JP2000203894A - Production of light-controlling glass and light- controlling glass produced thereby - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a process for producing a light-controlling glass leaving bubbles having small size immediately after the lamination of a light-controlling glass and quickly eliminating the bubbles and provide a light-controlling glass produced by the process. SOLUTION: A thermotropic material 4' is applied to the surface of a substrate 3 surrounded by a sealing material 5a' in divided form comprising dotted form, broken line form or their combination. Each allocation volume of the thermotropic material 4' allocated in divided state adjacent to the sealing material 5a' is 80-105% based on 100% of the product of the total allocation volume of the thermotropic material 4' and the ratio of the area surrounded by the attached sealing material 5a' and the intermediate line 10 of the divided allocation position of the adjacent thermotropic material 4' to the area of the substrate surrounded with the attached sealing material 5a'.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a light control glass comprising a liquid or wet gel-like thermotropic material laminated between two transparent plates, and to a light control glass.

[0002]

2. Description of the Related Art A dimming glass (hereinafter, simply referred to as a laminate) formed by laminating a liquid or wet gel-like thermotropic material between two transparent plates and sealing a peripheral portion thereof with a sealing material. For example, see JP-A-6-25501.
As described in JP-A No. 6 (1994) -6, a thermotropic polymer aqueous solution that changes from a transparent state to a cloudy state due to a temperature rise as a thermotropic material is laminated between two glass plates arranged in parallel. Tropic dimming glass has been proposed. Further, this thermotropic light control glass has been spotlighted because it is more durable, light-shielding, and inexpensive than light control glass using liquid crystal or the like.

[0003]

However, since such a thermotropic material is a liquid or gel-like substance having a higher viscosity than liquid crystals, it is filled between transparent substrates by a vacuum injection method like liquid crystals. Can not do it. Therefore, a sealing material is arranged around one of the substrates, a thermotropic material is divided and arranged inside the sealing material, and then the other substrate is overlaid on the upper surface and held under a reduced pressure condition. Is applied to remove the air while spreading the thermotropic material between the substrates to make them adhere to each other. However, immediately after the close contact, air bubbles remain in the portion along the sealing material, and it takes a leaving time of about one month, for example, for the air bubbles to dissolve in the thermotropic material and completely disappear.

An object of the present invention is to dispose a thermoplastic thermotropic material such as a highly viscous liquid or a gel inside a sealing material, and then place another substrate on the upper surface of the sealing material and hold it under reduced pressure. Further, the size of the bubbles remaining immediately after the light control glass is adhered to the substrate by pressing the substrate on the upper surface to remove the air while spreading the thermotropic material between the substrates and adhere to the substrate is small, and the method for manufacturing the light control glass and the light control time are short. Is to provide glass.

[0005]

According to a first aspect of the present invention, there is provided a method for manufacturing a light control glass, wherein at least a part or all of at least one of the substrates is reversibly switched between a transparent state and a cloudy state by a temperature change. In a method for manufacturing a light control glass in which a thermotropic material that changes state is encapsulated via a sealing material, an arrangement step of a sealing material that attaches the sealing material to a peripheral portion on at least one substrate constituting the light control glass, When the thermotropic material is divided inside the sealing material by coating and divided and arranged in a dot-like or broken-line shape or a combination thereof, the adjacent thermotropic material with respect to the area of the substrate surrounded by the attached sealing material. The ratio of the area surrounded by the middle line at the divided arrangement position and the attached sealing material, and the total arrangement of the thermotropic material Division of the thermotropic material in which the thermotropic material is divided and arranged on the substrate under the condition that the arrangement volume of the thermotropic material to be divided and arranged adjacent to the sealing material is 80 to 105% with respect to the product of 100%. An arranging step, a tentative laminating step of stacking the opposing substrates, interposing a thermotropic material and a sealing material between the substrates, and forming a closed space surrounded by the sealing material between the substrates, and depressurizing the tentatively laminated substrates. A decompression step of maintaining the enclosed space in a substantially vacuum state while maintaining the atmosphere in an atmosphere, and sealing the sealing material while deforming the sealing material in a decompressed atmosphere so that the enclosed space remains in a substantially vacuum state. And a contact step of filling the airtight closed space.

As described above, since the volume of each of the thermotropic materials to be divided and arranged adjacent to the sealing material is set to an appropriate range, the size of bubbles remaining in the portion of the thermotropic material along the sealing material is small. Become. If the filling amount per area of the thermotropic material divided and arranged adjacent to the sealing material is smaller than the central portion, the thermotropic material in the vicinity of the sealing material is difficult to spread to every corner, and bubbles are likely to remain. Also, if the filling amount per area of the thermotropic material divided and arranged adjacent to the sealing material is larger than the central portion, bubbles are less likely to remain, but the thermotropic material tends to protrude from the sealing material.

Here, in the step of dividing and arranging the thermotropic material, it is preferable that the distance between the arranging position of the thermotropic material adjacent to the sealing material and the sealing material is 5 to 30 mm. Here, the larger the distance, the larger the amount of the thermotropic material divided and arranged. Bubbles tend to increase in size as the spacing increases, especially at the four corners. On the other hand, if the width is too narrow, the thermotropic material tends to protrude above the sealing material, which is not preferable.

According to a third aspect of the present invention, in the step of dividing and arranging the thermotropic material, the portion is divided adjacent to the sealing material with respect to the distance between the sealing material and the arrangement position of the thermotropic material divided and arranged adjacent to the sealing material. It is preferable that an arrangement ratio of the arranged thermotropic material to an adjacent thermotropic material is in a range of 1.5 to 2.5. At this time, it is simple and preferable that the thermotropic material is applied in a constant amount over the entire surface, but when the ratio of the arrangement intervals is less than 1.5 or more than 2.5, the volume of the thermotropic material per area is reduced. In order to make the coating as uniform as possible, it is necessary to change the amount of application, and the operation becomes complicated, which is not preferable.

According to a fourth aspect of the present invention, in the depressurizing step, an apparatus having two adjacent depressurized tanks, at least a part of which is partitioned by a flexible film, is used to temporarily laminate the substrates in one depressurized tank. , And depressurize both decompression tanks,
It is preferable that the substrate is kept under a reduced pressure atmosphere of 0.1 to 20 Torr for 10 to 100 seconds. Here, even if the ultimate vacuum degree is too low or the holding time is short, the bubble size after the adhesion step increases, which is not preferable. On the other hand, if the holding time is too long, the amount of constituent water that evaporates from the surface of the disposed thermotropic material is undesirably increased.

According to a fifth aspect of the present invention, in the contacting step,
Using a device having two adjacent decompression tanks, at least a part of which is partitioned by a flexible membrane, set the temporarily laminated substrates in one of the decompression tanks, depressurize both decompression tanks, and depressurize for a predetermined time. After maintaining the atmosphere, the other decompression tank is opened to normal pressure so that the closed space is airtight, and the temporarily laminated substrate is compressed for 3 to 300 seconds through the film body, and the thermotropic material is removed. It is preferable to fill the airtight closed space. According to this method, both vacuum chambers are brought into a substantially vacuum state, and then only the other vacuum chamber is released from the substantially vacuum state.
It is preferable that the film body is swelled toward the decompression tank where the laminate is installed by the pressure difference between the two decompression tanks, and the entire surface of the laminate is compressed at atmospheric pressure through the film.

According to a sixth aspect of the present invention, there is provided a light control glass, wherein at least one part or all of the base is made transparent, a thermotropic material which reversibly changes between a transparent state and a cloudy state by a temperature change, A sealing material for sealing the tropic material between the substrates, wherein the sealing material is attached to a peripheral portion on one of the substrates, and the thermotropic materials are spaced from each other on the one substrate surrounded by the sealing material. In the light control glass in which the thermotropic material is sealed between the substrates by overlapping the two substrates in the arranged state, the division of the adjacent thermotropic material into the area of the substrate surrounded by the attached sealing material is performed. The ratio of the area surrounded by the intermediate line of the arrangement position and the attached sealing material, and the total arrangement volume of the thermotropic material and 100% product relative, is obtained by setting each placement volume of thermotropic material 80-105% for dividing disposed adjacent to the sealing material. In this light control glass, as in the first aspect, the arrangement volume of the thermotropic material to be divided and arranged adjacent to the sealing material is set in an appropriate range. The size of bubbles remaining in the portion becomes smaller.

[0012] As described in claim 7, the use of a material comprising a cellulose derivative and water as components in the thermotropic material is not limited to durability including weather resistance, and repetition of transparency and opacity. Excellent in stability and the like. Further, by adding a nonionic surfactant, the stability of the cloudy state can be remarkably improved, and the uniform cloudy state can be maintained for a long period of time. Further, by adding an inorganic electrolyte as required, it is possible to control the temperature at which the state changes between transparent and cloudy, which is preferable. This makes it possible to arbitrarily set the temperature at which the state changes from about 50 to 60 ° C. without addition to the lower temperature side. The light control glass of the present invention, and the light control glass obtained according to the manufacturing method of the present invention are used for a vertical window, a skylight, a louver window, a sliding window, a window, a bay window, and an outside window in a general house or a building. Casement window, side window, casement window, top and bottom sliding window,
Corner windows, terrace doors, waist panel doors, doors inside high places, patio doors, solarium, greenhouse glass, and more
It can be used for arcades, top lights in large facilities, sunroofs for cars, rear windows, side windows, carports, building exterior walls and heat storage walls.

[0013]

Embodiments of the present invention will be described below with reference to the drawings. As shown in FIG. 1, the light control glass 1 is basically opaque and transparent between liquid or wet gel-like temperature changes between substrates 2 and 3 at least partially or entirely of which is transparent. While providing the thermotropic material 4 that changes state to a state in a laminated state,
A sealing material 5 is provided in a laminated state between the peripheral portions of the base so as to surround the thermotropic material 4, and the thermotropic material 4 is sealed between the bases 2 and 3 via the sealing material 5.

In general, the thermotropic material having such properties includes an isotropic aqueous solution of a nonionic surfactant or a nonionic water-soluble polymer exhibiting a cloud point phenomenon.
Specific examples of such thermotropic materials include polyvinyl alcohol partially acetylated product, polyvinyl methyl ether, methyl cellulose, polyethylene oxide, polypropylene oxide, a copolymer of ethylene oxide and propylene oxide, and a polysaccharide derivative having a hydroxypropyl group ( For example, hydroxypropylcellulose, hydroxypropylmethylcellulose, etc.), polyvinylmethyloxazolidinone, poly N-substituted acrylamide derivatives (eg, poly N-isopropylacrylamide, poly N-ethoxyethyl acrylamide, etc.),
An aqueous solution of a water-soluble polymer such as a poly N, N-di-substituted acrylamide derivative (for example, poly N-methyl-N-ethylacrylamide) or a copolymer thereof, or a polymer solution using an alcohol or the like as a solvent is exemplified. Can be Among these exemplified substances, a polysaccharide derivative having a hydroxypropyl group having a good hydrophobic-hydrophilic balance is preferable in terms of sufficiently shielding sunlight, and has a structurally stable cellulose in the main chain. Cellulose derivatives, ie, hydroxypropylcellulose, are preferred, but the invention is not limited thereto. It is also within the scope of the present invention to add additives such as antioxidants, antifreezing agents, and stabilizers to these solutions.

When an aqueous solution of a cellulose derivative such as hydroxypropylcellulose is used alone, if it is left in a cloudy state for a long time, a non-uniform phase separation state may occur with the passage of time. Non-uniform phase separation refers to a state in which aggregates such as hydroxypropylcellulose aggregated to show a cloudy state are further aggregated and settled with the passage of time, so that they are separated into water as a solvent and two phases. However, by adding a surfactant, particularly a nonionic surfactant as described in JP-A-6-255016, a uniform phase separation state can be maintained for a long time.

As the nonionic surfactant used herein, those having a molecular weight of about 3000 or less, more preferably about 1000 or less in the oligomer region are easily used, and the ionic group has a very hydrophilic group. Since it is large, the hydrophobic group is preferably a higher alkyl group for balancing. Specific examples include polyoxypropylene 2-ethyl-2-hydroxymethyl-1,3-propanediol (polyoxypropylene trimethylolpropane ether), polypropylene glycol, diethylene glycol monobutyl ether, polyoxypropylene glycerin, and sodium lauryl sulfate. For example, any substance having the same action can be used. Further, in order to control the temperature at which the state of the thermotropic material changes as described above, the temperature at which the state changes can be arbitrarily shifted to a lower temperature side by adding an inorganic electrolyte such as sodium chloride as needed. Such a thermotropic material is suitable because it has excellent weather resistance and stability and is relatively inexpensive.

A gel obtained by crosslinking a part of these water-soluble polymers and swelling in a solvent such as water may be used as the thermotropic material. For example, US Pat.
As described in No. 2, a gel obtained by partially cross-linking the above-mentioned polymer solution, for example, a gel-like thermotropic material composed of a partially cross-linked product of hydroxyethyl methacrylate-hydroxyethyl acrylate copolymer and water is a preferred example. one of. However, as long as it is a liquid or wet gel-like thermotropic material that changes its state between a cloudy state and a transparent state due to a temperature change, various materials other than those described above may be used.

As the substrates 2 and 3, usually, flat inorganic glass or organic glass such as polycarbonate is used. Heat reflection glass, low radiation glass, laminated glass, tempered glass, double-strength glass, UV cut glass, meshed glass, template glass, ground glass, etc. can be arbitrarily adopted.
Usually, the bases 2 and 3 are configured to be transparent. However, a part of the bases 2 and 3 may be configured to be opaque, and when used as an outer wall of a building, at least one of the bases 2 and 3 is opaque. It may be composed of a simple glass plate, a metal plate or the like. The two substrates 2 and 3 may be of the same type or different types. Further, it is also possible to adopt glass in which at least one of them is formed in a block shape such as a glass block.

As the sealing material 5 adjacent to the thermotropic material, any material can be selected as long as it satisfies the following required characteristics, and it is preferable to use a combination of two or more types. It is. The main characteristics required for the sealing material of the light control glass of the present invention are as follows. (1) Adhering well to the glass constituting the light control glass and the synthetic resin film. (2) Gas retention is high, and it is difficult for gas to enter the thermotropic material through the sealing material or to release vapor of the thermotropic material. (3) No reaction that affects the properties of the contact portion with the thermotropic material occurs, and no substance is released. (4) Durability such as light resistance and heat resistance according to the place of use is ensured.

As a sealing material satisfying such characteristics, an adhesive isobutylene-based resin sealing material is used as shown in FIG.
And a two-stage sealing structure of a first sealing material 5a and a second sealing material 5b as shown in FIG. 2, which are within the scope of the present invention. . As the first sealing material 5a, a material having high gas retention such as a thermoplastic butyl rubber-based, polyisobutylene-based sealing material, or an adhesive isobutylene-based sealing material is used. As the outer second sealing material 5b, a deacetic acid type or deoxime-based material is used. It is preferable to select a material exhibiting good adhesiveness such as a silicone-based sealing material of a mold, an ultraviolet-curable acrylic adhesive, an adhesive isobutylene-based resin sealing material, and the like, and a preferable configuration of the sealing material of the light control glass of the present invention. However, the present invention is not limited to this.

Next, in the light control glass of the present invention, as shown in FIG. 2, it is preferable to provide a spacer 6 in the layer of the thermotropic material 4 for the purpose of uniformly adjusting and maintaining the layer thickness. This is a category of the present invention. Further, the spacer 6 may be provided also on the sealing material 5. By the action of the spacer 6, the layer thickness of the thermotropic material of the present invention exhibiting fluidity is adjusted and maintained at a desired value, and when used on a vertical surface, the glass deflects due to the weight of the thermotropic material. The phenomenon that the layer thickness of the thermotropic material is different between the upper and lower portions of the light control glass can be suppressed, and the layer thickness can be maintained uniform for a long period of time. The material of the spacer 6 is
From resin, glass, ceramic, metal, etc.,
It can be used as long as it does not react with the constituents of the thermotropic material, change its composition by adsorption or absorption, and affect the properties. Regarding the shape, in addition to the spherical shape shown in FIG. 3, various shapes such as a linear shape, a mesh shape, and a lattice shape can be selected. In the present invention, it is necessary to consider that this spacer does not become a noticeable visual defect, and from these points, a material made of colorless and transparent glass and a bead-shaped material are generally preferable choices. Become. When arranging bead-like materials, the minimum necessary amount of the thermotropic material 4
It is preferable to disperse and arrange the layers as uniformly as possible, and it depends on the size of the light control glass and the layer thickness of the thermotropic material, but it is generally present in an area of about 50 mm × 50 mm at a ratio of one or more. It is a quantitative guide. If the amount of the spacer is smaller than this, there is a possibility that the layer thickness of the thermotropic material is wavy at the portion where the spacer is present and at the portion where the spacer is not present, which may cause a problem that the view through the glass is distorted.
When a material made of a material harder than the synthetic resin film of the present invention is selected as the material of the spacer, since the spacer is held in a state of being sunk into the synthetic resin film, sedimentation of the spacer due to a difference in specific gravity between the spacer and the thermotropic material is performed. Can be suppressed. Further, the spacers may be bonded and fixed as necessary.

As shown in FIG. 2, it is possible to use a base material in which at least one of base members 2 and 3 is laminated with a locking film 7 made of a synthetic resin and use the base member facing the thermotropic material. The effect that the spacer 6 is fixed in a state of being sunk into the film is preferable. In particular, when the substrates 2 and 3 to be laminated are made of glass, using a shatterproof film as a locking film made of synthetic resin is a preferred form from the viewpoint of safety in the event of glass breakage. Further, a material made of a material softer than the spacer 6 is preferable because the effect as the engaging film 7 becomes more remarkable.

When the bases 2 and 3 on which the laminated film 7 is laminated are transparent, it is naturally preferable that the film is also transparent, and the material of the film for satisfying these conditions is polyethylene. , Polypropylene and other polyolefin resins, vinyl chloride resin, styrene resin, ABS resin, polyvinyl alcohol, acrylic resin, acrylonitrile-styrene resin, vinylidene chloride resin, AAS resin, AES resin, polyurethane resin, polyvinyl butyral resin, poly-4
-Methylpentene-1 resin, polybutene-1 resin, vinylidene fluoride resin, vinyl fluoride resin, fluorine resin, polycarbonate resin, polyamide resin, acetal resin, polyphenylene oxide resin, polyester resin such as polybutylene terephthalate, polyethylene terephthalate, polyphenylene Examples thereof include films of various resins such as a sulfide resin, a polyimide resin, a polysulfone resin, a polyethersulfone resin, an aromatic polyester resin, and a polyarylate resin, and a laminated film thereof. Among the above films, a polyester resin film is preferable from the viewpoints of rigidity, elongation resistance, dimensional stability, impact strength, transparency and lamination suitability, and more preferably polyethylene terephthalate (PET).

Specifically, those commercially available under the trade names such as Lumirror manufactured by Toray Industries, Inc., and emblet manufactured by Unitika Ltd. have high transparency and are preferred, but are not limited thereto. . The thickness of the base film of the locking film 7 of the present invention depends on the thickness of the thermotropic material.
Those with about 25 μm to 100 μm also exhibit sufficient effects,
It is preferable because it is easy to handle.

If necessary, known additives such as a plasticizer, a heat stabilizer, an antistatic agent, a lubricant, an ultraviolet absorber, and a filler may be added to these stop films.
In addition, since the stop film 7 is provided with an ultraviolet ray shielding function, when it is disposed outside the room, deterioration of the thermotropic material 4 and the sealing material 5 due to ultraviolet rays can be prevented. Further, even in the case where it is arranged indoors, it is possible to reduce the adverse effects of ultraviolet rays such as sunburn of people and objects in the room. The method of imparting the ultraviolet ray blocking function to the latch film 9 can be roughly classified into the following three types. (1) A method of compounding a light-shielding material represented by an aluminum foil (2) A method of using an inorganic UV-blocking agent (3) A method of using an organic UV-absorbing agent

The method (1), which blocks ultraviolet rays, is a technique often used for packaging materials for foods and medicines. However, these methods are not suitable for the present invention because they block the light itself. The method (2) is a method in which a white powder such as titanium oxide, zinc oxide, talc, kaolin, calcium carbonate or the like is kneaded into a film or dispersed and coated, and the ultraviolet light is blocked by absorption and scattering. is there. In order to maintain the transparency of the film, it is necessary that the particle size of these powders is sufficiently small with respect to the wavelength of visible light, and titanium dioxide having a particle size of 30 nm or less is generally used. However, when these white powders are mixed as metal cations in the material of the present invention, the discoloration due to deterioration may be remarkably accelerated, so that sufficient care is required.
The method (3) is a method using a salicylic acid-based, benzophenone-based, or benzotriazole-based organic ultraviolet absorber. As an application form, there is a method of directly kneading into a film or a method of coating. As a feature of these organic ultraviolet absorbers, the synthetic resin of the present invention can be melt-kneaded with a synthetic resin serving as a base material of a film and has high transparency compared to the inorganic ultraviolet blocker. This method is preferable as a method for imparting an ultraviolet shielding function to a locking film made of a resin. However, these organic ultraviolet absorbers have a narrow absorption range and a limited function,
Since it has a disadvantage that the light resistance itself is inferior, a method such as combining a plurality of organic ultraviolet absorbers or using the inorganic ultraviolet blocker in combination may be employed as necessary. . As the ultraviolet absorber used in the present invention, known compounds such as benzotriazole, benzophenone, indole and salicylic acid compounds can be used.

The hard coat layer is configured to improve the abrasion resistance of the film, thereby making it difficult for the film surface to be scratched or the like and improving the handling property. A transparent material that does not reduce the transmittance of the locking film is preferable, and a material containing a silicone resin as a main component is used.

Next, a method of manufacturing the light control glass 1 will be described. First, in the mixing step, after dissolving the nonionic surfactant and the inorganic electrolyte, which are the components of the thermotropic material, in water in a cylindrical container, a cellulose derivative is added, the container is closed, and the planetary system is used. It is preferable to mix the components of the thermotropic material by rotating the container by a combination of rotation and revolution by a stirring method, since a thermotropic material with less air bubbles can be obtained. If water is added after the cellulose derivative is added first, lumps are easily formed, which is not preferable. In addition, the components of the thermotropic material generate heat of dissolution by mixing. At this time, the temperature in the container is adjusted by using water cooled in advance, or by cooling the periphery of the container. It is preferred to keep it below the temperature.

Next, in the step of disposing the sealing material,
As shown in FIG. 4, the first sealing materials 5a ′ and 5b ′ are attached to the base 3. The attachment of the first sealing material 5a 'can be performed by using an extruder or an applicator provided with a heating device. In this case, an apparatus for applying a primary seal of a double-sealed double-glazed glass can be used almost as it is. Further, those processed in advance into a tape shape, a string shape, or the like and arranged in a release tape shape are preferable because they can be easily handled at room temperature. The attachment of the second sealing material 5b 'can be quantitatively and accurately applied by using a dispenser. When a sealant cartridge is used, a commercially available caulking gun can be used as it is. Further, it may be transferred to a syringe or the like and applied.

Here, as shown in FIG. 4, a central position between adjacent ones of the thermotropic materials 4 ', which are divided and arranged as described later, is used as a guide in the upper part of the first sealing material 5a'. May be provided. In addition, the second sealing material 5b is approximately 50 to 100 m as shown in FIG.
The gap 9 may be provided at intervals of approximately several mm to 10 mm at every m intervals. In such an attachment method, the opposing substrates 2,
5, the bases 2 and 3 are also temporarily laminated.
This is preferable because the closed space 11 made of the third sealing material 5b 'does not become airtight and the closed space 11 can be brought into a substantially vacuum state in the depressurization step. The recess 8 of the first sealing material 5a 'is not compressed and deformed in the subsequent contact step, and the first sealing material 5a'
a ′ adheres to the substrate 2 in an airtight manner.

Next, in the step of dividing and arranging the thermotropic material, the thermotropic material is applied onto the base 3, and the thermotropic material 4 'shown in FIG.
As shown in FIG. 6, the coating may be performed on the substrate 3 in an independent dot shape, or as shown in FIG. There is also a method of arranging only one required amount at the central portion on the base 3. For example, in a case where the size exceeds 500 mm square, the size of bubbles remaining in the four corners inside the first sealing material 5 a after the adhesion step Undesirably increases. In addition, since the upper substrate 2 is unstable in a decompression step described later, it is easy to move, and the positions of the substrate 2 and the substrate 3 are easily shifted. In addition, it is not preferable that the bases 2 and 3 are made of inorganic glass because they are easily broken. The number of the thermotropic materials 4 ′ divided and arranged increases as the effective area of the light control glass 1 increases.
Is preferably 10 to 50 mm. Further, in order to suppress bubbles remaining after the adhesion step described later, the area of the base 3 surrounded by the sealing material 5a 'is set to the effective area, and the intermediate line 10 of the divided arrangement position of the adjacent thermotropic material 4' is set.
When the area formed by the sealing material 5a ′ and the sealing material 5a ′ is defined as the side area, the product of the ratio of the side area to the effective area and the total arrangement volume of the thermotropic material is 100%.
On the other hand, the arrangement volume of the thermotropic material 4 'divided and arranged adjacent to the sealing material 5a' is 80 to 105%.
It is preferred that More preferably, it is 95 to 100%. If it is less than 80%, the amount of the thermotropic material 4 ′ divided and arranged adjacent to the sealing material 5 a ′ per area is too small as compared with the central portion, so that the thermotropic material 4 ′ in the vicinity of the sealing material 5 a ′ becomes too small. It is not preferable because it is difficult to spread to every corner and air bubbles are likely to remain. Also, if the filling amount per area of the thermotropic material 4 'divided and arranged adjacent to the sealing material 5a' is larger than the central portion, bubbles are less likely to remain, but the thermotropic material 4 'easily protrudes from the sealing material 5a'. It is not preferable.

Further, as shown in FIG.
It is preferable that the distance L between the divided arrangement position of the thermotropic material 4 'adjacent to a' and the sealing material 5a 'is 5 to 30 mm. More preferably, it is 10 to 25 mm, particularly preferably 10 to 20 mm. The interval L is 30m
If it exceeds m, the bubble size after the contacting step becomes large, and the bubble disappears after standing, and the tendency becomes prominent, especially at the four corners, which is not preferable. If the distance is less than 5 mm, the thermotropic material 4 ′ tends to protrude above the sealing material 5 a ′, which is not preferable.

Further, the sealing material 5a 'with respect to the distance L between the arrangement position of the thermotropic material 4' divided and arranged adjacent to the sealing material 5a 'and the sealing material 5a'.
It is preferable that the ratio of the arrangement position of the thermotropic material 4 'to be divided and arranged adjacently to the arrangement distance M of the adjacent thermotropic material 4' is in the range of 1.5 to 2.5. At this time, it is simple and preferable that the thermotropic material is applied in a constant amount over the entire surface, but when the ratio of the arrangement intervals is less than 1.5 or more than 2.5, the volume of the thermotropic material per area is reduced. In order to make the coating as uniform as possible, it is necessary to change the amount of application, and the operation becomes complicated, which is not preferable. As a method of dividing and arranging the thermotropic material 4 ', it is preferable to apply the material quantitatively by a dispenser. At this time, if the coating is performed using a dispenser having a plurality of coating heads, the coating can be quantitatively and quickly performed.

Next, in a temporary laminating step, as shown in FIG. 5, the substrates 2 and 3 are overlapped to produce a temporary laminated body 1 '. In the temporary laminate 1 ', the upper substrate 2 is supported by the sealing materials 5a' and 5b ',
A closed space 11 surrounded by the sealing materials 5a 'and 5b' is formed therebetween. Although the closed space 11 is surrounded by the sealing materials 5a 'and 5b',
And the space 9 is open to the atmosphere.
Next, in the decompression step, using a decompression device having two adjacent decompression tanks separated by a flexible film body, the temporary laminated body 1 ′ is set in the lower decompression tank and both decompressions are performed. The tank is depressurized, and the closed space 11 in which the thermotropic material 4 'is present is set to a substantially vacuum state. Then, in the subsequent contacting step, the depressurization of the upper depressurized tank is released so that the closed space 11 becomes airtight. The substrate 2 is compressed with the film at normal pressure, and the first sealing members 5a 'and 5b' are brought into close contact with the substrate 2 without any gap.

As the pressure reducing device, a laminator for manufacturing a general-purpose solar cell panel can be adopted.
And the like (US). As the degree of vacuum of the two decompression tanks at the time of depressurization is smaller, the degree of vacuum in the closed space 11 is higher, the number of air bubbles after the close contact is reduced, and the thermotropic material 4 'is easily filled completely. At this time, with the temporarily laminated substrates 2 and 3 installed, 0.1 to 20 Torr
It is preferable to hold for 10 to 100 seconds under a reduced pressure atmosphere of r. Here, even if the ultimate vacuum degree is too low, and even if the holding time is short, the bubble size after the adhesion step becomes large,
This is not good. On the other hand, if the holding time is too long, the evaporation of water as a constituent component from the surface of the disposed thermotropic material 4 'is undesirably large. Here, as the area of the light control glass 1 increases, the ultimate vacuum degree tends to decrease, so that the holding time is increased. For example,
Under a reduced pressure atmosphere of 0.1 Torr, a holding time of 10 to 30 seconds is taken, and at 1 Torr, a holding time of 10 seconds to 60 seconds.
In the case of seconds and 20 Torr, it is preferable to set 30 seconds to 100 seconds.

In the subsequent contact step, both depressurized tanks are depressurized and kept under a depressurized atmosphere for a predetermined time, and then the other depressurized tank is opened so that the closed space 11 of the temporary laminate 1 'is airtight. It is preferable to compress the temporary laminated body 1 ′ through the film body for 3 to 300 seconds by applying pressure, and to fill the airtight closed space 11 with the thermotropic material 4 ′. If the compression time is shorter than 3 seconds, the bubble size after the contacting step is large, and the contact of the first sealing material 5a 'is insufficient, which is not preferable. Further, even if it exceeds 300 seconds, the effect of reducing the bubble size is small, and the first sealing material 5a '
Has only a small effect on improving the adhesiveness, and it takes a long time, which is not preferable. According to this method, the depressurizing step of maintaining the closed space 11 in a substantially vacuum state and the contacting step of filling the closed space 11 with the thermotropic material 4 ′ can be performed continuously in the depressurizing device. Can be easily and efficiently performed.

In this embodiment, the dimming glass 1 in which the thermotropic material 4 is laminated between the two substrates 2 and 3 and the method of manufacturing the same are described. It is also possible to form a dimming glass having three or more substrates by laminating the same or different types of thermotropic materials on the glass 1. Also,
In this case, an air layer that is not filled with a thermotropic material can be formed between the substrates to enhance heat insulation and sound insulation.

[0038]

Next, an example of a specific example will be described. (Example 1) A thermotropic material used as a thermotropic material was prepared as follows. Hydroxypropylcellulose (HPC-L, manufactured by Nippon Soda Co., Ltd .; hereinafter, HPC) as a cellulose derivative; polyoxypropylene trimethylolpropane ether as a nonionic surfactant (Sannicks Triol TP-400, manufactured by Sanyo Chemical Industries, Ltd.) ), 3% as inorganic electrolyte and water
The aqueous sodium chloride solutions were mixed at a weight ratio of 5: 1: 9, respectively. A base plate of JIS standard float plate glass of 3 mm in thickness of 600 × 600 mm is used and a thermoplastic butyl rubber tape (1700 without naphthotherm butyl tape manufactured by PMG Co., Ltd.) is placed at a position 10 mm from the glass edge as a sealing material. And a silicone sealing material (K-Shin-Etsu Chemical Co., Ltd.)
E420). The adjusted thermotropic material is dispensed with a dispenser, and the gap between the arrangement positions of the thermotropic material adjacent to the butyl tape and the butyl tape is set to 46 mm. The temporary laminate was depressurized and adhered to each other with a pressure reducing device to obtain a light control glass. At this time, the ratio of the area formed by an intermediate line between the butyl tape adjacent to the thermotropic material to be divided and arranged adjacent to the butyl tape and the divided arrangement position of the adjacent thermotropic material to the total arrangement area of the thermotropic material When the product of the total arrangement volume of the thermotropic material and that of the thermotropic material is 100%, the arrangement volume of the thermotropic material to be divided and arranged adjacent to the butyl tape (hereinafter referred to as the filling rate) is 90% at the four corners, and , 100%.

Example 2 A thermotropic material was prepared in the same manner as in Example 1. The same base and sealing material as those used in Example 1 were used and arranged in the same manner. The mixed thermotropic material is dispensed with a dispenser at an arrangement interval of 20 mm, and an interval between the butyl tape and the arrangement position of the thermotropic material adjacent to the butyl tape is 10 mm.
Then, a glass having a thickness of 3 mm was layered on the upper surface, and the temporary laminate was depressurized and adhered to each other with a decompression device to obtain a light control glass. At this time, the filling rate of the thermotropic material was 100% at the four corners and 100% at the side.
%.

Comparative Example 1 A thermotropic material was prepared in the same manner as in Example 1. The same base and sealing material as those used in Example 1 were used and arranged in the same manner. The adjusted thermotropic material is dispensed by a dispenser, and the spacing between the thermotropic materials adjacent to the butyl tape and the butyl tape is 10 mm. The temporary laminate was depressurized and adhered to each other with a pressure reducing device to obtain a light control glass. At this time, the filling rate of the thermotropic material was 166% at the four corners and 125% at the sides.
Becomes

Comparative Example 2 A thermotropic material was prepared in the same manner as in Example 1. The same base and sealing material as those used in Example 1 were used and arranged in the same manner. The adjusted thermotropic material was dispensed by a dispenser, and the distance between the positions of the thermotropic material adjacent to the butyl tape and the butyl tape was set to 40 mm. The temporary laminate was depressurized and adhered to each other with a pressure reducing device to obtain a light control glass. At this time, the filling rate of the thermotropic material is 69% at the four corners and 86% at the sides.

Using Examples 1 and 2 and Comparative Examples 1 and 2, the size of bubbles remaining inside the butyl tape 1 day and 15 days after the adhesion, and the protrusion of the thermotropic material from the butyl tape Was measured. Table 1 shows the results.

[0043]

[Table 1]

As is apparent from Table 1, the filling rate of the thermotropic material close to the sealing material is 80 to 105.
In the light control glass of Examples 1 and 2 in the range of%, bubbles on the day after adhesion were as small as 1 mm at the maximum, and disappeared after 15 days. Also, there was no protrusion of the thermotropic material from the primary seal. On the other hand, in the light control glass of Comparative Example 1 in which the filling rate of the thermotropic material close to the sealing material exceeded 105%, bubbles on the day after adhesion were as small as 1 mm at the maximum, and disappeared after 15 days. The thermotropic material protruded from the primary seal. Further, in the light control glass of Comparative Example 2 in which the filling rate of the thermotropic material close to the sealing material was less than 80% at the four corners, the thermotropic material did not protrude from the primary seal, but one day after the close contact. The bubble was as large as 4 mm, and as large as 3 mm even after 15 days.

[0045]

The effects of the present invention have been made clear by the examples. According to the method of manufacturing the light control glass according to claim 1,
By setting each disposing volume of the thermotropic material divided and arranged adjacent to the sealing material in an appropriate range, it is possible to prevent the thermotropic material from protruding from the sealing material. In addition, since the size of bubbles remaining in the portion of the thermotropic material along the sealing material becomes smaller, the standing time until bubbles remaining immediately after the production of the light control glass dissolves in the thermotropic material and completely disappears. Can be significantly reduced.

In this case, when the divided arrangement position of the thermotropic material adjacent to the sealing material and the interval between the sealing materials are set to 5 to 30 mm, it is possible to prevent the thermotropic material from protruding above the sealing material. While preventing this, the bubble size immediately after the close contact can be further reduced. As described in claim 3, the arrangement position of the thermotropic material divided and arranged adjacent to the sealing material and the distance between the sealing material and the arrangement position of the thermotropic material divided and arranged adjacent to the sealing material are the same. When the arrangement interval ratio of the tropic material is in the range of 1.5 to 2.5, the operation of applying the thermotropic material can be simplified as compared with the case where the thermotropic material is applied over the entire surface.

As described in claim 4, in the depressurizing step, if the temporarily laminated substrate is kept in a depressurized atmosphere of 0.1 to 20 Torr for 10 to 100 seconds, the bubble size after the contacting step can be reduced, and the arrangement can be made. The amount of evaporation of water from the surface of the thermotropic material thus obtained can be reduced, the composition unevenness of the thermotropic material at the surface portion and the central portion can be prevented, and light control glass of good quality can be manufactured. Claim 5
According to the method described, both vacuum chambers are brought into a substantially vacuum state, and then only the vacuum state of the other vacuum chamber is released. This is preferable because the entire surface of the laminate can be compressed at atmospheric pressure through the film body, and the working efficiency can be improved.

According to the light control glass of the sixth aspect, by setting the arrangement volume of the thermotropic material divided and arranged adjacent to the sealing material within an appropriate range, the thermotropic material protrudes from the sealing material. Can be prevented. In addition, since the size of bubbles remaining in the portion of the thermotropic material along the sealing material can be reduced, the time required for bubbles remaining immediately after the production of the light control glass to dissolve in the thermotropic material and completely disappear is reduced. It can be significantly shortened. As described in claim 7, by using a cellulose derivative as a main component, a thermotropic material which is inexpensive and has excellent durability can be obtained. Further, by adding a nonionic surfactant, a thermotropic material which can be repeatedly transparent and opaque and can be maintained in a uniform turbid state for a long time can be obtained. Further, by adding an inorganic electrolyte, an optimum state change temperature according to the place of use can be set.

[Brief description of the drawings]

FIG. 1 is a sectional view of a main part of a light control glass of the present invention.

FIG. 2 is a cross-sectional view of a main part of a light control glass having another configuration.

FIG. 3 is a cross-sectional view of a main part of the tuning light glass.

FIG. 4 is an explanatory view of an arrangement method of a thermotropic material and a sealing material.

FIG. 5 is a sectional view of a main part of the temporary laminate.

FIG. 6 is an explanatory view of another arrangement method of a thermotropic material and a sealing material.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 Light control glass 2 Substrate 3 Substrate 4 Thermotropic material 5 Sealing material 5a First sealing material 5b Second sealing material 6 Spacer 7 Engagement film 8 Depression 9 Gap 10 Intermediate line 1 'Temporary laminate 4' Thermotropic material 5a ' First sealing material 5b 'Second sealing material 11 Closed space

 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 2E016 AA01 AA04 AA07 BA01 BA07 CA01 CB01 CC02 EA01 EA03 FA02 GA01 4G061 AA13 AA18 AA25 BA01 BA02 CB06 CB12 CB16 CD02 CD22 CD25 DA23 DA26 DA30

Claims (8)

[Claims] 1. A light control in which a thermotropic material which reversibly changes between a transparent state and a cloudy state due to a temperature change is sealed between a substrate having at least one part or the whole of which is transparent via a sealing material. In the method of manufacturing glass, a step of arranging a sealing material to adhere the sealing material to a peripheral portion on at least one substrate constituting the light control glass, and dividing the sealing material inside the sealing material by applying a , One of the broken lines, or a combination thereof, is surrounded by the middle line of the divided arrangement position of the adjacent thermotropic material and the attached sealing material with respect to the substrate area surrounded by the attached sealing material. Divided adjacent to the sealant for 100% of the product of the area ratio and the total arrangement volume of the thermotropic material A step of dividing the thermotropic material on the substrate under the condition that the arrangement volume of the thermotropic material to be disposed is 80 to 105%; and a step of overlapping the thermotropic material between the substrates by overlapping the opposing substrates. And a temporary laminating step of forming a closed space surrounded by the sealing material between the substrates, and a reduced pressure for maintaining the temporarily laminated substrates in a reduced-pressure atmosphere and maintaining the closed space in a substantially vacuum state. Under a reduced-pressure atmosphere, the sealing space is deformed and brought into close contact with each other so that the closed space becomes airtight while maintaining a substantially vacuum state, and a close contact step of filling the airtight closed space with the thermotropic material is provided. A method for producing a light control glass. 2. In the step of arranging the thermotropic material separately, the distance between the arranging position of the thermotropic material adjacent to the sealing material and the sealing material is 5 to 30 m.
The method for producing a light control glass according to claim 1, wherein m is m. 3. The thermotropic material divided and arranged adjacent to the sealing material with respect to the arrangement position of the thermotropic material divided and arranged adjacent to the sealing material and the interval between the sealing material in the thermotropic material dividing and arranging step. 3. The arrangement position ratio between the arrangement position and the adjacent thermotropic material is 1.5 to 2.5.
A method for producing the light control glass as described above. 4. In the decompression step, an apparatus having two adjacent decompression tanks, at least a part of which is partitioned by a flexible film, is used to set a temporarily laminated substrate in one of the decompression tanks. Reduce the pressure in the vacuum tank to 0.1-20 Torr
r is maintained for 10 to 100 seconds under a reduced pressure atmosphere of r.
4. The method for producing the light control glass according to any one of items 3 to 5. 5. In the contacting step, an apparatus having two adjacent decompression tanks, at least a part of which is partitioned by a flexible film, is used to set the temporarily laminated substrates in one of the decompression tanks. After depressurizing the depressurizing tank and maintaining it in a depressurized atmosphere for a predetermined time, the other depressurizing tank is opened to normal pressure so that the closed space is airtight, and the substrate temporarily laminated via the film body is removed. The method for producing a light control glass according to any one of claims 1 to 4, wherein the airtight closed space is filled with the thermotropic material by compressing for ~ 300 seconds. 6. A substrate having at least one part or all of which is transparent, a thermotropic material which reversibly changes between a transparent state and a cloudy state due to a temperature change, and sealing the thermotropic material between the substrates. A sealing material that adheres to the peripheral portion on one of the substrates, and the two substrates are arranged in such a manner that the thermotropic materials are arranged at intervals from each other on the one substrate surrounded by the sealing material. In the light control glass in which the thermotropic material is sealed between the substrates by overlapping, the intermediate line of the divided arrangement position of the adjacent thermotropic material with respect to the area of the substrate surrounded by the attached sealing material is attached. Product of the ratio of the area enclosed by the sealed sealing material and the total disposed volume of the thermotropic material.
The light control glass, wherein the volume of each of the thermotropic materials to be divided and arranged adjacent to the sealing material is set to 80 to 105% with respect to 0%. 7. The light control glass according to claim 6, wherein the thermotropic material comprises a cellulose derivative and water as constituents. 8. The light control glass according to claim 6, wherein the thermotropic material comprises a nonionic surfactant and, if necessary, an inorganic electrolyte in addition to the constituent components.