、質量比で6%以上15%以下添加されることが好ましい。
次に、上述の方法で製造した接着層20を用いて合わせガラス1を製造する方法を説明する。図6は、合わせガラスの製造方法を説明する図である。本製造方法においては、第1ガラス基体12と、中間層18と、反射層16と、上記のようにして製造した接着層20と、第2ガラス基体14とを積層して、合わせガラス1を製造する。具体的には、図6のステップS20に示すように、形成用基板B2の表面B2a上に形成された積層前の接着層20の表面20b上に、反射層16の表面16aを接触させて、表面20bと表面16aとを接着させる。これにより、反射層16と接着層20とが接着して、積層される。反射層16と接着層20とを接着する際には、例えば、温度80℃以上、好ましくは100℃以上、かつ温度150℃以下、好ましくは130℃以下、圧力0.6MPa以上、好ましくは1.0MPa以上、かつ圧力3.0MPa以下、好ましくは1.5MPa以下の条件で、反射層16と接着層20とを加熱加圧する圧着処理を用いる。
以上説明したように、本実施形態に係る合わせガラス1は、第1ガラス基体12と、第2ガラス基体14と、第1ガラス基体12と第2ガラス基体14との間に設けられる反射層16と、第2ガラス基体14と反射層16との間に設けられて第2ガラス基体14と反射層16とを接着する接着層20とを有する。接着層20は、厚さD5が2μm以上25μm以下であり、シロキサン結合を含む。本実施形態に係る合わせガラス1は、接着層20の厚さD5を25μm以下と薄くすることで、オレンジピールを抑制してHUD像の視認性の低下を抑制しつつ、2μm以上とすることで、接着層20による接着性を担保することを可能としている。また、本実施形態に係る合わせガラス1は、接着層20にシロキサン結合を含ませることで、接着層20と第2ガラス基体14との接着性を向上させて、衝撃を受けた場合に、破片の脱落の度合いを小さくすることが可能となる。
以下に、実施例について説明する。実施例においては、積層後の接着層の厚み、接着層の形成に用いるシラン化合物の材料、及びシラン化合物の含有量を異ならせて、合わせガラスを製造し、像鮮明度と落球試験で評価を行った。合わせガラスは、第1のガラス基板、中間層、反射層、接着層、第2のガラス基板の順に積層させた。なお、以下の各例では、接着層の形成のために用いたシラン化合物の添加量を開示しているが、各例で形成された接着層には、シラン化合物の添加量の6割以上10割以下程度のシラノール化合物が含まれていると想定される。
例1では、樹脂材料としてPVBを用いて、樹脂材料としてのPVBの添加量に対して、エポキシシラン(信越シリコーン社製:KBM403)の添加量が2.5質量%、アミノシラン(信越シリコーン社製:KBM903)の添加量が2.5質量%となるように、接着層を形成した。そして、積層後の接着層の厚さが2μmとなるように、合わせガラスを製造した。なお、例1において、第1ガラス基体、第2ガラス基体の厚みは、ともに2.0mmであり、中間層は、PVBであり、厚みが0.76mmであり、反射層は75μm~100μmであった。
例2では、積層後の接着層の厚さを4μmとした以外は、例1と同じ方法で、合わせガラスを製造した。
例3では、積層後の接着層の厚さを8μmとした以外は、例1と同じ方法で、合わせガラスを製造した。
例4では、積層後の接着層の厚さを25μmとした以外は、例1と同じ方法で、合わせガラスを製造した。
例5では、積層後の接着層の厚さを30μmとした以外は、例1と同じ方法で、合わせガラスを製造した。
例6では、樹脂材料としてのPVBの添加量に対して、エポキシシラン(信越シリコーン社製:KBM403)の添加量が5質量%となるように、接着層を形成した。そして、積層後の接着層の厚さが4μmとなるように、合わせガラスを製造した。
例7では、樹脂材料としてのPVBの添加量に対して、エポキシシラン(信越シリコーン社製:KBM403)の添加量が10質量%となるように、接着層を形成した。そして、積層後の接着層の厚さが4μmとなるように、合わせガラスを製造した。
例8では、樹脂材料としてのPVBの添加量に対して、アミノシラン(信越シリコーン社製:KBM903)の添加量が5質量%となるように、接着層を形成した。そして、積層後の接着層の厚さが4μmとなるように、合わせガラスを製造した。
例9では、樹脂材料をPVBとして接着層を形成して、積層後の接着層の厚さが4μmとなるように、合わせガラスを製造した。接着層にはシラン化合物を添加しなかった。
例10では、樹脂材料をPVBとして接着層を形成して、積層後の接着層の厚さが30μmとなるように、合わせガラスを製造した。接着層にはシラン化合物を添加しなかった。
像鮮明度は、合わせガラスの2m先に0.034deg(=2min)幅の横線を投影した場合の「線の縦方向の歪量」が0.017degを超えるか否かについて評価を行い、「線の縦方向の歪量」が0.017deg(=1min)を超えない場合をマルとし、0.017deg(=1min)を超える場合をバツとした。
落球試験の評価においては、JIS R3211,3212-2015における耐衝撃性試験に準拠して評価を行った。JIS R3211,3212-2015における耐衝撃性試験に従い、40℃及び-20℃の両方で評価を行い、落球試験後に合わせガラスから剥離された破片の重さが、40℃及び-20℃の両方において3g未満の場合を二重丸とし、40℃及び-20℃の両方において15g未満であり、かつ、40℃及び-20℃の少なくとも一方で3g以上15g未満の場合をマルとし、40℃及び-20℃の少なくとも一方で15g以上の場合をバツとした。
表1に、例1から例10の条件と評価結果を示す。評価においては、落球試験が二重丸又はマルであり、かつ、像鮮明度がマルであるものを合格とした。また、落球試験がバツ、像鮮明度がバツの少なくとも一方を満たすものを不合格とした。例1から例4、例6から例8が実施例に該当し、例5、例9、例10が比較例に該当する。例1から例10に示すように、接着層の厚みを2μm以上25μm以下とすることで、像鮮明度の低下を抑制できることが分かる。また、シラン化合物を添加することで、シロキサン結合が形成されて接着性が向上し、衝撃を受けた場合に、破片の脱落の度合いを小さくできることが分かる。また、シラン化合物としてエポキシシランとアミノシランとを用いることで、破片の脱落の度合いをより小さくできることが分かる。
12 第1ガラス基体
14 第2ガラス基体
16 反射層
18 中間層
20 接着層
Claims (9)
- 第1ガラス基体と、
第2ガラス基体と、
前記第1ガラス基体と前記第2ガラス基体との間に設けられる反射層と、
前記第2ガラス基体と前記反射層との間に設けられて、前記第2ガラス基体と前記反射層とを接着する接着層と、
を有する合わせガラスであって、
前記接着層は、厚さが2μm以上25μm以下であり、シロキサン結合を含む、
合わせガラス。 - 前記接着層は、ポリビニルブチラール樹脂を含む、請求項1に記載の合わせガラス。
- 前記接着層は、前記接着層に含まれる全ての元素の含有量に対し、Siの含有量が、0.10質量%以上3.2質量%以下である、請求項1又は請求項2に記載の合わせガラス。
- 前記接着層は、前記接着層に含まれる全ての元素の含有量に対し、Nの含有量が、0.05質量%以上1.5質量%以下である、請求項1から請求項3のいずれか1項に記載の合わせガラス。
- 前記接着層は、前記接着層に含まれる全ての元素の含有量に対し、エポキシ基の含有量が、0.05質量%以上1.5質量%以下である、請求項3又は請求項4に記載の合わせガラス。
- 前記第1ガラス基体と前記反射層との間に設けられてポリビニルブチラール樹脂で形成される中間層をさらに備え、
前記中間層は、前記接着層よりも厚さが大きい、請求項1から請求項5のいずれか1項に記載の合わせガラス。 - 前記接着層の厚さが4μm以上25μm以下である、請求項1から請求項6のいずれか1項に記載の合わせガラス。
- 前記接着層の厚さが4μm以上20μm以下である、請求項7に記載の合わせガラス。
- 樹脂材料とシラン化合物とを用いて、厚さが30μm以下であり、シロキサン結合を含む接着層を形成するステップと、
第1ガラス基体と、反射層と、前記接着層と、第2ガラス基体とを積層して合わせガラスを形成するステップと、
を含む、合わせガラスの製造方法。
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WO2023155431A1 (zh) * | 2022-09-21 | 2023-08-24 | 福耀玻璃工业集团股份有限公司 | 一种夹层玻璃及车辆 |
WO2024071341A1 (ja) * | 2022-09-30 | 2024-04-04 | 積水化学工業株式会社 | 合わせガラス用中間膜及び合わせガラス |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH04275956A (ja) * | 1991-03-01 | 1992-10-01 | Asahi Glass Co Ltd | ホログラム封入合せガラス |
JPH07281029A (ja) * | 1994-02-18 | 1995-10-27 | Nippondenso Co Ltd | 光学部材及びその製造方法 |
WO2017223023A1 (en) * | 2016-06-20 | 2017-12-28 | Solutia Inc. | Interlayers comprising optical films having enhanced optical properties |
-
2022
- 2022-03-03 CN CN202280017942.3A patent/CN116940539A/zh active Pending
- 2022-03-03 WO PCT/JP2022/009142 patent/WO2022186338A1/ja active Application Filing
- 2022-03-03 JP JP2023503947A patent/JPWO2022186338A1/ja active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH04275956A (ja) * | 1991-03-01 | 1992-10-01 | Asahi Glass Co Ltd | ホログラム封入合せガラス |
JPH07281029A (ja) * | 1994-02-18 | 1995-10-27 | Nippondenso Co Ltd | 光学部材及びその製造方法 |
WO2017223023A1 (en) * | 2016-06-20 | 2017-12-28 | Solutia Inc. | Interlayers comprising optical films having enhanced optical properties |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2023155431A1 (zh) * | 2022-09-21 | 2023-08-24 | 福耀玻璃工业集团股份有限公司 | 一种夹层玻璃及车辆 |
WO2024071341A1 (ja) * | 2022-09-30 | 2024-04-04 | 積水化学工業株式会社 | 合わせガラス用中間膜及び合わせガラス |
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CN116940539A (zh) | 2023-10-24 |
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