WO2011152500A1 - 水蒸気バリア性フィルム及びその製造方法 - Google Patents
水蒸気バリア性フィルム及びその製造方法 Download PDFInfo
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- WO2011152500A1 WO2011152500A1 PCT/JP2011/062735 JP2011062735W WO2011152500A1 WO 2011152500 A1 WO2011152500 A1 WO 2011152500A1 JP 2011062735 W JP2011062735 W JP 2011062735W WO 2011152500 A1 WO2011152500 A1 WO 2011152500A1
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- clay
- film
- water vapor
- vapor barrier
- barrier film
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-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/008—Additives improving gas barrier properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Definitions
- the present invention relates to a backsheet that is used by being disposed on the back side of a solar cell module. More specifically, the present invention relates to a clay coated with PET (polyethylene terephthalate) as a base material, and has water vapor barrier properties and gas barrier properties. In addition, the present invention relates to a film for a solar battery back sheet having excellent mechanical strength and heat resistance, and excellent productivity and quality, and a method for producing the same.
- PET polyethylene terephthalate
- the present invention has excellent weather resistance, can satisfy all the requirements of water vapor barrier properties, gas barrier properties, flexibility, heat resistance, electrical insulation and water resistance, and is easier to handle and roll-to-roll than conventional clay films.
- roll-type continuous production is possible, and in addition to the solar battery backsheet, for example, a novel water vapor that can be suitably used as a substrate or protective film for electronic devices such as LCD substrate films and LED films It provides new technologies and new products related to barrier films.
- a solar cell module is a unit in which several tens of solar cells (cells) are electrically wired in series or in parallel and a protective package is applied.
- the surface exposed to sunlight is covered with transparent glass or a transparent film, and a solar cell (cell) is sealed with a filler mainly composed of light-transmitting EVA (ethylene vinyl acetate copolymer resin).
- EVA ethylene vinyl acetate copolymer resin
- the back sheet has weather resistance (ultraviolet ray resistance, moisture resistance, heat resistance, salt damage resistance, etc.), water vapor barrier properties, electrical insulation properties, mechanical strength, chemical resistance to prevent peeling of the filler, discoloration, and corrosion of the wiring.
- weather resistance ultraviolet ray resistance, moisture resistance, heat resistance, salt damage resistance, etc.
- water vapor barrier properties electrical insulation properties
- mechanical strength mechanical strength
- chemical resistance to prevent peeling of the filler discoloration, and corrosion of the wiring.
- the compatibility of the adhesive integration with the filler is necessary. In particular, there is a demand for preventing intrusion of moisture, oxygen gas, etc., minimizing performance deterioration over the long term, having high durability, and being safe and low cost.
- thin-film solar cells have attracted attention in order to realize low cost and high efficiency of solar cells, and thin-film silicon solar cells such as amorphous silicon and crystalline silicon have been put into practical use.
- CdTe tellurization
- Flexible solar cells such as cadmium) and CIS / CIGS (copper indium selenide / copper indium gallium selenide) are also being developed and put to practical use.
- Flexible solar cells are expected to expand dramatically because of their light weight and good processability, and they can be used for a wide range of applications, including ground-mounted, roof-mounted, building material-integrated, consumer electronics, and automotive.
- the protective package is required to have flexibility, and its characteristics are a technical issue.
- Inorganic sheets are made by processing natural or synthetic minerals such as mica and vermiculite into sheets, which have high heat resistance and are used as a gas seal member as a gland packing. Therefore, the path through which minute gas molecules flow cannot be completely blocked, and the gas barrier property is not so high.
- the metal sheet has excellent gas barrier properties, it has drawbacks in weather resistance, electrical insulation, chemical resistance, etc., and its application is limited.
- various organic polymer materials are blended with inorganic materials as a dispersant, a thickener, and a binder in addition to a molding material.
- the laminated film has excellent moisture resistance and gas barrier properties and can be applied to food packaging and the like. Can be obtained (see Patent Document 2). Since the heat resistance of this type of laminated film is determined by the organic material having the lowest heat resistance, that is, in this case, polyolefin, this type of material is generally high heat resistance. I don't get it.
- Non-Patent Document 1 Various clays such as smectite, mica, talc and vermiculite have been added to the resin as fillers for the purpose of improving the heat resistance and gas barrier properties of the organic polymer resin, and its effects have been confirmed, but water dispersibility Since high smectite is hydrophilic, it has a low affinity for a hydrophobic resin and is difficult to be highly dispersed in the resin as it is to be combined. Therefore, when complexing with a hydrophobic resin, modified clay in which the clay is modified and the hydrophilicity / hydrophobicity is controlled is used (see Non-Patent Document 1).
- One method for producing the modified clay is ion exchange with a quaternary ammonium cation or a quaternary phosphonium cation. Hydrophilicity / hydrophobicity can be controlled by the type and introduction ratio of these organic cations (see Non-Patent Document 2). The other is silylation. A hydroxyl group exists at the terminal of the clay crystal, and the hydroxyl group and the added silylating agent react to make the terminal hydrophobic. In this case as well, hydrophilicity / hydrophobicity can be controlled by the type and introduction ratio of the silylating agent. These two types of reforming methods can be used in combination.
- an inorganic layered compound thin film is applied by applying the Langmuir-Blodgett Method (see, for example, Non-Patent Document 3).
- various methods for preparing functional inorganic layered compound thin films have been reported.
- a method for producing a clay thin film comprising forming an aqueous dispersion of a hydrotalcite-based intercalation compound into a film and drying the reaction (see Patent Document 3), utilizing a reaction between a clay mineral and phosphoric acid or a phosphate group, and the reaction
- a method for producing a clay mineral thin film in which the bond structure of the clay mineral is oriented and fixed by applying a heat treatment for promoting clay see Patent Document 4
- a film containing a complex compound of a smectite clay mineral and a bivalent or higher metal There are many cases including an aqueous composition for treatment (see Patent Document 5) and the like.
- an inorganic layered compound-oriented self-supporting film having mechanical strength that can be used as a self-supporting film and having a gas barrier property by highly orienting a laminate of clay particles has not been obtained so far.
- the inventors have invented and proposed a basic method for producing a clay self-supporting film by simple means as described below (see, for example, Patent Document 6).
- (1) Disperse clay particles in a liquid as a dispersion medium to prepare a uniform clay dispersion.
- This dispersion is poured into a tray or the like and allowed to stand to deposit clay particles, and the liquid as a dispersion medium is separated by solid-liquid separation means to form a clay film.
- a clay free-standing film is produced by optionally drying at a temperature of 110 to 300 ° C.
- the present inventors added a small amount of additives based on modified clay obtained by modifying clay, and have gas barrier properties and water vapor barrier properties, And the material which consists of a modified clay film
- membrane was proposed (patent document 7).
- this modified clay film is used in the field of electronic devices such as solar cells, displays, fuel cells, etc., for further gas barrier properties and water vapor barrier properties, flexibility and mechanical strength, high heat resistance, water resistance, weather resistance.
- the actual situation is that it has not been put into practical use.
- the present inventors satisfy the above-described further gas barrier property and water vapor barrier property, flexibility and mechanical strength, high heat resistance, water resistance, and weather resistance in view of the above-described conventional technology.
- the modified clay was greatly improved, and a preferable modified clay and an additive suitable for the modified clay, a suitable mixing ratio of the modified clay and the additive, a suitable solid-liquid ratio of the dispersion, a preferred dispersion method, etc.
- a laminate in which a modified clay paste is coated on a resin film can greatly improve the water vapor barrier and gas barrier properties of the resin film and improve the adhesion between the resin film and the clay film. Found that, it has led to the completion of the present invention.
- the present invention is obtained by applying a modified clay on a resin film, orienting and crystallizing clay crystals, having flexibility, mechanical strength, excellent thermal stability,
- An object of the present invention is to provide a water vapor barrier film for a solar battery back sheet having improved water vapor barrier properties, water resistance and gas barrier properties, and a method for producing the same.
- the present invention for solving the above-described problems comprises the following technical means.
- the clay film is composed of an additive composed of clay and a thermoplastic or thermosetting resin, 2)
- the weight ratio of clay to the total solid is 60 to 90% by weight, 3)
- water-resistant heat treatment is applied,
- the permeability coefficient of oxygen gas at room temperature is less than 4.0 ⁇ 10 ⁇ 15 cm 2 s ⁇ 1 cmHg ⁇ 1
- the volume resistivity in the vertical direction of the film is 10 M ⁇ or more
- the water vapor permeability is 3 g / m 2.
- the additive is polyimide.
- a clay paste prepared from clay, an additive made of thermoplastic or thermosetting, and a dispersion medium is applied to a resin film with a flat surface, dried, the solvent as the dispersion medium is removed, and then water resistant
- a method for producing a water vapor barrier film for performing a heat treatment 1) the clay has at least 90% mol% lithium ions in the interlayer ionic material; 2) In the clay film, the weight ratio of clay to the total solid is 60 to 90% by weight, 3) The temperature condition of the heat-resistant heat treatment is 100 to 200 ° C.
- a method for producing a water vapor barrier film comprising: (6) The method for producing a water vapor barrier film according to the above (5), wherein the clay is natural or synthetic clay, and a raw material clay is mixed with a silylating agent. (7) The method for producing a water vapor barrier film according to (5), wherein the resin film is made of polyethylene terephthalate (PET). (8) The method for producing a water vapor barrier film according to the above (5), which is flexible, excellent in flexibility, and capable of roll-to-roll continuous coating. (9) A solar battery backsheet comprising the water vapor barrier film according to any one of (1) to (4).
- the present invention is a film having a water vapor barrier property in which a clay film is coated and dried on a resin film substrate, and the clay film is composed of an additive composed of clay and a thermoplastic or thermosetting resin.
- the weight ratio of the clay to the total solid is 60 to 90% by weight, and after the coating and drying, a water-resistant heat treatment is performed, and the permeability coefficient of oxygen gas at room temperature is 4.0 ⁇ 10 ⁇ 15 cm.
- the volume resistivity in the vertical direction of the membrane is 10 M ⁇ or more, and the water vapor permeability is less than 3 g / m 2 ⁇ day (measurement method: cup method, test time: 140 hr). It is characterized by being.
- the present invention provides a method for producing a water vapor barrier film, wherein clay, a thermoplastic or thermosetting additive, and a clay paste prepared from a dispersion medium are applied to a resin film having a flat surface. Drying, removing the solvent as a dispersion medium, and then performing a water-resistant heat treatment, wherein the clay has an interlayer ionic substance containing at least 90% mol% lithium ions.
- the weight ratio of the clay to the total solid is 60 to 90% by weight, and the temperature condition of the water-resistant heat treatment is 100 to 200 ° C.
- the water vapor barrier film of the present invention is a laminated film obtained by coating a modified clay on a resin film, has water vapor barrier properties, and has a water vapor permeability of 3 g / m at 40 ° C. and a relative humidity of 90%.
- the film is less than 2 ⁇ day (JIS Z0208-1976, cup method), heat resistant, flexible, and capable of continuous coating, and can be produced efficiently.
- hydrophobicity by silylation and organic cation exchange with high water resistance, or lithium ion exchange, or a combination of these treatments are combined to disperse the modified clay and a small amount of water-resistant additive in a solvent.
- this clay paste is applied to a resin film with a flat surface, dried, and a solvent as a dispersion medium is removed to produce a laminated film.
- water-resistant heat treatment is performed at a temperature higher than the coating drying temperature. Thereby, a water vapor barrier film having high water resistance, flexibility, excellent gas barrier properties and high heat resistance can be obtained.
- the clay used in the present invention is a natural or synthetic material, for example, one or more of beidellite, nontronite, saponite, hectorite, stevensite, and montmorillonite belonging to the smectite system from the crystal structure and characteristics, preferably purified.
- examples include bentonite or synthetic smectite.
- refined bentonite is a natural clay having a high smectite content.
- what made the silylating agent react with clay is illustrated. At that time, the composition of the silylating agent with respect to the total weight of the clay and the silylating agent is less than 30% by weight.
- the silylating agent contained in the clay of the present invention is not particularly limited, but methyltrimethoxysilane, methyltriethoxysilane, propyltrimethoxysilane, butyltrimethoxysilane, hexyltrimethoxysilane, octyltrimethoxy Examples include silane, dodecyltrimethoxysilane, and octadecyltrimethoxysilane.
- Examples of the method for introducing the silylating agent into the clay include a method in which about 2% by weight of the silylating agent is mixed with the raw clay and the raw clay and milled with a ball mill for about one hour.
- silylating agents for preparing silylated clay are commercially available, and some have reactive functional groups such as epoxy groups, acrylic groups, amino groups, halogens. It has a reactive functional group such as a group. Silylated clays prepared using a silylating agent having such a reactive end have a reactive end at the end and can be subjected to various chemical reactions.
- silylated clay having various different reactive ends can be prepared, silylated clay A having one reactive end and silylated clay B having another reactive end are mixed together. It is possible to form a film as a raw material and chemically bond the reactive ends of clay A and clay B to each other during the film formation or after the film formation. Thereby, it is possible to improve light transmittance, gas barrier property, water vapor
- the interlayer lithium moves into the clay octahedron layer, and the ion component between the layers decreases, thereby improving water resistance.
- This improvement in water resistance is noticeable when the lithium ion is 90 mol% or more of the ionic substances between the layers.
- the heat treatment is usually after film formation, and the effect appears from a temperature condition of about 100 ° C. Conditions on the high temperature side can be appropriately set depending on the heat resistance of the resin film as the base material.
- the heat treatment time is 20 minutes or more and 24 hours or less. When the temperature is low, a longer treatment time is required.
- thermoplastic resins such as polyethylene, polypropylene, polyvinyl chloride, polystyrene, ABC resin, PET resin and other general-purpose plastics, polycarbonate, fluororesin and acetal resin, so-called engineering plastics
- main plastics such as phenolic resin, melamine resin, urea resin, polyurethane, epoxy resin, unsaturated polyester, polyimide and the like, which are thermosetting resins, are effective as the additive of the present invention.
- polyamide and polyimide are preferable, and polyimide is preferable.
- the modified clay used in the present invention is well dispersed in an organic solvent.
- Such an additive and modified clay have an affinity for each other, and when they are mixed in an organic solvent, they are easily combined and combined.
- a uniform dispersion obtained by adding modified clay and additives to an organic solvent is prepared to obtain a clay paste.
- the dispersion is prepared by dispersing the modified clay and then adding the additive, dispersing the modified clay in the solution containing the additive, and simultaneously adding the modified clay and the additive to the dispersion medium. And a method in which the modified clay and additives are separately made into dispersions and mixed together.
- the modified clay is added to a solvent to prepare a dilute and uniform modified clay dispersion.
- the modified clay concentration in the modified clay dispersion is preferably 0.3 to 15% by weight, more preferably 1 to 10% by weight.
- the concentration of the denatured clay is too low, drying takes too much time, and there is a problem that continuous coating becomes difficult.
- the concentration of the modified clay is too high, the modified clay will not disperse well, so it will easily generate lumps and uniform coating will not occur. Problems such as film thickness non-uniformity occur.
- the dispersion is degassed as necessary.
- a method of deaeration treatment for example, there is a method by vacuuming, heating, centrifugation, etc., but a method including vacuuming is more preferable.
- a degassed dispersion, so-called clay paste is applied to the resin film with a certain thickness.
- the coating method is not particularly limited.
- the resin film examples include, but are not limited to, resins such as acrylic, polyolefin, polyvinyl chloride, fluorine, and polyester.
- resins such as acrylic, polyolefin, polyvinyl chloride, fluorine, and polyester.
- PET which is a versatile polyester, as a resin film.
- the thickness dimension is also determined from the design values of the solar cell module and the back sheet, and is not particularly limited. Generally, the thickness is 5 to 300 ⁇ m.
- the thickness of the clay film of the present invention a film having an arbitrary thickness can be obtained by increasing or decreasing the solid weight used in the dispersion.
- a thinner film tends to be excellent in surface smoothness.
- the flexibility is reduced by increasing the thickness of the film, and the coating thickness of the clay paste is desirably 0.5 mm or less.
- highly orienting the lamination of the clay particles means that the unit structure layers (thickness of about 1 nm to 1.5 nm) of the clay particles are stacked with the direction of the layer surface being the same, and in the direction perpendicular to the layer surface, It means having a high periodicity.
- a thin and uniform clay paste containing clay and additives is applied to the resin film, and the liquid as a dispersion medium is slowly evaporated to make the clay particles dense. It is important to form a laminated film.
- drying conditions by a heat-drying method are based also on the kind of solvent to be used, it is the temperature conditions of room temperature to 90 degreeC, More preferably, the temperature conditions of 30 degreeC to 60 degreeC are about 10 minutes to 24 hours. Set the time for the solvent to evaporate completely. Next, water resistance treatment is performed under a temperature condition of 100 to 200 ° C. The time is about 40 hours at 140 ° C., depending on the processing temperature.
- the water resistance treatment temperature is determined by the heat resistance temperature of the resin film.
- a heat resistant temperature of general PET which is inexpensive and versatile is approximately 140 ° C., but a stretched PET film has a heat resistant temperature of approximately 200 ° C.
- the clay film on the resin film has a film thickness of 3 to 100 ⁇ m, preferably 3 to 80 ⁇ m, and the gas barrier performance of the obtained water vapor barrier film is that the permeability coefficient of oxygen gas at room temperature is 4.0 ⁇ 10 It is less than ⁇ 15 cm 2 s ⁇ 1 cmHg ⁇ 1 , and the volume resistivity in the vertical direction of the film is 10 M ⁇ or more.
- the clay film can be widely used as an electric insulating film by making use of its electric insulating properties.
- the water vapor barrier film of the present invention has flexibility and excellent workability.
- the film of the present invention is composed of a clay film containing silicate as a main component, is excellent in ultraviolet resistance and radiation resistance, and is suitable as a solar battery back sheet. Further, the water vapor barrier film is chemically stable and can maintain water resistance, and can be used as a flexible packaging material, sealing material, insulating material, and the like.
- the water vapor barrier film according to the present invention is excellent in weather resistance and can satisfy all the requirements of water vapor barrier property, gas barrier property, flexibility, heat resistance, electrical insulation and water resistance.
- the water vapor barrier film of the present invention can be suitably used as a substrate or a protective film for electronic devices such as a substrate film for LCD and a film for LED, in addition to a solar battery backsheet.
- the water vapor barrier film of the present invention can also be suitably used as a flexible gas seal material, packaging material, sealing material, electrical insulating material, and the like.
- the water vapor barrier film of the present invention can be widely used as a multilayer film by laminating with, for example, metal, plastic, rubber, paper, ceramic and the like.
- silylated clay 24 g was added to 400 mL of a 0.5 N aqueous lithium nitrate solution, and mixed and dispersed by shaking. The mixture was shaken and dispersed for 2 hours to exchange the interlayer ions of the clay with lithium ions. Next, the dispersion was subjected to solid-liquid separation by centrifugation, and the obtained solid was washed with a mixed solution of 280 g of distilled water and 120 g of ethanol to remove excess salt. This washing operation was repeated twice or more. The obtained product was sufficiently dried in an oven and then crushed to obtain lithium exchanged clay.
- the clay paste was applied on a PET film with a casting knife so as to have a uniform thickness.
- the coating thickness of the paste was 0.25 mm.
- the PET film used was Toyobo Ester (registered trademark) A4300 manufactured by Toyobo Co., Ltd., with a thickness of 75 ⁇ m.
- a uniform clay-PET film having a thickness of 3.5 ⁇ m is obtained by drying the coated clay film together with the PET film in a forced air oven at 60 ° C. overnight. A coated film was obtained. The obtained clay-PET film coating film was placed in an oven and subjected to a heat treatment at 140 ° C., which is below the softening point of the PET film, for 40 hours to 216 hours to obtain a predetermined water vapor barrier film. .
- the water vapor permeability of the water vapor barrier film was measured for the PET / clay film produced in Example 1 above using a moisture sensor (trade name: L80-5000, manufactured by Lyssy). .
- the lower atmosphere was adjusted to a relative humidity of 100% and the upper atmosphere was adjusted to a relative humidity of 9.9% or less, respectively, with a 50 cm 2 sample film.
- the water vapor transmission rate (g / m 2 ⁇ day) is determined from the time until the relative humidity of the atmosphere on the upper side of the sample film becomes 9.9% to 10.1% by the water vapor passing through the clay film. Calculated.
- the results are shown in Table 2.
- the water vapor permeability measured by a humidity sensor is 1.9 and 2.0 (g / m 2 ⁇ day), and a result consistent with the value measured by the cup method was obtained. Also, it was confirmed that there was no difference between the front and back sides by the film setting method.
- the present invention has excellent water vapor barrier properties, water resistance, excellent gas barrier properties, flexibility, and a multilayer film formed by lamination with other material films, and the surface of other materials.
- the present invention relates to a water vapor barrier film that can be used as a protective film, and according to the present invention, provides a water vapor barrier film that has the above-described characteristics and can be used for many products in addition to a back sheet for a solar cell. be able to.
- the water vapor barrier film of the present invention is an LCD substrate film, an organic EL substrate film, an electronic paper substrate film, an electronic device sealing film, a PDP film, an LED film, an IC tag film, and a solar cell protection film.
- Films for electronic devices such as films, optical communication members, other flexible films for electronic devices, various functional films, film for food packaging, film for beverage packaging, film for pharmaceutical packaging, film for daily use packaging It is useful as a packaging film for industrial products, a packaging film for various products, a multilayer packaging film, an antioxidant film, a corrosion-resistant film, a weather-resistant film, a non-flammable film, a heat-resistant film, a chemical-resistant film, and the like.
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Abstract
Description
(1)粘土粒子を分散媒である液体に分散し、均一な粘土分散液を調整する。
(2)この分散液をトレイ等に流入し、静置して粘土粒子を沈積させ、分散媒である液体を固液分離手段で分離し、粘土膜を形成する。
(3)任意に110~300℃の温度条件下で乾燥し、粘土自立膜を製作する。
(1)樹脂フィルムの基材に、粘土膜が塗工、乾燥された水蒸気バリア性を有する積層フィルムであって、
1)粘土膜が、粘土と熱可塑性又は熱硬化性樹脂からなる添加物から構成され、
2)粘土膜において、粘土の全固体に対する重量比が60~90重量%であり、
3)塗工、乾燥後に、耐水化熱処理が施され、
室温における酸素ガスの透過係数が4.0×10-15cm2s-1cmHg-1未満であり、膜の垂直方向への体積抵抗率が10MΩ以上であり、水蒸気透過度が3g/m2・day未満(測定法:カップ法、試験時間:140hr)であることを特徴とする水蒸気バリア性フィルム。
(2)前記粘土が、精製ベントナイト、あるいは合成スメクタイトであり、粘土の層間の交換性イオンの少なくとも90モル%が、リチウムイオンである、前記(1)記載の水蒸気バリア性フィルム。
(3)前記添加物が、ポリイミドである、前記(1)記載の水蒸気バリア性フィルム。
(4)前記樹脂フィルムが、ポリエチレンテレフタレート(PET)製である、前記(1)記載の水蒸気バリア性フィルム。
(5)前記(1)から(4)のいずれかに記載の水蒸気バリア性を有する積層フィルムを製造する方法において、
粘土と、熱可塑性又は熱硬化性からなる添加物と、分散媒から調製される粘土ペーストを、表面が平坦な樹脂フィルムに塗工、乾燥し、分散媒である溶剤を除去し、次いで、耐水化熱処理を行う水蒸気バリア性フィルムの製造方法であって、
1)粘土が、層間のイオン性物質が少なくとも90%モル%のリチウムイオンを有し、
2)粘土膜において、粘土の全固体に対する重量比が60~90重量%であり、
3)耐水化熱処理の温度条件が100~200℃である、
ことを特徴とする水蒸気バリア性フィルムの製造方法。
(6)前記粘土が、天然あるいは合成粘土であり、原料粘土に対してシリル化剤を混合したものである、前記(5)記載の水蒸気バリア性フィルムの製造方法。
(7)前記樹脂フィルムが、ポリエチレンテレフタレート(PET)製である、前記(5)記載の水蒸気バリア性フィルムの製造方法。
(8)フレキシブルであり、屈曲性に優れ、ロールツーロール方式の連続塗工が可能である、前記(5)記載の水蒸気バリア性フィルムの製造方法。
(9)前記(1)から(4)のいずれかに記載の水蒸気バリア性フィルムからなることを特徴とする太陽電池バックシート。
本発明は、樹脂フィルムの基材に、粘土膜が塗工、乾燥された水蒸気バリア性を有するフィルムであって、粘土膜が、粘土と熱可塑性又は熱硬化性樹脂からなる添加物から構成され、粘土膜において、粘土の全固体に対する重量比が60~90重量%であり、塗工、乾燥後に、耐水化熱処理が施され、室温における酸素ガスの透過係数が4.0×10-15cm2s-1cmHg-1未満であり、膜の垂直方向への体積抵抗率が10MΩ以上であり、水蒸気透過度が3g/m2・day未満(測定法:カップ法、試験時間:140hr)であることを特徴とするものである。
(1)本発明による水蒸気バリア性フィルムは、耐候性に優れ、水蒸気バリア性、ガスバリア性、柔軟性、耐熱性、電気絶縁性及び耐水性の要件を全て満たすことができる。
(2)本発明の水蒸気バリア性フィルムは、太陽電池バックシートのほか、例えば、LCD用基板フィルム、LED用フィルム、等の電子デバイス用の基板や保護フィルムとして好適に用いることができる。
(3)本発明の水蒸気バリア性フィルムは、柔軟なガスシール材料、包装材料、封止材料、電気絶縁材料等としても好適に用いることができる。
(4)本発明の水蒸気バリア性フィルムは、例えば、金属、プラスチック、ゴム、紙、セラミック等と積層することによって、多層膜として広範に用いることが可能である。
天然の精製ベントナイト(クニピアF クニミネ工業株式会社製)を、オーブンで110℃以上の温度で十分乾燥させた。当該ベントナイト300gを、アルミナボールとともに、ボールミルポットに入れた。次に、これに、シリル化剤(チッソ株式会社製 サイラエースS330)6gを加え、ポット内を窒素ガスに置換し、1時間のボールミル処理を行うことにより、シリル化粘土を得た。シリル化剤には、端末にアミノ基を持つものを使用した。
上記リチウム交換粘土10gを容器に取り、90gの純水を加え、混練することにより、リチウム交換粘土プレゲルを調製した。得られたゲルを、ホモジナイザー(IKA社製 ULTORA TURRAX T50,シャフトは同社製 S50N-G45F)を使って、ジメチルアセトアミドに分散させた。
次に、上記粘土ペーストを、PETフィルム上に、キャスティングナイフにより、均一厚みとなるように塗工した。ここで、ペーストの塗工厚みを0.25mmとした。また、PETフィルムは、東洋紡績(株)製の東洋紡エステル(登録商標)A4300、厚さ75μmを使用した。
上記140℃の加熱処理を施したPETフィルム単体及び水蒸気バリア性フィルムの40℃、相対湿度90%における水蒸気透過度を、JIS Z0208-1976に規定する、カップ法により、試験評価時間140hrで、比較測定した。測定に際し、水蒸気バリア性フィルムの粘土膜層が、カップの内側になるように取り付けた。測定された水蒸気透過度を表1に示す。
2 樹脂フィルム(PET)
3 コーティングロール
4 バックアップロール
5 塗工液(粘土ペースト)
6 カキトリ刃
Claims (9)
- 樹脂フィルムの基材に、粘土膜が塗工、乾燥された水蒸気バリア性を有する積層フィルムであって、
(1)粘土膜が、粘土と熱可塑性又は熱硬化性樹脂からなる添加物から構成され、
(2)粘土膜において、粘土の全固体に対する重量比が60~90重量%であり、
(3)塗工、乾燥後に、耐水化熱処理が施され、
室温における酸素ガスの透過係数が4.0×10-15cm2s-1cmHg-1未満であり、膜の垂直方向への体積抵抗率が10MΩ以上であり、水蒸気透過度が3g/m2・day未満(測定法:カップ法、試験時間:140hr)であることを特徴とする水蒸気バリア性フィルム。 - 前記粘土が、精製ベントナイト、あるいは合成スメクタイトであり、粘土の層間の交換性イオンの少なくとも90モル%が、リチウムイオンである、請求項1記載の水蒸気バリア性フィルム。
- 前記添加物が、ポリイミドである、請求項1記載の水蒸気バリア性フィルム。
- 前記樹脂フィルムが、ポリエチレンテレフタレート(PET)製である、請求項1記載の水蒸気バリア性フィルム。
- 請求項1から4のいずれかに記載の水蒸気バリア性を有する積層フィルムを製造する方法において、
粘土と、熱可塑性又は熱硬化性からなる添加物と、分散媒から調製される粘土ペーストを、表面が平坦な樹脂フィルムに塗工、乾燥し、分散媒である溶剤を除去し、次いで、耐水化熱処理を行う水蒸気バリア性フィルムの製造方法であって、
(1)粘土が、層間のイオン性物質が少なくとも90%モル%のリチウムイオンを有し、
(2)粘土膜において、粘土の全固体に対する重量比が60~90重量%であり、
(3)耐水化熱処理の温度条件が100~200℃である、
ことを特徴とする水蒸気バリア性フィルムの製造方法。 - 前記粘土が、天然あるいは合成粘土であり、原料粘土に対してシリル化剤を混合したものである、請求項5記載の水蒸気バリア性フィルムの製造方法。
- 前記樹脂フィルムが、ポリエチレンテレフタレート(PET)製である、請求項5記載の水蒸気バリア性フィルムの製造方法。
- フレキシブルであり、屈曲性に優れ、ロールツーロール方式の連続塗工が可能である、請求項5記載の水蒸気バリア性フィルムの製造方法。
- 請求項1から4のいずれかに記載の水蒸気バリア性フィルムからなることを特徴とする太陽電池バックシート。
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