WO2012029464A1 - 太陽電池封止材及びそれを用いて作製された太陽電池モジュール - Google Patents
太陽電池封止材及びそれを用いて作製された太陽電池モジュール Download PDFInfo
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- WO2012029464A1 WO2012029464A1 PCT/JP2011/067227 JP2011067227W WO2012029464A1 WO 2012029464 A1 WO2012029464 A1 WO 2012029464A1 JP 2011067227 W JP2011067227 W JP 2011067227W WO 2012029464 A1 WO2012029464 A1 WO 2012029464A1
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- WIPO (PCT)
- Prior art keywords
- solar cell
- ethylene
- resin
- layer
- olefin
- Prior art date
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Images
Classifications
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- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/048—Encapsulation of modules
- H01L31/0481—Encapsulation of modules characterised by the composition of the encapsulation material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/04—Homopolymers or copolymers of ethene
- C09J123/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/048—Encapsulation of modules
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09K2200/0617—Polyalkenes
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09K2200/0617—Polyalkenes
- C09K2200/062—Polyethylene
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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
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
- Y10T428/2852—Adhesive compositions
- Y10T428/2878—Adhesive compositions including addition polymer from unsaturated monomer
Definitions
- the present invention relates to a solar cell element sealing material in a solar cell module and a solar cell module manufactured using the same, and more specifically, the solar cell module can be easily formed, and the long-term stability of adhesiveness and adhesive force.
- the present invention relates to a solar cell sealing material excellent in transparency, heat resistance, and the like, and a solar cell module manufactured using the same.
- a solar cell is a power generator that directly converts solar light energy into electricity. Photovoltaic power generation does not require burning fuel such as oil during power generation, and does not generate greenhouse gas (such as CO 2 ) or harmful waste (such as crude ash or heavy oil ash) due to combustion. Recently, it has attracted attention as one of the clean energy.
- a solar cell is a device in which a large number of solar cell elements (cells) are wired in series and parallel, and since it is installed outdoors, it avoids the effects of moisture and dust, and it is resistant to collisions such as firewood and pebbles or wind pressure. The solar cell element is sealed in a resin so as to withstand, and the outside is protected by glass or a sheet. Such a structure is called a solar cell module.
- a surface on which sunlight is applied is an upper protective material
- a transparent substrate glass / translucent solar cell sheet; front sheet
- a back surface is a lower protective material.
- a back surface sealing sheet for example, polyvinyl fluoride resin film
- a sealing material for example, ethylene-vinyl acetate copolymer.
- sealing material sealing resin layer
- water vapor barrier properties flexibility to protect solar cell elements
- process suitability in solar cell module manufacturing specifically cells and wiring
- Adhesiveness with a sheet and a cell, durability, dimensional stability, insulation, etc. are mainly required.
- EVA ethylene-vinyl acetate copolymer
- Patent Document 1 ethylene-vinyl acetate copolymer
- Patent Document 2 discloses an amorphous ⁇ -olefin polymer and a crystalline ⁇ -olefin polymer as solar cell encapsulants that do not use an EVA sheet and that can omit the crosslinking step.
- the solar cell sealing material which consists of a resin composition to contain is disclosed, Specifically, the resin composition which consists of a polymer which has a propylene as a main component is used.
- Patent Document 3 discloses a solar cell encapsulating material characterized by being a polymer blend or polymer alloy comprising at least one polyolefin copolymer and at least one crystalline polyolefin.
- Patent Document 4 discloses a solar cell encapsulant having a silane-modified resin (silane crosslinkable resin) obtained by polymerizing an ethylenically unsaturated silane compound and a polymerization polyethylene.
- the resin composition comprising a polymer mainly composed of propylene used in Patent Document 2 still has insufficient transparency (total light transmittance: 83.2% (see Examples)). . Further, the polymer mainly composed of propylene has a problem that the embrittlement temperature is high and the low temperature characteristics are insufficient. Moreover, in the example of the polymer blend used in Patent Document 3, the transparency is not necessarily good, and there is still a problem in balancing the flexibility, heat resistance and transparency. In the filler layer for a solar cell module of Patent Document 4, when a large amount of a silane-modified resin is added so as to sufficiently exhibit adhesion to an adherend such as glass or a back sheet, haze increases and transparency decreases.
- An object of the present invention is to provide a solar cell encapsulant that is easy to form a solar cell module and excellent in adhesion, long-term stability of adhesive strength, transparency, and heat resistance, and a solar cell produced using the solar cell encapsulant The object is to provide a battery module.
- the inventors of the present invention contain an adhesive layer, an ethylene- ⁇ -olefin random copolymer having specific thermal characteristics, and an ethylene- ⁇ -olefin block copolymer having specific thermal characteristics. It has been found that a solar cell encapsulant having a layer made of a resin composition can satisfy adhesiveness, long-term stability of adhesive strength, transparency and heat resistance at the same time, and has completed the present invention.
- the present invention includes at least an adhesive layer, in particular, a layer ((I) layer) comprising a specific resin composition (Z) containing a polyethylene resin (X) and a silane-modified ethylene resin (Y), A resin composition comprising an ethylene- ⁇ -olefin random copolymer (A) that satisfies the following condition (a) and an ethylene- ⁇ -olefin block copolymer (B) that satisfies the following condition (b):
- the solar cell sealing material which has a layer ((II) layer) which consists of C).
- the calorie of crystal melting measured at a heating rate of 10 ° C./min in differential scanning calorimetry is 0 to 70 J / g.
- the crystal melting peak temperature measured at a heating rate of 10 ° C./min in differential scanning calorimetry is 100 ° C. or more, and the crystal melting heat amount is 5 to 70 J / g.
- the solar cell module can be easily formed, and the solar cell encapsulant excellent in both adhesiveness, long-term stability of adhesive force, transparency and heat resistance, and the sun produced using the solar cell encapsulant
- a battery module can be provided.
- the manufacturing facility can be applied to a roll-to-roll manufacturing facility in addition to a batch manufacturing facility. It is also possible to prevent a decrease in transparency during regeneration addition.
- the term “main component” is intended to allow other components to be contained within a range that does not interfere with the action and effect of the resin constituting each layer of the solar cell encapsulant of the present invention. . Further, this term does not limit the specific content, but generally, when the total component of the resin composition is 100 parts by mass, it is 50 parts by mass or more, preferably 65 parts by mass or more, Preferably, the component occupies a range of 80 parts by mass or more and 100 parts by mass or less.
- the layer (I) is an adhesive layer, and in the solar cell encapsulant of the present invention, it is of course an adhesive layer and a surface layer. It is a layer having a role.
- the resin composition used for the (I) layer is not particularly limited, but it is produced when the solar cell encapsulant is formed in addition to the adhesiveness, long-term stability of adhesive strength, transparency and heat resistance. From the viewpoint of properties, those having a polyolefin resin as a main component are preferably used.
- the polyolefin-based resin used for the layer (I) is not particularly limited, but from the viewpoint of adhesiveness, transparency, productivity, and industrial availability, an ethylene-methyl methacrylate copolymer (E -MMA), ethylene-ethyl acrylate copolymer (E-EAA), ethylene-glycidyl methacrylate copolymer (E-GMA), ethylene-vinyl alcohol copolymer (EVOH), ionomer resin (ionic crosslinkable ethylene- At least one modified polyolefin resin selected from the group consisting of a methacrylic acid copolymer, an ion-crosslinkable ethylene-acrylic acid copolymer), a silane-modified polyolefin (silane-crosslinkable polyolefin), and a maleic anhydride graft copolymer; Preferably used.
- E MMA ethylene-methyl methacrylate copolymer
- E-EAA ethylene-ethyl
- a silane crosslinkable polyolefin or an ionomer resin can be preferably used from the viewpoint of adhesiveness and heat resistance.
- silane crosslinkable polyethylene can be used more suitably.
- silane-crosslinkable linear low-density polyethylene density: 0.850 to 0.920 g / cm 3
- silane-crosslinkable linear low-density polyethylene can be particularly preferably used because of further improved transparency.
- the content of the various monomers that modify the modified polyolefin resin is not particularly limited, but is usually 0.5 mol% or more with respect to the total amount of monomers constituting the modified polyolefin resin, preferably Is 1 mol% or more, more preferably 2 mol% or more, and usually 40 mol% or less, preferably 30 mol% or less, more preferably 25 mol% or less. Within this range, the crystallinity is reduced by the copolymerization component, so that the transparency is improved and problems such as blocking of the raw material pellets are less likely to occur.
- the type and content of various monomers that modify the modified polyolefin polymer can be qualitatively and quantitatively analyzed by a well-known method, for example, a nuclear magnetic resonance (NMR) measuring device or other instrumental analyzer.
- NMR nuclear magnetic resonance
- the method for producing the modified polyolefin resin is not particularly limited, and a known olefin polymerization catalyst is used except for the ionomer resin, silane crosslinkable polyolefin, and maleic anhydride graft copolymer shown below.
- Polymerization method for example, slurry polymerization method, solution polymerization method, bulk polymerization method, gas phase polymerization method, etc. using multi-site catalyst typified by Ziegler-Natta type catalyst and single-site catalyst typified by metallocene catalyst, It can be obtained by a bulk polymerization method using a radical initiator.
- the ionomer resin contains at least a part of an unsaturated carboxylic acid component of a copolymer comprising ethylene, an unsaturated carboxylic acid, and other unsaturated compounds as optional components, at least one of a metal ion and an organic amine. It can be obtained by summing.
- the ionomer resin can also be obtained by saponifying at least a part of an unsaturated carboxylic acid ester component of a copolymer comprising ethylene, an unsaturated carboxylic acid ester, and other unsaturated compounds as optional components. .
- the silane crosslinkable polyolefin can be obtained by melt-mixing a polyolefin-based resin, a silane coupling agent described below, and a radical generator described below at a high temperature and graft polymerization.
- the maleic anhydride graft copolymer can be obtained by melt-mixing a polyolefin resin, maleic anhydride, and a radical generator described later at a high temperature and graft polymerization.
- E-MMA ethylene-methyl methacrylate copolymer
- ACRIFT ethylene-methyl methacrylate copolymer
- E-EAA ethylene-ethyl acrylate copolymer
- REXPEARL EEA product name manufactured by Nippon Polyethylene Co., Ltd.
- E-GMA ethylene-glycidyl methacrylate copolymer
- BONDAST product name manufactured by Sumitomo Chemical Co., Ltd.
- EVOH ethylene-vinyl alcohol copolymer
- Soarnol manufactured by Nippon Synthetic Chemical Co., Ltd., Kuraray Co., Ltd.
- the melt flow rate (MFR) of the polyolefin-based resin used for the (I) layer is not particularly limited, but usually MFR (JIS K7210, temperature: 190 ° C., load: 21.18 N) is 0.1. What is about 5 to 100 g / 10 min, preferably 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min is used.
- the MFR may be selected in consideration of molding processability when molding a sheet, adhesion when sealing a solar cell element (cell), a wraparound condition, and the like.
- the MFR is preferably relatively low, specifically about 0.5 to 5 g / 10 min from the handling property when the sheet is peeled off from the forming roll.
- the MFR is preferably 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min, from the viewpoint of reducing the extrusion load and increasing the extrusion rate.
- the MFR is preferably 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min. Good.
- the adhesive layer ((I) layer) it is preferable to use a layer made of a resin composition (Z) containing a polyethylene resin (X) and a silane-modified ethylene resin (Y). At this time, it is necessary for the resin composition (Z) that the heat of crystal melting measured at a heating rate of 10 ° C./min in the condition (a) differential scanning calorimetry satisfies 0 to 70 J / g.
- the polyethylene resin (X) used in the present invention is not particularly limited as long as the resin composition (Z) is of a kind that does not prevent the resin composition (Z) from satisfying the condition (a).
- the polyethylene resin (X) used in the present invention is not particularly limited as long as the resin composition (Z) is of a kind that does not prevent the resin composition (Z) from satisfying the condition (a).
- the low-density polyethylene resin suitably used in the present invention usually includes a random copolymer of ethylene and an ⁇ -olefin having 3 to 20 carbon atoms.
- Examples of the ⁇ -olefin copolymerized with ethylene include propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene and 3-methyl-butene. -1,4-methyl-pentene-1 and the like.
- propylene, 1-butene, 1-hexene, and 1-octene are preferably used as the ⁇ -olefin copolymerized with ethylene from the viewpoints of industrial availability, various characteristics, and economical efficiency. It is done.
- the ⁇ -olefin copolymerized with ethylene may be used alone or in combination of two or more.
- the content of ⁇ -olefin copolymerized with ethylene is usually 2 mol% or more, preferably 40 mol% or less, based on all monomer units in the ethylene- ⁇ -olefin random copolymer. More preferably, it is 3 to 30 mol%, and further preferably 5 to 25 mol%. If the content of ⁇ -olefin is within the above range, crystallinity is reduced by the copolymerization component, so that the transparency is improved and problems such as blocking of raw material pellets are not likely to occur.
- the type and content of the ⁇ -olefin copolymerized with ethylene can be qualitatively and quantitatively analyzed by a known method, for example, a nuclear magnetic resonance (NMR) measuring device or other instrumental analyzer.
- NMR nuclear magnetic resonance
- the ethylene- ⁇ -olefin random copolymer may contain monomer units based on monomers other than ⁇ -olefin.
- the monomer include cyclic olefins, vinyl aromatic compounds (such as styrene), polyene compounds, and the like.
- the content of the monomer unit is 20 mol% or less, more preferably 15 mol% or less when the total monomer units in the ethylene- ⁇ -olefin random copolymer is 100 mol%. preferable.
- the steric structure, branching, branching degree distribution and molecular weight distribution of the ethylene- ⁇ -olefin random copolymer are not particularly limited.
- a copolymer having a long chain branch generally has mechanical properties.
- melt tension (melt tension) at the time of molding the sheet is increased and the calendar moldability is improved.
- a copolymer having a narrow molecular weight distribution polymerized using a single site catalyst has advantages such as a low molecular weight component and a relatively low blocking of raw material pellets.
- the melt flow rate (MFR) of the polyethylene-based resin (X) used in the present invention is not particularly limited, but usually MFR (JIS K7210, temperature: 190 ° C., load: 21.18 N) is 0.1. What is about 1 to 100 g / 10 min, preferably 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min is used.
- the MFR may be selected in consideration of molding processability when molding a sheet, adhesion when sealing a solar cell element (cell), a wraparound condition, and the like.
- the MFR is preferably relatively low, specifically about 0.5 to 5 g / 10 min from the handling property when the sheet is peeled off from the forming roll.
- the MFR is preferably 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min, from the viewpoint of reducing the extrusion load and increasing the extrusion rate.
- the MFR is preferably 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min. Good.
- the polyethylene resin (X) used in the present invention has a heat of crystal melting measured at a heating rate of 10 ° C./min in the differential scanning calorimetry in order to satisfy the condition (a) for the resin composition (Z). It is preferably 0 to 70 J / g. More preferably, it is 5 to 70 J / g, and still more preferably 10 to 65 J / g. If it is in this range, since the softness
- the heat of crystal melting can be measured at a heating rate of 10 ° C./min according to JIS K7122 using a differential scanning calorimeter.
- the average refractive index of the polyethylene resin (X) used in the present invention is usually in the range of 1.4800 or more and 1.5000 or less, particularly preferably 1.4810 or more and 1.4990 or less. It is preferably 4820 or more and 1.4980 or less. By setting the composition ratio of the polyethylene-based resin (X) within the above range, the average refractive index can be set to such a suitable range.
- the average refractive index is sodium D at a temperature of 23 ° C. in accordance with JIS K7142.
- the line (589 nm) can be measured as a light source.
- the polyethylene resin (X) may be a single type or a combination of two or more types.
- the production method of the polyethylene resin (X) used in the present invention is not particularly limited, and a known polymerization method using a known olefin polymerization catalyst can be employed.
- a known polymerization method using a known olefin polymerization catalyst can be employed.
- the low-density ethylene- ⁇ -olefin random copolymer that is preferably used is a relatively soft resin, so that it is easy to granulate after polymerization, prevent blocking of raw material pellets, etc. From this viewpoint, a polymerization method using a single-site catalyst that can polymerize a raw material having a low molecular weight component and a narrow molecular weight distribution is suitably used.
- polyethylene resin (X) used in the present invention examples include trade names “Engage”, “Affinity”, “Infuse”, and Mitsui Chemicals, manufactured by Dow Chemical Co., Ltd.
- examples thereof include trade names “TAFMER A”, “TAFMER P” manufactured by Nippon Kayaku Co., Ltd., and “kernel” manufactured by Nippon Polyethylene Co., Ltd.
- silane-modified ethylene resin (Y) used in the present invention is usually obtained by melt-polymerizing a polyethylene resin, a vinylsilane compound described later, and a radical generator described later at a high temperature (about 160 ° C. to 220 ° C.) and graft polymerization. Can be obtained.
- the polyethylene resin used to obtain the (Y) has the same composition, density, MFR, heat of crystal fusion, and average refractive index as those exemplified as the polyethylene resin suitable for the (X). It is preferable to use it.
- the polyethylene resin is preferably a density of 0.850 ⁇ 0.920g / cm 3, the density is more preferably a linear low density polyethylene 0.860 ⁇ 0.880g / cm 3.
- melt flow rate is not particularly limited, but usually MFR (JIS K7210, temperature: 190 ° C., load: 21.18 N) is about 0.5 to 100 g / 10 min, preferably What is 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min is used.
- the heat of crystal fusion measured at a heating rate of 10 ° C./min in differential scanning calorimetry is preferably 0 to 70 J / g. More preferably, it is 5 to 70 J / g, and still more preferably 10 to 65 J / g.
- the average refractive index is usually in the range of 1.4800 or more and 1.5000 or less, preferably 1.4810 or more and 1.4990 or less, particularly 1.4820 or more and 1.4980 or less. preferable.
- the content of ⁇ -olefin copolymerized with ethylene is defined as all monomers in the ethylene- ⁇ -olefin random copolymer. It is usually 2 mol% or more, preferably 40 mol% or less, more preferably 3 to 30 mol%, still more preferably 5 to 25 mol%, based on the unit. If the content of ⁇ -olefin is within the above range, crystallinity is reduced by the copolymerization component, so that the transparency is improved and problems such as blocking of raw material pellets are not likely to occur.
- the vinyl silane compound is not particularly limited as long as it is graft-polymerized with the polyethylene resin.
- vinyltrimethoxysilane is preferably used from the viewpoints of reactivity, adhesiveness and color tone.
- the addition amount of the vinylsilane compound is not particularly limited, but is usually about 0.01 to 10.0 parts by mass with respect to 100 parts by mass of the polyethylene resin used, and 0.3 to 8. It is more preferable to add 0 part by mass, and it is even more preferable to add 1.0 to 5.0 parts by mass.
- the radical generator is not particularly limited.
- hydroperoxides such as diisopropylbenzene hydroperoxide, 2,5-dimethyl-2,5-di (hydroperoxy) hexane; -Butyl peroxide, t-butyl cumyl peroxide, dicumyl peroxide, 2,5-dimethyl-2,5-di (t-butylperoxy) hexane, 2,5-dimethyl-2,5-di (t -Peroxy) dialkyl peroxides such as hexyne-3; bis-3,5,5-trimethylhexanoyl peroxide, octanoyl peroxide, benzoyl peroxide, o-methylbenzoyl peroxide, 2,4-dichlorobenzoylper Diacyl peroxides such as oxides; t-butylperoxya Tate, t-butylperoxy-2-ethy
- the addition amount of the radical generator is not particularly limited, but is usually about 0.01 to 5.0 parts by mass with respect to 100 parts by mass of the polyethylene resin used, and 0.02 to 1 More preferably, 0.0 part by mass is added, and 0.03 to 0.5 part by mass is more preferably added. Furthermore, the residual amount of the radical generator is preferably 0.001% by mass or less in each resin layer constituting the multilayer body for solar cell of the present invention, and the gel fraction is preferably 30% or less.
- silanol condensation catalyst for promoting a condensation reaction between silanols is not substantially contained.
- the silanol condensation catalyst include dibutyltin diacetate, dibutyltin dilaurate, dibutyltin dioctate, and dioctyltin dilaurate.
- being substantially not contained means 0.05 parts by mass or less, preferably 0.03 parts by mass or less with respect to 100 parts by mass of the resin.
- a silanol condensation catalyst is not substantially contained is that, in the present invention, polar groups such as silanol groups grafted on the polyethylene resin to be used without actively proceeding with the silanol crosslinking reaction.
- polar groups such as silanol groups grafted on the polyethylene resin to be used without actively proceeding with the silanol crosslinking reaction.
- the silane-modified ethylene resin (Y) used in the present invention is usually obtained by melt-mixing the polyethylene resin with a vinylsilane compound and a radical generator at a high temperature (about 160 ° C. to 220 ° C.) and graft polymerization. It is obtained. Therefore, the density of the silane-modified ethylene resin (Y) used in the present invention and the preferred range of MFR are the same as the density of the polyethylene resin and the preferred range of MFR.
- the silane-modified ethylene resin (Y) used in the present invention has a crystal melting measured at a heating rate of 10 ° C./min in differential scanning calorimetry in order to satisfy the condition (a) for the resin composition (Z).
- the amount of heat is preferably 0 to 70 J / g. More preferably, it is 5 to 70 J / g, and still more preferably 10 to 65 J / g. If it is in this range, since the softness
- the average refractive index of the silane-modified ethylene-based resin (Y) used in the present invention is usually in the range of 1.4800 or more and 1.5000 or less, preferably 1.4810 or more and 1.4990 or less. It is preferable that it is 1.4820 or more and 1.4980 or less.
- the average refractive index of the silane-modified ethylene-based resin (Y) is set to such a suitable range. it can.
- the silane-modified ethylene-based resin (Y) may be a single type or a combination of two or more types.
- the solar cell encapsulant of the present invention is The haze is small and particularly excellent in transparency, which is preferable.
- the absolute value of the difference in average refractive index is more preferably 0.0080 or less, and particularly preferably 0.0060 or less.
- silane-modified ethylene resin (Y) used in the present invention trade name “LINKLON” manufactured by Mitsubishi Chemical Corporation can be exemplified.
- the resin composition which comprises a layer has a polyolefin resin as a main component, various physical properties (a softness
- a resin mainly composed of the modified polyolefin resin but it is preferable to use a polyolefin resin other than the modified polyolefin resin (hereinafter referred to as “unmodified polyolefin resin”) in combination. More preferably, the combination is used as a main component.
- the unmodified polyolefin resin is not particularly limited, but it is preferable from the viewpoint of transparency that the main component is an olefin monomer constituting the modified polyolefin resin. If the unmodified polyolefin-based resin is an ethylene- ⁇ -olefin random copolymer (A) or an ethylene- ⁇ -olefin block copolymer (B) used in the layer (II) described later, (I) From the viewpoint of interlayer adhesion between the layer and the (II) layer, flexibility, heat resistance, and the like.
- the modified polyolefin resin and the unmodified polyolefin resin are used in combination in the resin composition constituting the layer, the content ratio is not particularly limited, but from the viewpoint of developing good adhesiveness, the modified polyolefin
- the range of resin / unmodified polyolefin resin is preferably in the range of 3/97 to 100/0, and more preferably in the range of 5/95 to 100/0.
- the modified polyolefin resin and the unmodified polyolefin resin to be used are the same type of resin, for example, a modified resin.
- a polyethylene resin and an unmodified polyethylene resin are preferred.
- the resin composition (Z) constituting the layer contains the polyethylene resin (X) and the silane-modified ethylene resin (Y), and the polyethylene resin (X) and the silane-modified resin. It is preferable that a resin composition composed of the ethylene-based resin (Y) is a main component.
- the mixing mass ratio of the polyethylene resin (X) and the silane-modified ethylene resin (Y) in the resin composition (Z) is not particularly limited, but polyethylene resin (X) / silane modification.
- the mass ratio of the ethylene-based resin (Y) is 1 to 99/99 to 1, preferably 30 to 98/70 to 2, and more preferably 60 to 97/40 to 3.
- the content of the silane-modified ethylene resin (Y) in the (I) layer that is, the concentration of the silane-modified group is easy to adjust, and the adhesive layer that is the main role of the (I) layer While maintaining the function, it is preferable because various properties such as flexibility, transparency, sealing property, and heat resistance as the surface layer and the sealing layer can be adjusted relatively easily.
- each of the resin compositions (Z) may be a combination of more than one species.
- the polyethylene-based resin (X) and the silane can be used as long as the purpose of achieving the balance can be achieved without impairing the excellent transparency, adhesiveness, and heat resistance of the solar cell sealing material of the present invention.
- the modified ethylene resin (Y) may be composed of two or more types having different properties such as composition, density, MFR, heat of crystal fusion, and average refractive index, and those within the preferred ranges of the composition and properties. , Any of which is out of range can be used.
- the content ratio is the resin composition (Z).
- the lower limit is preferably 1% by mass, and more preferably 2% by mass, when the mass of all resins constituting the resin is 100% by mass.
- the upper limit is preferably 10% by mass, and more preferably 5% by mass. It is preferable to set the content ratio within the above range and to set the lower limit value so that the transparency, adhesiveness, and heat resistance of the solar cell sealing material of the present invention can be balanced.
- the resin composition (Z) needs to satisfy 0 to 70 J / g of crystal melting heat amount measured at a heating rate of 10 ° C./min in the condition (a) differential scanning calorimetry, Is from 5 to 70 J / g, more preferably from 10 to 65 J / g. Within such a range, the flexibility and transparency (haze, total light transmittance) and the like of the solar cell encapsulant of the present invention are secured, which is preferable. Further, if the heat of crystal fusion is 5 J / g or more, it is preferable because problems such as blocking of raw material pellets hardly occur.
- the polyolefin-based resin is used for the purpose of further improving various physical properties (flexibility, heat resistance, transparency, adhesiveness, etc.), molding processability, economy and the like without departing from the gist of the present invention.
- Other resins other than the resin can be mixed.
- other resins for example, other polyolefin resins and various elastomers (olefins, styrenes, etc.), polar groups such as carboxyl groups, amino groups, imide groups, hydroxyl groups, epoxy groups, oxazoline groups, thiol groups, etc. Examples thereof include resins modified with groups and tackifying resins.
- the tackifying resin examples include petroleum resins, terpene resins, coumarone-indene resins, rosin resins, and hydrogenated derivatives thereof.
- the petroleum resin includes cyclopentadiene or an alicyclic petroleum resin derived from a dimer thereof and an aromatic petroleum resin derived from a C9 component
- the terpene resin includes a terpene resin derived from ⁇ -pinene and a terpene resin.
- the phenol resin include rosin resins such as gum rosin and wood rosin, and esterified rosin resins modified with glycerin, pentaerythritol, and the like.
- the tackifying resin can be obtained with various softening temperatures mainly depending on the molecular weight, but the compatibility, bleed over time and color tone when mixed with the polyolefin resin and modified polyolefin resin component described above.
- the softening temperature is preferably 100 or higher, more preferably 120 ° C. or higher, and preferably 150 ° C. or lower, more preferably 140 ° C. or lower. preferable.
- the method of mixing these resins when forming the (I) layer using the polyethylene resin (X), the silane-modified ethylene resin (Y), and the other resin is not particularly limited. However, after dry blending together with the resin, it may be supplied to the hopper, or may be supplied after all materials are melted and mixed to produce pellets. In the present invention, since the vinylsilane compound and the radical generator added when obtaining the silane-modified ethylene resin (Y) may remain without reacting as described above, the polyethylene resin (X ) And the silane-modified ethylene resin (Y) are preferably removed by a vacuum vent.
- the thickness of the (I) layer constituting the solar cell encapsulating material of the present invention is not particularly limited, but is usually 0.005 mm or more, preferably from the viewpoint of sealing property and unevenness of the cell, transparency, etc. It may be 0.01 mm or more, more preferably 0.02 mm or more, and about 0.9 mm or less, preferably 0.6 mm or less, more preferably 0.5 mm or less. In addition, from the viewpoint of sealing properties, adhesiveness, and economy for filling gaps between cells and wirings, it is preferably about 0.01 to 0.5 mm, and preferably 0.02 to 0.4 mm. Is more preferable, and 0.04 to 0.3 mm is particularly preferable.
- the layer (II) satisfies the following condition (a) and the ethylene- ⁇ -olefin random copolymer (A) and the following condition (b): And a layer made of the resin composition (C) containing the ethylene- ⁇ -olefin block copolymer (B).
- the calorie of crystal melting measured at a heating rate of 10 ° C./min in differential scanning calorimetry is 0 to 70 J / g.
- the crystal melting peak temperature measured at a heating rate of 10 ° C./min in differential scanning calorimetry is 100 ° C. or more, and the crystal melting heat amount is 5 to 70 J / g.
- the ethylene- ⁇ -olefin random copolymer (A) used in the present invention is not particularly limited as long as the above condition (a) is satisfied. Usually, ethylene and ⁇ -olefin having 3 to 20 carbon atoms are used. A random copolymer with olefin is preferably used. Examples of the ⁇ -olefin copolymerized with ethylene include propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene and 3-methyl-butene. -1,4-methyl-pentene-1, etc.
- propylene, 1-butene, 1-hexene, and 1-octene are preferably used as the ⁇ -olefin copolymerized with ethylene from the viewpoints of industrial availability, various characteristics, and economical efficiency. It is done.
- the ⁇ -olefin copolymerized with ethylene may be used alone or in combination of two or more.
- the content of the ⁇ -olefin copolymerized with ethylene is not particularly limited as long as the above-mentioned condition (a) is satisfied, but the ethylene- ⁇ -olefin random copolymer (A) in the ethylene- ⁇ -olefin random copolymer (A) is not limited. It is usually 2 mol% or more, preferably 40 mol% or less, more preferably 3 to 30 mol%, still more preferably 5 to 25 mol%, based on all monomer units. Within this range, the crystallinity is reduced by the copolymerization component, so that the transparency is improved and problems such as blocking of the raw material pellets are less likely to occur.
- the type and content of the ⁇ -olefin copolymerized with ethylene can be qualitatively and quantitatively analyzed by a known method, for example, a nuclear magnetic resonance (NMR) measuring device or other instrumental analyzer.
- NMR nuclear magnetic resonance
- the ethylene- ⁇ -olefin random copolymer (A) may contain monomer units based on monomers other than ⁇ -olefin as long as the above-mentioned condition (a) is satisfied.
- the monomer include cyclic olefins, vinyl aromatic compounds (such as styrene), polyene compounds, and the like.
- the content of the monomer unit is 20 mol% or less and 15 mol% or less, assuming that all monomer units in the ethylene- ⁇ -olefin random copolymer (A) are 100 mol%. It is preferable.
- the steric structure, branching, branching degree distribution and molecular weight distribution of the ethylene- ⁇ -olefin random copolymer (A) are not particularly limited as long as the above-described condition (a) is satisfied.
- a copolymer having a long chain branch generally has good mechanical properties, and has an advantage that the melt tension (melt tension) at the time of molding a sheet is increased and the calendar moldability is improved.
- a copolymer having a narrow molecular weight distribution polymerized using a single site catalyst has advantages such as a low molecular weight component and a relatively low blocking of raw material pellets.
- the melt flow rate (MFR) of the ethylene- ⁇ -olefin random copolymer (A) used in the present invention is not particularly limited, but is usually MFR (JIS K7210, temperature: 190 ° C., load: 21). .18N) is about 0.5 to 100 g / 10 min, more preferably 2 to 50 g / 10 min, still more preferably 3 to 30 g / 10 min.
- the MFR may be selected in consideration of molding processability when molding a sheet, adhesion when sealing a solar cell element (cell), a wraparound condition, and the like.
- the MFR is preferably relatively low, specifically about 0.5 to 5 g / 10 min from the handling property when the sheet is peeled off from the forming roll.
- the MFR is preferably 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min, from the viewpoint of reducing the extrusion load and increasing the extrusion rate.
- the MFR is preferably 2 to 50 g / 10 min, more preferably 3 to 30 g / 10 min. Good.
- the production method of the ethylene- ⁇ -olefin random copolymer (A) used in the present invention is not particularly limited, and a known polymerization method using a known olefin polymerization catalyst can be employed.
- a known polymerization method using a known olefin polymerization catalyst can be employed.
- the ethylene- ⁇ -olefin random copolymer (A) is a relatively soft resin, it has a low molecular weight from the viewpoint of easy granulation after polymerization and prevention of blocking of raw material pellets.
- a polymerization method using a single site catalyst capable of polymerizing a raw material with few components and a narrow molecular weight distribution is suitable.
- the heat of crystal melting measured at a heating rate of 10 ° C./min in the condition (a) differential scanning calorimetry satisfies 0 to 70 J / g. Preferably 5 to 70 J / g, more preferably 10 to 65 J / g. If it is in this range, since the softness
- general-purpose high-density polyethylene is about 170 to 220 J / g
- low-density polyethylene resin LDPE
- linear low-density polyethylene LLDPE
- the heat of crystal melting can be measured at a heating rate of 10 ° C./min according to JIS K7122 using a differential scanning calorimeter.
- the crystal melting peak temperature of the ethylene- ⁇ -olefin random copolymer (A) used in the present invention is not particularly limited, but is usually less than 100 ° C. and 30 to 90 ° C. There are many.
- general-purpose high-density polyethylene (HDPE) is about 130 to 145 ° C.
- low-density polyethylene resin (LDPE) and linear low-density polyethylene (LLDPE) are 100 to 125. It is about °C.
- the crystal melting peak temperature measured at a heating rate of 10 ° C./min in differential scanning calorimetry is 100 ° C. or higher, and It is difficult to achieve a heat of crystal melting of 5 to 70 J / g.
- the crystal melting peak temperature can be measured at a heating rate of 10 ° C./min according to JIS K7121 using a differential scanning calorimeter.
- ethylene- ⁇ -olefin random copolymer (A) used in the present invention include trade names “Engage”, “Affinity”, Mitsui Chemicals (manufactured by Dow Chemical Co., Ltd.).
- examples include trade name “TAFMER ⁇ ⁇ A”, “TAFMER P”, and trade name “KERNEL” manufactured by Nippon Polyethylene Co., Ltd.
- the ethylene- ⁇ -olefin block copolymer (B) used in the present invention is not particularly limited as long as the above-mentioned condition (b) is satisfied.
- ethylene and ⁇ having 3 to 20 carbon atoms are used.
- -Block copolymers with olefins are preferably used.
- Examples of the ⁇ -olefin copolymerized with ethylene include propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene and 3-methyl-butene. -1,4-methyl-pentene-1, etc.
- propylene, 1-butene, 1-hexene, and 1-octene are preferably used as the ⁇ -olefin copolymerized with ethylene from the viewpoints of industrial availability, various characteristics, and economical efficiency. It is done.
- the ⁇ -olefin copolymerized with ethylene may be used alone or in combination of two or more.
- the ethylene- ⁇ -olefin block copolymer (B) may contain monomer units based on monomers other than ⁇ -olefin as long as the above-mentioned condition (b) is satisfied.
- the monomer include cyclic olefins, vinyl aromatic compounds (such as styrene), polyene compounds, and the like.
- the content of the monomer units is 20 mol% or less and 15 mol% or less, assuming that all monomer units in the ethylene- ⁇ -olefin block copolymer (B) are 100 mol%. It is preferable.
- the block structure of the ethylene- ⁇ -olefin block copolymer (B) used in the present invention is not particularly limited as long as the above-mentioned condition (b) is satisfied, but flexibility, heat resistance, transparency 2 or more, preferably 3 or more segments or blocks having different comonomer contents, crystallinity, density, crystal melting peak temperature (melting point Tm), or glass transition temperature (Tg)
- a multi-block structure is preferable. Specific examples include a completely symmetric block, an asymmetric block, and a tapered block structure (a structure in which the ratio of the block structure gradually increases in the main chain).
- 2005/090425 (WO2005 / 090425), International Publication No. 2005/090426 (WO2005 / 090426), and International Publication No.2005. / 090427 pamphlet (WO2005 / 090427) or the like can be employed.
- the ethylene- ⁇ -olefin block copolymer having the multi-block structure will be described in detail below.
- the ethylene- ⁇ -olefin block copolymer having a multiblock structure can be suitably used in the present invention, and an ethylene-octene multiblock copolymer having 1-octene as a copolymerization component as an ⁇ -olefin is preferable.
- a multiblock copolymer having two or more highly crystalline hard segments each having a copolymerized crystal melting peak temperature of 110 to 145 ° C. is preferred.
- chain length and ratio of these soft segments and hard segments By controlling the chain length and ratio of these soft segments and hard segments, both flexibility and heat resistance can be achieved.
- trade name “Infuse” manufactured by Dow Chemical Co., Ltd. may be mentioned.
- the melt flow rate (MFR) of the ethylene- ⁇ -olefin block copolymer (B) used in the present invention is not particularly limited, but is usually MFR (JIS K7210, temperature: 190 ° C., load: 21). .18N) is about 0.5 to 100 g / 10 min, more preferably 1 to 50 g / 10 min, still more preferably 1 to 30 g / 10 min, and particularly preferably 1 to 10 g / 10 min.
- the MFR may be selected in consideration of molding processability when molding a sheet, adhesion when sealing a solar cell element (cell), a wraparound condition, and the like.
- the MFR is preferably relatively low, specifically about 0.5 to 5 g / 10 min from the handling property when the sheet is peeled off from the molding roll.
- an MFR of 1 to 30 g / 10 min is preferably used from the viewpoint of reducing the extrusion load and increasing the extrusion amount.
- an MFR of 3 to 50 g / 10 min is preferably used.
- the ethylene- ⁇ -olefin block copolymer (B) used in the present invention has a crystal melting peak temperature of 100 ° C. or higher measured at a heating rate of 10 ° C./min in the condition (b) differential scanning calorimetry, and Further, it is necessary that the heat of crystal fusion satisfies 5 to 70 J / g.
- the crystal melting peak temperature is 105 ° C. or higher, more preferably 110 ° C. or higher, and the upper limit is usually 145 ° C.
- the heat of crystal melting is preferably 10 to 60 J / g, more preferably 15 to 55 J / g.
- the method for measuring the crystal melting peak temperature and the crystal melting heat amount is as described above.
- a solar cell module is heated to about 85 to 90 ° C. due to heat generated during power generation or radiant heat of sunlight, but if the crystal melting peak temperature is 100 ° C. or higher, the heat resistance of the solar cell encapsulant of the present invention is increased.
- the upper limit temperature is 145 ° C., it is preferable because the sealing can be performed without increasing the temperature in the sealing step of the solar cell element.
- the solar cell encapsulant of the present invention is ensured in flexibility, transparency (total light transmittance), etc., and it is difficult for problems such as blocking of raw material pellets to occur. preferable.
- the layer (II) in the present invention comprises the resin composition (C) containing the above-mentioned ethylene- ⁇ -olefin random copolymer (A) and the ethylene- ⁇ -olefin block copolymer (B).
- the kind of ⁇ -olefin used in each of these copolymers (A) and copolymers (B) may be the same or different, but in the present invention, It is preferable that they are the same because the compatibility when mixed and the transparency of the solar cell sealing material are improved, that is, the photoelectric conversion efficiency of the solar cell is improved.
- the viewpoint of the ease of regeneration addition during the production of the solar cell encapsulant of the present invention the improvement of the economics such as the yield, and the maintenance of the transparency of the layer (II) when regeneration addition is performed.
- the type of ⁇ -olefin used in each of the polyethylene resin (X) and the silane-modified ethylene resin (Y) when the layer (I) is made of the resin composition (Z), and the layer (II) It is preferable that the ⁇ -olefins used in each of the copolymer (A) and the copolymer (B) are the same.
- the contents of the ethylene- ⁇ -olefin random copolymer (A) and the ethylene- ⁇ -olefin block copolymer (B) in the resin composition (C) are flexibility, heat resistance, transparency, etc.
- the resin composition (C) is 100 parts by mass from the viewpoint of having an excellent balance, it is preferably 50 to 99 parts by mass and 1 to 50 parts by mass, and more preferably 60 to 98 parts by mass, respectively. Part, 2 to 40 parts by weight, more preferably 70 to 97 parts by weight, and 3 to 30 parts by weight.
- the mixed (contained) mass ratio is within the above range because a solar cell encapsulant having an excellent balance of flexibility, heat resistance, transparency and the like can be easily obtained.
- the resin composition (C) constituting the layer has various physical properties (flexibility, heat resistance, transparency, adhesiveness, etc.), molding processability, economical efficiency, etc. within the scope of the present invention.
- a resin other than the ethylene- ⁇ -olefin random copolymer (A) and the ethylene- ⁇ -olefin block copolymer (B) described above examples include the same resins as the polyolefin-based resin and other resins used in the (I) layer.
- the resin composition (C) is 100 parts by mass, It is preferably 20 parts by mass or less, and more preferably 10 parts by mass or less.
- additives can be added to each of the (I) layer and the (II) layer as necessary.
- the additive include an antioxidant, an ultraviolet absorber, a weathering stabilizer, a light diffusing agent, a nucleating agent, a pigment (for example, a white pigment), a flame retardant, and a discoloration preventing agent.
- at least one additive selected from an antioxidant, an ultraviolet absorber, and a weathering stabilizer is added for the reason described later.
- a crosslinking agent and a crosslinking aid can be added to the resin composition (C).
- a crosslinking agent and / or a crosslinking aid is blended. be able to.
- antioxidant various commercial products can be applied, and various types such as monophenol type, bisphenol type, polymer type phenol type, sulfur type and phosphite type can be exemplified.
- monophenols include 2,6-di-tert-butyl-p-cresol, butylated hydroxyanisole, and 2,6-di-tert-butyl-4-ethylphenol.
- bisphenols examples include 2,2'-methylene-bis- (4-methyl-6-tert-butylphenol), 2,2'-methylene-bis- (4-ethyl-6-tert-butylphenol), 4,4 '-Thiobis- (3-methyl-6-tert-butylphenol), 4,4'-butylidene-bis- (3-methyl-6-tert-butylphenol), 3,9-bis [ ⁇ 1,1-dimethyl- 2- ⁇ - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionyloxy ⁇ ethyl ⁇ 2,4,9,10-tetraoxaspiro] 5,5-undecane.
- Examples of the high molecular phenolic group include 1,1,3-tris- (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, 1,3,5-trimethyl-2,4,6-tris (3 , 5-di-tert-butyl-4-bidoxybenzyl) benzene, tetrakis- ⁇ methylene-3- (3 ', 5'-di-tert-butyl-4'-hydroxyphenyl) propionate ⁇ methane, bis ⁇ (3,3′-bis-4′-hydroxy-3′-tert-butylphenyl) butyric acid ⁇ glycol ester, 1,3,5-tris (3 ′, 5′-di-tert-butyl-4 '-Hydroxybenzyl) -s-triazine-2,4,6- (1H, 3H, 5H) trione, triphenol (vitamin E) and the like.
- sulfur-based compounds include dilauryl thiodipropionate, dim
- phosphites include triphenyl phosphite, diphenylisodecyl phosphite, phenyl diisodecyl phosphite, 4,4′-butylidene-bis (3-methyl-6-tert-butylphenyl-di-tridecyl) phosphite, Crick neopentanetetrayl bis (octadecyl phosphite), tris (mono and / or di) phenyl phosphite, diisodecyl pentaerythritol diphosphite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Oxide, 10- (3,5-di-tert-butyl-4-hydroxybenzyl) -9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 10-decyloxy-9,10 pho
- phenol-based and phosphite-based antioxidants are preferably used in view of the effect of the antioxidant, thermal stability, economy and the like, and it is more preferable to use a combination of both.
- the addition amount of the antioxidant is usually about 0.1 to 1 part by mass, and 0.2 to 0 with respect to 100 parts by mass of the resin composition constituting each of the layers (I) and (II). It is preferable to add 5 parts by mass.
- UV absorber various commercially available products can be applied, and various types such as benzophenone-based, benzotriazole-based, triazine-based, and salicylic acid ester-based materials can be exemplified.
- benzophenone ultraviolet absorbers include 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-2′-carboxybenzophenone, 2-hydroxy-4-octoxybenzophenone, 2-hydroxy-4-n.
- benzotriazole ultraviolet absorber examples include hydroxyphenyl-substituted benzotriazole compounds such as 2- (2-hydroxy-5-methylphenyl) benzotriazole and 2- (2-hydroxy-5-tert-butylphenyl).
- Benzotriazole 2- (2-hydroxy-3,5-dimethylphenyl) benzotriazole, 2- (2-methyl-4-hydroxyphenyl) benzotriazole, 2- (2-hydroxy-3-methyl-5-t- Butylphenyl) benzotriazole, 2- (2-hydroxy-3,5-di-t-amylphenyl) benzotriazole, 2- (2-hydroxy-3,5-di-t-butylphenyl) benzotriazole, etc. be able to.
- triazine ultraviolet absorbers examples include 2- [4,6-bis (2,4-dimethylphenyl) -1,3,5-triazin-2-yl] -5- (octyloxy) phenol, 2- ( Examples include 4,6-diphenyl-1,3,5-triazin-2-yl) -5- (hexyloxy) phenol.
- salicylic acid esters include phenyl salicylate and p-octylphenyl salicylate.
- the addition amount of the ultraviolet absorber is usually 0.01 parts by mass or more, preferably 0.05 parts by mass or more with respect to 100 parts by mass of the resin composition constituting each of the (I) layer and the (II) layer. And it is preferable to add in 2.0 mass parts or less, Preferably it is 0.5 mass part or less.
- Hindered amine light stabilizers are preferably used as the weather stabilizer for imparting weather resistance in addition to the above ultraviolet absorbers.
- a hindered amine light stabilizer does not absorb ultraviolet rays like an ultraviolet absorber, but exhibits a remarkable synergistic effect when used together with an ultraviolet absorber.
- hindered amines there are some that function as light stabilizers, but they are often colored and are not preferred for the (I) layer in the present invention.
- hindered amine light stabilizers include dimethyl-1- (2-hydroxyethyl) succinate-4-hydroxy-2,2,6,6-tetramethylpiperidine polycondensate, poly [ ⁇ 6- (1,1 , 3,3-tetramethylbutyl) amino-1,3,5-triazine-2,4-diyl ⁇ ⁇ (2,2,6,6-tetramethyl-4-piperidyl) imino ⁇ hexamethylene ⁇ 2, 2,6,6-tetramethyl-4-piperidyl ⁇ imino ⁇ ], N, N′-bis (3-aminopropyl) ethylenediamine-2,4-bis [N-butyl-N- (1,2,2, 6,6-pentamethyl-4-piperidyl) amino] -6-chloro-1,3,5-triazine condensate, bis (2,2,6,6-tetramethyl-4-piperidyl) sebacate, 2- (3 , 5-Di-tert-4 Hydroxybenzyl) -2-
- the amount of the hindered amine light stabilizer added is usually 0.01 parts by mass or more, preferably 0.05 parts by mass with respect to 100 parts by mass of the resin composition constituting each of the layers (I) and (II). It is suitable to add in the range of 0.5 parts by mass or less, preferably 0.3 parts by mass or less.
- antioxidants can be used alone or in combination of two or more, and ultraviolet absorbers and weathering stabilizers can also be used in combination. These generally tend to cause yellowing as the addition amount increases, so it is preferable to add only the minimum necessary amount.
- the thickness of the (II) layer constituting the solar cell encapsulant of the present invention is not particularly limited, but cushioning properties against impacts on the solar cell module, sealing properties against the uneven surface of the cells, insulating properties, From the viewpoint of transparency and the like, it is usually 0.02 mm or more, preferably 0.04 mm or more, more preferably 0.1 mm or more, further preferably 0.15 mm or more, and about 1 mm or less, preferably 0.8 mm or less. More preferably, it may be 0.6 mm or less, more preferably 0.5 mm or less.
- the solar cell encapsulant of the present invention needs to have at least the (I) layer and the (II) layer.
- the layer structure is not particularly limited as long as it has at least one (I) layer and (II) layer.
- the structure has (I) layer in at least one of the outermost layers. It is more preferable to have.
- the method for forming a solar cell encapsulant in the present invention has a known method, for example, a single-screw extruder, a multi-screw extruder, a Banbury mixer, a kneader or other melt mixing equipment, and an extrusion casting method using a T die or Although a calendar method etc. can be employ
- the coextrusion method using a some extruder is used suitably from surfaces, such as handling property and productivity.
- the molding temperature in the co-extrusion method using a T die is appropriately adjusted depending on the flow characteristics and film-forming properties of the resin composition to be used, but is generally 80 ° C or higher, preferably 100 ° C or higher, more preferably 120 ° C or higher, More preferably 140 ° C. or higher, and 300 ° C. or lower, preferably 250 ° C. or lower, more preferably 200 ° C. or lower, more preferably 180 ° C. or lower.
- a radical generator or a silane coupling agent is added It is preferable to lower the molding temperature in order to suppress an increase in the resin pressure and a fish eye associated with the crosslinking reaction.
- additives such as radical generators, silane coupling agents, antioxidants, ultraviolet absorbers, weathering stabilizers, light diffusing agents, nucleating agents, pigments (for example, white pigments), flame retardants, anti-discoloring agents, After dry blending with the resin, it may be supplied to the hopper, or it may be supplied after melt-mixing all the materials in advance to produce pellets, or a master batch in which only the additive is concentrated in the resin in advance. It may be produced and supplied.
- the sheet On the surface of the solar cell encapsulant of the present invention obtained in the form of a sheet, if necessary, the sheet can be used as a scroll to prevent blocking between sheets and to handle solar cells in the process of sealing and air Embossing and various unevenness (cone, pyramid shape, hemispherical shape, etc.) processing may be performed for the purpose of improving ease of punching.
- the solar cell sealing material of this invention can give surface treatments, such as a corona treatment and a plasma treatment, to the at least one surface from a viewpoint of improving adhesiveness.
- another base film such as an expanded polyester film (OPET) or an expanded polypropylene film (OPP)
- OPT expanded polypropylene film
- extrusion laminate when a sheet is formed, another base film (such as an expanded polyester film (OPET) or an expanded polypropylene film (OPP)) and an extrusion laminate are used for the purpose of improving the handleability when forming the sheet.
- the layers may be laminated by a method such as sandrami.
- the flexibility of the solar cell encapsulant of the present invention may be appropriately adjusted in consideration of the shape, thickness, installation location, etc. of the applied solar cell.
- the vibration frequency in dynamic viscoelasticity measurement is 10 Hz
- the storage elastic modulus (E ′) at 20 ° C. is preferably 1 to 2000 MPa.
- the storage elastic modulus (E ′) is preferably lower from the viewpoint of protection of the solar cell element, but it is 3 to 1000 MPa in consideration of handling properties in the case of a sheet shape, prevention of blocking between sheet surfaces, and the like. More preferably, it is 5 to 500 MPa, more preferably 10 to 100 MPa.
- the storage elastic modulus (E ′) is obtained by measuring at a predetermined temperature at a vibration frequency of 10 Hz using a viscoelasticity measuring device and obtaining a value at a temperature of 20 ° C.
- the total light transmittance of the solar cell encapsulant of the present invention is not so great when applied to a type of solar cell to be applied, for example, an amorphous thin film silicon type or a portion that does not block sunlight reaching the solar electronic element. Although it may not be regarded as important, it is usually preferably 85% or more, more preferably 87% or more, taking into consideration the photoelectric conversion efficiency of the solar cell and handling properties when various members are superimposed, 90% % Or more is more preferable.
- the total light transmittance and haze can be obtained by measuring using a haze meter according to JIS K7361.
- the heat resistance of the solar cell encapsulant of the present invention is as follows.
- (I) Various characteristics of the resin composition constituting the layer (crystal melting peak temperature, crystal melting heat amount, MFR, molecular weight, etc.),
- the crystal melting peak temperature of the ethylene- ⁇ -olefin block copolymer (B) is strongly influenced by the heat of crystal melting, MFR, molecular weight, and the like.
- a solar cell module is heated to about 85 to 90 ° C. due to heat generated during power generation or radiant heat of sunlight, but if the crystal melting peak temperature is 100 ° C. or higher, the heat resistance of the solar cell encapsulant of the present invention is increased. It is preferable because the property can be secured.
- a sheet-like sealing material is laminated between white glass and an aluminum plate, and a sample obtained by laminating and pressing at a predetermined temperature using a vacuum press machine is prepared. It can be installed at a predetermined angle in the tank and can be evaluated by observing the state after a predetermined time.
- the flexibility, heat resistance and transparency of the solar cell encapsulant of the present invention tend to be contradictory. Specifically, when the crystallinity of the resin composition (C) used for improving flexibility in the (II) layer is excessively lowered, the heat resistance is lowered and becomes insufficient. On the other hand, when the crystallinity of the resin composition (C) used for improving the heat resistance in the (II) layer is excessively improved, the transparency is lowered and becomes insufficient.
- these balances are used as an index of flexibility, a storage elastic modulus (E ′) at a vibration frequency of 10 Hz and a temperature of 20 ° C. in dynamic viscoelasticity measurement, and an ethylene- ⁇ -olefin block copolymer as an index of heat resistance.
- the three indices are storage elastic modulus (E ′) Is preferably 1 to 2000 MPa, the crystal melting peak temperature is 100 ° C. or more, and the total light transmittance is 85% or more, the storage elastic modulus (E ′) is 5 to 500 MPa, and the crystal melting peak temperature is 105 to 145 ° C.
- the total light transmittance is more preferably 85% or more, the storage elastic modulus (E ′) is 10 to 100 MPa, the crystal melting peak temperature is 110 to 145 ° C., the total light transmittance is The excess rate is particularly preferably 90% or more.
- the solar cell encapsulant of the present invention is excellent in adhesiveness and long-term stability of adhesive force.
- the method of adding an adhesion force by adding a silane coupling agent used in the conventional technology causes the adhesion force to decrease as the silane coupling agent bleeds out over time and reacts with moisture.
- the sealing material of the present invention exhibits an excellent adhesive force without using a silane coupling agent and has at least a layer (I) that is free from the concern of bleeding out of the additive. It is a sealing material excellent in both long-term stability of force.
- a white plate glass having a thickness of 2 mm, a length of 150 mm, and a width of 25 mm
- a 0.16 mm-thick fluorine-based back sheet (trade name: AKASOL, manufactured by KREMPEL) and a sheet-form sealing material having a thickness of 0.45 mm and a PET film having a thickness of 0.012 mm, a length of 50 mm, and a width of 30 mm
- the adhesive strength when the above-mentioned adhesiveness is carried out after leaving the film of the sealing material of the present invention at 25 ° C. and 50% RH for 4 months is preferable.
- the thickness ratio of the (I) layer and the (II) layer in the solar cell encapsulant of the present invention is not particularly limited, but from the viewpoint of adhesiveness and transparency, (I) / (II) is 50 / The range is preferably 50 to 10/90, and more preferably 40/60 to 10/90.
- the total thickness of the solar cell encapsulant of the present invention is not particularly limited, it is usually from the viewpoints of cushioning against impacts on the solar cell module, sealing against uneven surfaces of cells, insulation, etc. 0.02 mm or more, preferably 0.04 mm or more, more preferably 0.1 mm or more, more preferably 0.15 mm or more, further preferably 0.2 mm or more, and about 1 mm or less, preferably 0.8 mm or less. More preferably, it is 0.6 mm or less, and further preferably 0.5 mm or less.
- a solar cell module can be manufactured by using the solar cell encapsulant of the present invention and fixing the solar cell element with glass or a front sheet and a back sheet as upper and lower protective materials.
- a solar cell module various types can be exemplified, and preferably, the solar cell sealing material, the upper protective material, the solar cell element, and the lower protective material of the present invention are used. Specifically, the solar cell module produced by the above method is mentioned.
- the upper protective material / the sealing material of the present invention (sealing resin layer) / the solar cell element / the sealing material of the present invention (sealing resin layer) / A structure in which the sealing material of the present invention is sandwiched from both sides of the solar cell element as in the lower protective material (see FIG. 1), and the book on the solar cell element formed on the inner peripheral surface of the lower protective material Sputtering of an amorphous solar cell element on a solar cell element formed on the inner peripheral surface of the upper protective material, for example, a fluororesin-based transparent protective material
- a sealing material of the present invention Mamoruzai and the like as constituted as to form.
- the solar cell sealing material of the present invention when the sealing material is used in two or more parts, the solar cell sealing material of the present invention may be used for all parts. Or the solar cell sealing material of this invention may be used for only one site. Moreover, when a sealing material is used for two or more parts, the resin composition which comprises the solar cell sealing material of this invention used for each site
- the solar cell element is arranged and wired between the sealing resin layers.
- single crystal silicon type, polycrystalline silicon type, amorphous silicon type, III-V and II-VI group compound semiconductor types such as gallium-arsenic, copper-indium-selenium, cadmium-tellurium, dye-sensitized type, organic A thin film type is mentioned.
- each member which comprises the solar cell module produced using the solar cell sealing material of this invention although it does not specifically limit,
- an upper protective material glass, an acrylic resin, a polycarbonate, polyester, for example Examples thereof include a plate material such as a fluorine-containing resin and a single layer or multilayer protective material for a film.
- the lower protective material is a single layer or multilayer sheet such as metal or various thermoplastic resin films, for example, metals such as tin, aluminum and stainless steel, inorganic materials such as glass, polyester, inorganic vapor deposition polyester, fluorine-containing resin And a single-layer or multilayer protective material such as polyolefin.
- the surface of these upper and lower protective materials can be subjected to known surface treatments such as primer treatment and corona treatment in order to improve the adhesion to the solar cell encapsulant of the present invention and other members.
- the transparent substrate 10 the sealing resin layer 12A using the solar cell sealing material of the present invention, the solar cell elements 14A and 14B, and the solar cell sealing material of the present invention in order from the sunlight receiving side.
- the sealing resin layer 12B and the back sheet 16 used are laminated, and a junction box 18 (a terminal box for connecting wiring for taking out the electricity generated from the solar cell element) is provided on the lower surface of the back sheet 16. Bonded.
- Solar cell elements 14A and 14B are connected by wiring 20 in order to conduct the generated current to the outside. The wiring 20 is taken out through a through hole (not shown) provided in the back sheet 16 and connected to the junction box 18.
- a known method can be applied and is not particularly limited, but generally, an upper protective material, a sealing resin layer, a solar cell element, a sealing resin layer, a lower protection It has the process of laminating
- the solar cell module produced using the solar cell encapsulant of the present invention is a small solar cell represented by a mobile device, a large size installed on a roof or a roof, depending on the type of solar cell applied and the shape of the module. It can be applied to various uses regardless of whether it is indoors or outdoors, such as solar cells.
- the adhesiveness was evaluated under the conditions of an angle of 180 degrees and a tensile speed of 50 mm / sec, and evaluated according to the following criteria.
- the adhesive strength was 10N / 15mm width or more.
- the adhesive strength was less than 10N / 15mm width.
- Adhesive strength was 100N / 15mm width or more
- Adhesive strength was 20N / 15mm width or more and less than 100N / 15mm width
- Adhesion force was less than 20N / 15mm width
- a white plate glass with embossment made by Asahi Glass Co., Ltd., product name: Solite
- a fluorine-based back sheet (Cybrid) Made, wet index: 42 mN / m, no easy adhesion layer, PVdF / PET / PVdF laminate) with a thickness of 0.012 mm, length 90 mm, width 150 mm PET film (Mitsubishi Resin Co., Ltd., trade name: Dia Foil) and a corona-treated sheet-like encapsulant with a thickness of 0.45mm, and a PET film is created between the glass and the encapsulant to create a vacuum laminator.
- a white plate glass with embossment made by Asahi Glass Co., Ltd., product name: Solite
- a fluorine-based back sheet (Cybrid) Made, wet index: 42 mN / m, no easy adhesion layer, PVdF / PET / PVdF laminate
- the thickness is 0.5 mm between white plate glass (size: length 75 mm, width 25 mm) and aluminum plate (size: length 120 mm, width 60 mm) having a thickness of 2 mm (in Examples 6 to 9 and Comparative Example 4, the thickness is 0. 0).
- 45 mm) sheet-like sealing material is stacked, and using a vacuum press machine, a sample that is laminated and pressed at 150 ° C. for 15 minutes (10 minutes in Examples 6 to 9 and Comparative Example 4) is produced.
- a SUS-made heavy stone (size: length 75 mm, width 25 mm, weight: about 32 g) is fixed on glass, and the sample is installed at an inclination of 60 degrees in a thermostat at 100 ° C., after 500 hours have passed. Were observed and evaluated according to the following criteria.
- ⁇ The glass deviated from the initial reference position, or the sheet melted.
- Table 2 shows the absolute value of the difference in average refractive index between the polyethylene resin (X) and the silane-modified ethylene resin (Y) in the layer (I). Moreover, the absolute value of the difference in average refractive index between the polyethylene resin (X) and the other silane-modified ethylene resin (W) is shown in parentheses in Table 2 as reference values.
- Silane-modified ethylene resin (Y)] (Y-1); Silane-modified ethylene-octene random copolymer (manufactured by Mitsubishi Chemical Corporation, trade name: Linkron SL800N, density: 0.868 g / cm 3 , crystal melting peak temperature: 54 ° C. and 116 ° C., Heat of crystal fusion: 22 J / g and 4 J / g, storage elastic modulus (E ′) at 20 ° C .: 15 MPa, average refractive index: 1.4857, MFR (temperature: 190 ° C., load: 21.18 N): 1.7 g / 10min)
- Example 1 A resin composition in which (X-1) and (W-1) are mixed in a mass ratio of 95: 5 to the (I) layer, and (A-1) and (B-1) as the (II) layer Are mixed at a mass ratio of 95: 5, and a co-directional twin-screw extruder is used so as to obtain a layered structure of (I) layer / (II) layer / (I) layer. Were co-extruded at a resin temperature of 180 to 220 ° C.
- Example 4 In Example 3, the resin composition in which the mass ratio of (X-1) and (W-1) in the (I) layer was mixed at a ratio of 90:10 was used as the (II) layer as (A-2) and A sheet was obtained in the same manner as in Example 3 except that (B-1) was changed to a resin composition mixed at a mass ratio of 95: 5. Table 1 shows the results of the evaluation of each characteristic using the obtained sheet.
- Example 2 A sheet was obtained in the same manner as in Example 1 except that the layer (II) in Example 1 was changed to (A-1) 100 parts by mass of the resin composition. Table 1 shows the results of the evaluation of each characteristic using the obtained sheet.
- Comparative Example 3 The same procedure as in Comparative Example 1 was conducted except that 0.5 mass parts of a silane coupling agent (trade name: SILQUEST, manufactured by Momentive Co., Ltd.) was added to the resin composition of (A-1), and the resin composition was changed to a dry blended resin composition. Thus, a single layer sheet was obtained. Table 1 shows the results of the evaluation of each characteristic using the obtained sheet.
- a silane coupling agent trade name: SILQUEST, manufactured by Momentive Co., Ltd.
- Example 5 Using a vacuum laminator (trade name: LM30 ⁇ 30, manufactured by NPC Corporation), hot plate temperature: 150 ° C., processing time: 10 minutes (breakdown, evacuation: 3 minutes, press: 7 minutes) Crimping speed: Under rapid conditions, in order from the hot plate side, white plate glass having a thickness of 3 mm (made by Asahi Glass Co., Ltd., trade name: Solite) as the upper protective material, the thickness collected in Example 1 is 0.45 mm Sheet (encapsulant), solar cell having a thickness of 0.4 mm (manufactured by Photowatt, model: 101 ⁇ 101 MM), sheet (encapsulant) having a thickness of 0.45 mm collected in Example 1, and lower protection Five layers of a weather-resistant PET film (trade name: Lumirror X10S, manufactured by Toray Industries, Inc.) having a thickness of 0.125 mm as a material were vacuum-pressed to produce a solar cell module (size: 150 mm ⁇ 150 mm). The obtained solar cell module
- Example 7 In Example 6, as the (I) layer, a resin composition in which (X-3), (Y-1), and (W-1) were mixed at a mass ratio of 85: 13: 2, and (II) A sheet was obtained in the same manner as in Example 6 except that the layer was changed to a resin composition in which (A-3) and (B-2) were mixed at a mass ratio of 80:20. Table 2 shows the results of evaluation of each characteristic using the obtained sheet.
- Example 6 (Comparative Example 4) In Example 6, a sheet was obtained in the same manner as in Example 6 except that the resin composition constituting the layer (II) was changed to only (A-3). Table 2 shows the results of evaluation of each characteristic using the obtained sheet.
- the solar cell encapsulant defined in the present invention is excellent in all of adhesiveness, transparency (total light transmittance), and heat resistance (Examples 6 to 9).
- regulated by this invention can confirm that transparency (total light transmittance) or heat resistance is inadequate.
- the layer (II) does not contain the ethylene- ⁇ -olefin block copolymer (B), it can be confirmed that the heat resistance is insufficient (Comparative Example 4).
- Example 10 Using a vacuum laminator (Nisshinbo Co., Ltd., trade name: PVL0505S), hot plate temperature: 150 ° C., processing time: 10 minutes (breakdown, evacuation: 3 minutes, press: 7 minutes), pressure bonding speed: under rapid conditions
- a white plate glass having a thickness of 3 mm (trade name: Solite, manufactured by Asahi Glass Co., Ltd.), a sheet (sealing material) having a thickness of 0.45 mm collected in Example 1, and a thickness Is 0.4 mm solar battery cell (Photowatt Co., Ltd., model: 101 ⁇ 101 MM), 0.45 mm thick sheet (sealing material) collected in Example 7, and 0.125 mm thick as the lower protective material
- Five layers of weather-resistant PET film (trade name: Lumirror X10S, manufactured by Toray Industries, Inc.) were vacuum-pressed to produce a solar cell module (size: 150 mm ⁇ 150 mm
- Example 11 The sheet obtained in Example 9 was subjected to corona treatment on the sealing material under the conditions of irradiation intensity: 300 W and irradiation speed: 10 m / min (corona treatment amount: 60 W ⁇ min / m 2 ), and then thickness 3 .2 mm, 150 mm long, 150 mm wide embossed white plate glass (Asahi Glass Co., Ltd., trade name: Solite) and 0.33 mm thick fluorine-based back sheet (Cybrid, wetting index: 42 mN / m, no easy adhesion layer) Sheet having a thickness of 0.012 mm, a length of 90 mm and a width of 150 mm between the PVdF / PET / PVdF laminate) and a corona treatment thickness of 0.45 mm.
- a layer of sealing material is stacked, and a PET film is created between the glass and the sealing material.
- a vacuum laminator (trade name: PVL0505S, manufactured by Nisshinbo Co., Ltd.) ), A sample laminated at a temperature of 150 ° C., a vacuum of 3 minutes, and a press of 7 minutes was prepared, then a test piece having a width of 10 mm was prepared, and a chuck of a tensile tester (product name: 200X, manufactured by INTERSCO) A glass sheet was sandwiched between them, a back sheet and a sealing material were attached to the other chuck, and the adhesive strength was evaluated under the conditions of an angle of 180 degrees and a tensile speed of 50 mm / min. Moreover, the adhesive force was evaluated by the method mentioned above using the sample produced without carrying out the corona treatment to the sheet
- Example 12 In Example 11, the adhesive strength was evaluated in the same manner as in Example 11 except that the sheet obtained in Example 7 was changed. The results are shown in Table 3.
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Abstract
Description
前述したように、太陽電池モジュールは主に屋外で長期間使用されるため、その構成や材質構造等に種々の特性が必要とされる。前述した各保護部材の中でも封止材(封止樹脂層)に注目すると、水蒸気バリア性、太陽電池素子を保護する為の柔軟性、太陽電池モジュール製造におけるプロセス適性、具体的にはセルや配線の間隙を埋めるための流動特性、耐衝撃性、太陽電池モジュールが発熱した際の耐熱性、太陽電池素子へ太陽光が効率的に届く為の透明性(全光線透過率など)、ガラスやバックシート及びセルとの接着性、耐久性、寸法安定性、絶縁性等が主に要求される。
しかしながら、EVAシートを用いて太陽電池モジュールを製造する場合、その加熱圧着などの諸条件により、EVAの熱分解による酢酸ガスが発生し、作業環境および製造装置に悪影響を及ぼしたり、太陽電池の回路腐食や、太陽電池素子、フロントシート、バックシートなど各部材との界面で剥離が発生したりする等の問題があった。
また、特許文献3には、少なくとも一種のポリオレフィン系共重合体と、少なくとも一種の結晶性ポリオレフィンからなるポリマーブレンドまたはポリマーアロイであることを特徴とする太陽電池封止材が開示されており、具体的には、エチレン-メタクリル酸共重合体と汎用の結晶性ポリエチレンとのポリマーブレンド(実施例2参照)、エチレン-アクリル酸メチル共重合体と汎用の結晶性ポリプロピレンとのポリマーブレンド(実施例3参照)が用いられている。
また、特許文献4には、エチレン性不飽和シラン化合物と重合用ポリエチレンとを重合させてなるシラン変成樹脂(シラン架橋性樹脂)を有する太陽電池封止材が開示されている。
特許文献4の太陽電池モジュール用充填材層においては、ガラスやバックシートなど被着体との接着性を十分に発現させるようにシラン変性樹脂を多量添加すると、ヘーズが上昇して透明性が低下することが懸念され、接着性と透明性のバランスにおいては未だ問題があった。
また、通常封止材に接着性を付与するため、シランカップリング剤を添加する方法が知られているが、時間の経過と共にシランカップリング剤がブリードアウトし、水分と反応することにより接着力が低下するなどの懸念があり、さらなる改善の余地が残されていた。
本発明の課題は、太陽電池モジュールの形成が容易で、接着性、接着力の長期安定性、透明性及び耐熱性のいずれにも優れた太陽電池封止材およびそれを用いて作製された太陽電池モジュールを提供することにある。
すなわち、本発明は、少なくとも、接着層、特に、ポリエチレン系樹脂(X)及びシラン変性エチレン系樹脂(Y)を含有する特定の樹脂組成物(Z)からなる層((I)層)と、下記(a)の条件を満足するエチレン-α-オレフィンランダム共重合体(A)と下記(b)の条件を満足するエチレン-α-オレフィンブロック共重合体(B)を含有する樹脂組成物(C)からなる層((II)層)とを有する太陽電池封止材に関する。
(a)示差走査熱量測定における加熱速度10℃/分で測定される結晶融解熱量が0~70J/g
(b)示差走査熱量測定における加熱速度10℃/分で測定される結晶融解ピーク温度が100℃以上であり、かつ、結晶融解熱量が5~70J/g
また、酢酸による配線腐食や、水蒸気浸透による太陽電池素子の劣化の懸念がなく、作業環境および製造装置への悪影響や、太陽電池モジュールの劣化や発電効率の低下も防ぐことが出来る。さらに、製造設備についてもバッチ式の製造設備に加えて、ロール・ツー・ロール式の製造設備にも適用可能である。また、再生添加の際に透明性の低下を防止することも可能である。
なお、本明細書において、「主成分」とは、本発明の太陽電池封止材の各層を構成する樹脂の作用・効果を妨げない範囲で、他の成分を含むことを許容する趣旨である。さらに、この用語は、具体的な含有率を制限するものではないが、一般に樹脂組成物の構成成分全体を100質量部とした場合、50質量部以上であり、好ましくは65質量部以上、さらに好ましくは80質量部以上であって100質量部以下の範囲を占める成分である。
本発明の太陽電池封止材を構成する層のうち、(I)層は接着層であり、本発明の太陽電池封止材において、封止層であることはもちろん、接着層かつ表面層としての役割を有する層である。(I)層に用いられる樹脂組成物は、特に限定されるものではないが、接着性、接着力の長期安定性、透明性及び耐熱性の他、太陽電池封止材の製膜時の生産性の観点から、ポリオレフィン系樹脂を主成分とするものが好適に用いられる。
(I)層に用いられるポリオレフィン系樹脂としては、特に限定されるものではないが、接着性、透明性、生産性及び工業的に入手し易い点から、エチレン-メチルメタアクリレート共重合体(E-MMA)、エチレン-エチルアクリレート共重合体(E-EAA)、エチレン-グリシジルメタアクリレート共重合体(E-GMA)、エチレン-ビニルアルコール共重合体(EVOH)、アイオノマー樹脂(イオン架橋性エチレン-メタクリル酸共重合体、イオン架橋性エチレン-アクリル酸共重合体)、シラン変性ポリオレフィン(シラン架橋性ポリオレフィン)、及び無水マレイン酸グラフト共重合体からなる群から選ばれる少なくとも一種の変性ポリオレフィン系樹脂が好適に用いられる。
無水マレイン酸グラフト共重合体は、ポリオレフィン系樹脂、無水マレイン酸、及び後述するラジカル発生剤を高温で溶融混合し、グラフト重合することにより得ることができる。
本発明に用いるポリエチレン系樹脂(X)は、前記樹脂組成物(Z)が前記条件(a)を満足することを妨げない種類のものであれば、特に限定されるものではないが、具体的には、低密度ポリエチレン、超低密度ポリエチレン、または直鎖状低密度ポリエチレンが挙げられる。より具体的には、密度が0.850~0.920g/cm3のポリエチレン系樹脂が好ましく、特には、密度が0.860~0.880g/cm3の直鎖状低密度ポリエチレンが好ましい。また、密度が異なるポリエチレン系樹脂を組み合わせて用いてもかまわない。
当該結晶融解熱量は、示差走査熱量計を用いて、JIS K7122に準じて加熱速度10℃/分で測定することができる。
当該平均屈折率は、JIS K7142に準拠して、温度23℃においてナトリウムD線(589nm)を光源として測定することができる。
上記ポリエチレン系樹脂(X)は、一種であってもよいが二種以上の組み合わせであってもよい。
本発明に用いるシラン変性エチレン系樹脂(Y)は、通常、ポリエチレン系樹脂と後述するビニルシラン化合物、及び後述するラジカル発生剤を高温(160℃~220℃程度)で溶融混合し、グラフト重合することにより得ることができる。
前記(Y)を得るために用いられるポリエチレン系樹脂は、前記(X)に好適なポリエチレン系樹脂として例示したものと同様の組成や密度、MFR、結晶融解熱量、及び平均屈折率を有するものを用いることが好ましい。
具体的には、密度が0.850~0.920g/cm3のポリエチレン系樹脂が好ましく、密度が0.860~0.880g/cm3の直鎖状低密度ポリエチレンがより好ましい。また、メルトフローレート(MFR)は、特に限定されるものではないが、通常、MFR(JIS K7210、温度:190℃、荷重:21.18N)が、0.5~100g/10min程度、好ましくは2~50g/10min、さらに好ましくは3~30g/10minであるものが用いられる。
また、示差走査熱量測定における加熱速度10℃/分で測定される結晶融解熱量は0~70J/gであることが好ましい。より好ましくは、5~70J/g、さらに好ましくは、10~65J/gである。平均屈折率は、通常1.4800以上、1.5000以下の範囲であり、中でも1.4810以上、1.4990以下であることが好ましく、特に1.4820以上、1.4980以下であることが好ましい。
ビニルシラン化合物としては、前記ポリエチレン系樹脂とグラフト重合するものであれば特に限定されるものではないが、例えばビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリプロポキシシラン、ビニルトリイソプロポキシシラン、ビニルトリブトキシシラン、ビニルトリペンチロキシシラン、ビニルトリフェノキシシラン、ビニルトリベンジルオキシシラン、ビニルトリメチレンジオキシシラン、ビニルトリエチレンジオキシシラン、ビニルプロピオニルオキシシラン、ビニルトリアセトキシシラン、および、ビニルトリカルボキシシランからなる群より選ばれる少なくとも1種類のものを用いることができる。本発明においては、反応性、接着性や色調などの観点からビニルトリメトキシシランが好適に用いられる。
ラジカル発生剤としては、特に限定されるものではないが、例えば、ジイソプロピルベンゼンヒドロパーオキサイド、2,5-ジメチル-2,5-ジ(ヒドロパーオキシ)ヘキサン等のヒドロパーオキサイド類;ジ-t-ブチルパーオキサイド、t-ブチルクミルパーオキサイド、ジクミルパーオキサイド、2,5-ジメチル-2,5-ジ(t-ブチルパーオキシ)ヘキサン、2,5-ジメチル-2,5-ジ(t-パーオキシ)ヘキシン-3等のジアルキルパーオキサイド類;ビス-3,5,5-トリメチルヘキサノイルパーオキサイド、オクタノイルパーオキサイド、ベンゾイルパーオキサイド、o-メチルベンゾイルパーオキサイド、2,4-ジクロロベンゾイルパーオキサイド等のジアシルパーオキサイド類;t-ブチルパーオキシアセテート、t-ブチルパーオキシ-2-エチルヘキサノエート、t-ブチルパーオキシピバレート、t-ブチルパーオキシオクトエート、t-ブチルパーオキシイソプロピルカーボネート、t-ブチルパーオキシベンゾエート、ジ-t-ブチルパーオキシフタレート、2,5-ジメチル-2,5-ジ(ベンゾイルパーオキシ)ヘキサン、2,5-ジメチル-2,5-ジ(ベンゾイルパーオキシ)ヘキシン-3等のパーオキシエステル類;メチルエチルケトンパーオキサイド、シクロヘキサノンパーオキサイド等のケトンパーオキサイド類等の有機過酸化物、または、アゾビスイソブチロニトリル、アゾビス(2,4-ジメチルバレロニトリル)等のアゾ化合物等が挙げられる。
本発明に用いるシラン変性エチレン系樹脂(Y)は、前述の通り、通常は前記ポリエチレン系樹脂をビニルシラン化合物及びラジカル発生剤を高温(160℃~220℃程度)で溶融混合し、グラフト重合させて得られるものである。よって、本発明に用いるシラン変性エチレン系樹脂(Y)の密度、及びMFRの好適な範囲については、前記ポリエチレン系樹脂の密度、及びMFRの好適な範囲と同様となる。
上記シラン変性エチレン系樹脂(Y)は、一種であってもよいが二種以上の組み合わせであってもよい。
(I)層を構成する樹脂組成物は、ポリオレフィン系樹脂を主成分とするものであるが、諸物性(柔軟性、耐熱性、透明性、接着性など)や成形加工性あるいは経済性などを考慮して、前記変性ポリオレフィン系樹脂を主成分とするものを使用することもできるが、変性ポリオレフィン系樹脂以外のポリオレフィン系樹脂(以下、「未変性ポリオレフィン系樹脂」という)を併用することが好ましく、この併用したものを主成分とすることがより好ましい。
該未変性ポリオレフィン系樹脂は特に限定されないが、前記変性ポリオレフィン系樹脂を構成するオレフィン単量体を主成分として構成されているものであることが、透明性の観点から好ましい。また、未変性ポリオレフィン系樹脂が、後述する(II)層で用いるエチレン-α-オレフィンランダム共重合体(A)や、エチレン-α-オレフィンブロック共重合体(B)であれば、(I)層と(II)層との層間接着性や柔軟性、耐熱性などの観点から好ましい。
また、(I)層を構成する樹脂組成物に、変性ポリオレフィン系樹脂と未変性ポリオレフィン系樹脂を併用する場合、用いる変性ポリオレフィン系樹脂と未変性ポリオレフィン系樹脂は、同一系統の樹脂、例えば、変性ポリエチレン系樹脂と未変性ポリエチレン系樹脂であることが好ましい。
該樹脂組成物(Z)中の前記ポリエチレン系樹脂(X)と前記シラン変性エチレン系樹脂(Y)の混合質量比は、特に限定されるものではないが、ポリエチレン系樹脂(X)/シラン変性エチレン系樹脂(Y)質量比で、1~99/99~1であり、好ましくは、30~98/70~2、より好ましくは、60~97/40~3である。かかる範囲内であれば、(I)層中のシラン変性エチレン系樹脂(Y)の含有量、すなわち、シラン変性基濃度が調整し易く、(I)層の主な役割である接着層としての機能を保持しつつ、表面層、封止層としての柔軟性、透明性、封止性や耐熱性などの諸特性の調整が比較的容易にできるため好ましい。
本発明の太陽電池封止材を構成する層のうち、(II)層は下記(a)の条件を満足するエチレン-α-オレフィンランダム共重合体(A)と下記(b)の条件を満足するエチレン-α-オレフィンブロック共重合体(B)を含有する樹脂組成物(C)からなる層である。
(a)示差走査熱量測定における加熱速度10℃/分で測定される結晶融解熱量が0~70J/g
(b)示差走査熱量測定における加熱速度10℃/分で測定される結晶融解ピーク温度が100℃以上であり、かつ、結晶融解熱量が5~70J/g
本発明に用いられるエチレン-α-オレフィンランダム共重合体(A)は、上記の条件(a)を満足すれば特に限定されるものではないが、通常、エチレンと炭素数3~20のα-オレフィンとのランダム共重合体が好適に用いられる。ここでエチレンと共重合するα-オレフィンとしては、プロピレン、1-ブテン、1-ペンテン、1-へキセン、1-へプテン、1-オクテン、1-ノネン、1-デセン、3-メチル-ブテン-1、4-メチル-ペンテン-1等が例示される。本発明においては、工業的な入手し易さや諸特性、経済性などの観点からエチレンと共重合するα-オレフィンとしては、プロピレン、1-ブテン、1-へキセン、1-オクテンが好適に用いられる。エチレンと共重合するα-オレフィンは1種のみを単独でまたは2種以上を組み合わせて用いてもかまわない。
当該結晶融解熱量は、示差走査熱量計を用いて、JIS K7122に準じて加熱速度10℃/分で測定することができる。
当該結晶融解ピーク温度は、示差走査熱量計を用いて、JIS K7121に準じて加熱速度10℃/分で測定することができる。
本発明に用いられるエチレン-α-オレフィンブロック共重合体(B)は、既述の条件(b)を満足すれば特に限定されるものではないが、通常、エチレンと炭素数3~20のα-オレフィンとのブロック共重合体が好適に用いられる。ここでエチレンと共重合するα-オレフィンとしては、プロピレン、1-ブテン、1-ペンテン、1-へキセン、1-へプテン、1-オクテン、1-ノネン、1-デセン、3-メチル-ブテン-1、4-メチル-ペンテン-1等が例示される。本発明においては、工業的な入手し易さや諸特性、経済性などの観点からエチレンと共重合するα-オレフィンとしては、プロピレン、1-ブテン、1-へキセン、1-オクテンが好適に用いられる。エチレンと共重合するα-オレフィンは1種のみを単独でまたは2種以上を組み合わせて用いてもかまわない。
該マルチブロック構造を有するエチレン-α-オレフィンブロック共重合体は、本発明において好適に使用でき、α-オレフィンとして1-オクテンを共重合成分とするエチレン-オクテンマルチブロック共重合体が好ましい。該ブロック共重合体としては、エチレンに対してオクテン成分が多く(約15~20モル%)共重合されたほぼ非晶性のソフトセグメントと、エチレンに対してオクテン成分が少なく(約2モル%未満)共重合された結晶融解ピーク温度が110~145℃である高結晶性のハードセグメントが、各々2つ以上存在するマルチブロック共重合体が好ましい。これらのソフトセグメントとハードセグメントの連鎖長や比率を制御することにより、柔軟性と耐熱性の両立を達成することができる。
該マルチブロック構造を有する共重合体の具体例としては、ダウ・ケミカル(株)製の商品名「インフューズ(Infuse)」が挙げられる。
本発明における(II)層は、上述したエチレン-α-オレフィンランダム共重合体(A)とエチレン-α-オレフィンブロック共重合体(B)を含有する樹脂組成物(C)からなる。ここで、これらの共重合体(A)及び共重合体(B)の各々に用いられるα-オレフィンの種類は、同一であってもよいし、異なっていてもよいが、本発明においては、同一である方が、混合した際の相溶性や太陽電池封止材の透明性が向上する、すなわち、太陽電池の光電変換効率が向上するため好ましい。
硫黄系としては、ジラウリルチオジプロピオネート、ジミリスチルチオジプロピオネート、ジステアリルチオプロピオネートなどを挙げることができる。
該紫外線吸収剤の添加量は、(I)層及び(II)層の各々を構成する樹脂組成物100質量部に対し、通常0.01質量部以上、好ましくは0.05質量部以上であり、かつ、2.0質量部以下、好ましくは0.5質量部以下の範囲で添加することが好ましい。
本発明の太陽電池封止材は、少なくとも前記(I)層と前記(II)層とを有することが必要である。層構成としては、(I)層と(II)層とを各々少なくとも1層有していれば特に限定されるものではなく、例えば(I)層/(II)層という2種2層構成や、(I)層/(II)層/(I)層という2種3層構成、(I)層/(II)層/(I)層/(II)層という2種4層構成などが挙げられる。
このうち、本発明においては、フロントシートやバックシート、太陽電池素子との接着性の向上を図る観点から、(I)層を、最外層の少なくとも一方に有する構成であることが好ましく、その両方に有することがより好ましい。
また、本発明の太陽電池封止材は、接着性を向上させる観点から、その少なくとも一方の面にコロナ処理やプラズマ処理等の表面処理を施すことができる。
さらに、シートを製膜する際に、シート製膜時のハンドリング性を向上するなどの目的のため、別の基材フィルム(延伸ポリエステルフィルム(OPET)や延伸ポリプロピレンフィルム(OPP)など)と押出ラミやサンドラミなどの方法で積層しても構わない。
貯蔵弾性率(E´)は、粘弾性測定装置を用いて、振動周波数10Hzにおいて所定温度で測定し、温度20℃における値を求めることで得られる。
全光線透過率及びヘーズは、JIS K7361に準じてヘーズメーターを用いて測定することで得られる。
本発明においては、耐熱性は、例えば、白板ガラスとアルミ板の間にシート状の封止材を重ね、真空プレス機を用いて所定温度で積層プレスした試料を作製し、該試料を100℃の恒温槽内で所定角度に傾斜して設置し所定時間経過後の状態を観察して評価することができる。
本発明においては、これらのバランスを柔軟性の指標として動的粘弾性測定における振動周波数10Hz、温度20℃の貯蔵弾性率(E´)、耐熱性の指標としてエチレン-α-オレフィンブロック共重合体(B)について示差走査熱量測定における加熱速度10℃/分で測定される結晶融解ピーク温度を、および透明性の指標として全光線透過率を用いた場合、3つの指標が、貯蔵弾性率(E´)が1~2000MPa、結晶融解ピーク温度が100℃以上、全光線透過率85%以上であることが好ましく、貯蔵弾性率(E´)が5~500MPa、結晶融解ピーク温度が105~145℃、全光線透過率85%以上であることがさらに好ましく、貯蔵弾性率(E´)が10~100MPa、結晶融解ピーク温度が110~145℃、全光線透過率90%以上であることが特に好ましい。
本発明の太陽電池封止材を用い、太陽電池素子を上下の保護材であるガラス又はフロントシートおよびバックシートで固定することにより、太陽電池モジュールを製作することができる。このような太陽電池モジュールとしては、種々のタイプのものを例示することができ、好ましくは、本発明の太陽電池封止材と、上部保護材と、太陽電池素子と、下部保護材とを用いて作製された太陽電池モジュールが挙げられ、具体的には、上部保護材/本発明の封止材(封止樹脂層)/太陽電池素子/本発明の封止材(封止樹脂層)/下部保護材のように太陽電池素子の両側から本発明の封止材ではさむ様な構成のもの(図1参照)、下部保護材の内周面上に形成させた太陽電池素子の上に本発明の封止材と上部保護材を形成させるような構成のもの、上部保護材の内周面上に形成させた太陽電池素子、例えばフッ素樹脂系透明保護材上にアモルファス系太陽電池素子をスパッタリング等で作製したものの上に本発明の封止材として下部保護材を形成させるような構成のものなどを挙げることができる。なお、本発明の太陽電池封止材を用いた太陽電池モジュールにおいて、封止材が2箇所以上の部位に使用される場合、すべての部位に本発明の太陽電池封止材を用いてもかまわないし、1箇所のみの部位に本発明の太陽電池封止材を用いてもかまわない。また、封止材が2箇所以上の部位に使用される場合、各々の部位に使用される本発明の太陽電池封止材を構成する樹脂組成は同一であっても良いし、異なっていてもよい。
これらの上部および下部の保護材の表面には、本発明の太陽電池封止材やその他の部材との接着性を向上させるためにプライマー処理やコロナ処理など公知の表面処理を施すことができる。
本実施例における封止材シートについての種々の測定および評価は次のようにして行った。
(結晶融解ピーク温度(Tm))
示差走査熱量計((株)パーキンエルマー製の、商品名「PyrIs1 DSC」)を用いて、JIS K7121に準じて、試料約10mgを加熱速度10℃/分で-40℃から200℃まで昇温し、200℃で5分間保持した後、冷却速度10℃/分で-40℃まで降温し、再度、加熱速度10℃/分で200℃まで昇温した時に測定されたサーモグラムから結晶融解ピーク温度(Tm)(℃)を求めた。
示差走査熱量計((株)パーキンエルマー製の、商品名「PyrIs1 DSC」)を用いて、JIS K7122に準じて、試料約10mgを加熱速度10℃/分で-40℃から200℃まで昇温し、200℃で5分間保持した後、冷却速度10℃/分で-40℃まで降温し、再度、加熱速度10℃/分で200℃まで昇温した時に測定されたサーモグラムから結晶融解熱量(ΔHm)(J/g)を求めた。
(1)実施例1~4及び比較例1~3のシート
ガラスとの接着性については、厚み2mm、縦150mm、横25mmの白板ガラスと厚み0.16mmのフッ素系バックシート(KREMPEL社製、商品名:AKASOL、易接着コート層有り、PVF/PET/PVF積層体)の間に厚みが0.45mmのシート状の封止材と厚み0.012mm、縦50mm、横30mmのPETフィルム(三菱樹脂(株)製、商品名:ダイアホイル)を重ね、ガラスと封止材の間にきっかけをつくり、真空プレス機を用い、温度150℃、10分の条件で積層プレスした試料を作製した後、引張試験機(INTESCO社製、商品名:200X型試験機)のチャックにガラスを挟み、もう一方のチャックにバックシートと封止材を取り付けることにより、角度180度、引張速度50mm/secの条件で接着性を評価し、以下の基準で評価した。
(○)接着力が10N/15mm巾以上であったもの
(×)接着力が10N/15mm巾未満であったもの
厚み3.2mm、縦150mm、横150mmのエンボス付白板ガラス(旭硝子社製、商品名:ソライト)と厚み0.33mmのフッ素系バックシート(Krempel社製、商品名:ACASOL、易接着コート層有り、PVF/PET/PVF積層体)の間に厚み0.012mm、縦90mm、横150mmのPETフィルム(三菱樹脂(株)製、商品名:ダイアホイル)と厚みが0.45mmのシート状の封止材を重ね、ガラスと封止材の間にPETフィルムできっかけをつくり、真空ラミネーター(日清紡社製、商品名:PVL0505S)を用い、温度150℃、真空3分、プレス7分の条件で積層した試料を作製した後、幅10mmの試験片を作製し、引張試験機(INTESCO社製、商品名:200X)のチャックにガラスを挟み、もう一方のチャックにバックシートと封止材を取り付け、角度180度、引張速度50mm/minの条件で接着性を評価し、以下の基準で評価した。
(◎)接着力が100N/15mm巾以上であったもの
(○)接着力が20N/15mm巾以上、100N/15mm巾未満であったもの
(×)接着力が20N/15mm巾未満であったもの
照射幅が0.5mのコロナ処理機を用いて、照射強度:300W、照射スピード:10m/minの条件(コロナ処理量:60W・min/m2)で、封止材にコロナ処理を行なった後、厚み3.2mm、縦150mm、横150mmのエンボス付白板ガラス(旭硝子社製、商品名:ソライト)と厚み0.33mmのフッ素系バックシート(Cybrid社製、濡れ指数:42mN/m、易接着層無し、PVdF/PET/PVdF積層体)の間に厚み0.012mm、縦90mm、横150mmのPETフィルム(三菱樹脂(株)製、商品名:ダイアホイル)とコロナ処理をした厚みが0.45mmのシート状の封止材を重ね、ガラスと封止材の間にPETフィルムできっかけをつくり、真空ラミネーター(日清紡社製、商品名:PVL0505S)を用い、温度150℃、真空3分、プレス7分の条件で積層した試料を作製した後、幅10mmの試験片を作製し、引張試験機(INTESCO社製、商品名:200X)のチャックにガラスを挟み、もう一方のチャックにバックシートと封止材を取り付け、角度180度、引張速度50mm/minの条件で接着性を評価した。
各種封止材を製膜後、温度25℃、湿度50%の条件下で4ヶ月曝露した後、前記接着性の評価と同様にサンプルを作製して、接着性を評価し、以下の基準で評価した。
(○)接着力が10N/15mm巾以上であったもの
(×)接着力が10N/15mm巾未満であったもの
(1)実施例1~4及び比較例1~3のシート
厚み2mmの白板ガラス(SCHOTT社製、商品名:B270、サイズ;縦50mm、横50mm)2枚の間に厚みが0.45mmのシート状の封止材を重ね、熱プレス機を用いて、150℃、1分の条件でプレスした試料を作製し、JIS K7105に準じて全光線透過率を測定し、その値を記載するとともに、下記の基準で評価した結果も併記した。
(◎)全光線透過率が90%以上であったもの
(○)全光線透過率が85%以上、90%未満であったもの
(×)全光線透過率が85%未満、あるいは、明らかに白濁している場合(未測定)
厚み2mmの白板ガラス(SCHOTT社製、商品名:B270、サイズ;縦50mm、横50mm)2枚の間に厚みが0.45mmのシート状の封止材を重ね、前記と同様の真空ラミネーターを用いて、温度150℃、真空5分、プレス30秒の条件で積層プレスした試料を作製した後、JIS K7361に準じてヘーズメーター(日本電色工業(株)社製、商品名:NDH-5000)を用いて全光線透過率を測定し、その値を記載するとともに、下記の基準で評価した結果も併記した。
(○)全光線透過率が85%以上であったもの
(×)全光線透過率が85%未満、あるいは、明らかに白濁している場合(未測定)
前記全光線透過率の評価で作製した方法と同様にサンプルを作製し、JIS K7361に準じてヘーズメーターを用いてヘーズを測定し、その値を記載するとともに、下記の基準で評価した結果も併記した。
(○)ヘーズが10%未満であったもの
(×)ヘーズが10%以上、あるいは、明らかに白濁している場合(未測定)
厚み2mmの白板ガラス(サイズ;縦75mm、横25mm)と厚み5mmのアルミ板(サイズ;縦120mm、横60mm)の間に厚みが0.5mm(実施例6~9及び比較例4では0.45mm)のシート状の封止材を重ね、真空プレス機を用いて、150℃、15分(実施例6~9及び比較例4では10分)の条件で積層プレスした試料を作製し、白板ガラス上にSUS製の重石(サイズ:縦75mm、横25mm、重量:約32g)を固定し、該試料を100℃の恒温槽内で60度に傾斜して設置し、500時間経過後の状態を観察し、下記の基準で評価した。
(○)ガラスが初期の基準位置からずれなかったもの
(×)ガラスが初期の基準位置からずれたり、シートが溶融したもの
(株)アタゴ製アッベ屈折計を用いて、JIS K7142に準拠して、温度23℃においてナトリウムD線(589nm)を光源として測定した。(I)層におけるポリエチレン系樹脂(X)と、シラン変性エチレン系樹脂(Y)の平均屈折率の差の絶対値を表2に示した。また、参考値として、ポリエチレン系樹脂(X)と、その他のシラン変性エチレン系樹脂(W)の平均屈折率の差の絶対値を表2の括弧内に示した。
以下に、実施例・比較例に用いた構成材料を示す。
[ポリエチレン系樹脂(X)]
(X-1); エチレン-オクテンランダム共重合体(ダウ・ケミカル(株)製、商品名:エンゲージ8200、エチレン/1-オクテン=69/31質量%(89/10モル%)、MFR:5、Tm:65℃、ΔHm:53J/g)
(X-2);エチレンーオクテンブロック共重合体(ダウ・ケミカル(株)製、商品名:インフューズ9000、密度:0.875g/cm3、エチレン/1-オクテン=65/35質量%(88/12モル%)、結晶融解ピーク温度:122℃、結晶融解熱量:44J/g、20℃における貯蔵弾性率(E’):27MPa、平均屈折率:1.4899、MFR(温度:190℃、荷重:21.18N):0.5g/10min)
(X-3); エチレン-オクテンランダム共重合体(ダウ・ケミカル(株)製、商品名:アフィニティーEG8200G、密度:0.870g/cm3、エチレン/1-オクテン=68/32質量%(89/11モル%)、結晶融解ピーク温度:59℃、結晶融解熱量:49J/g、20℃における貯蔵弾性率(E’):14MPa、平均屈折率:1.4856、MFR(温度:190℃、荷重:21.18N):5g/10min)
(Y-1);シラン変性エチレン-オクテンランダム共重合体(三菱化学(株)製、商品名:リンクロンSL800N、密度:0.868g/cm3、結晶融解ピーク温度:54℃と116℃、結晶融解熱量:22J/gと4J/g、20℃における貯蔵弾性率(E’):15MPa、平均屈折率:1.4857、MFR(温度:190℃、荷重:21.18N):1.7g/10min)
(W-1);シラン変性エチレン-ヘキセンランダム共重合体(三菱化学(株)製、商品名:リンクロンXLE815N、密度:0.915g/cm3、結晶融解ピーク温度:121℃、結晶融解熱量:127J/g、20℃における貯蔵弾性率(E’):398MPa、平均屈折率:1.5056、MFR(温度:190℃、荷重:21.18N):0.5g/10min)
[エチレン-α-オレフィンランダム共重合体(A)]
(A-1);エチレン-オクテンランダム共重合体(ダウ・ケミカル(株)製、商品名:エンゲージ8200、エチレン/1-オクテン=69/31質量%(89/10モル%)、MFR:5、Tm:65℃、ΔHm:53J/g)
(A-2);エチレン-プロピレン-ヘキセン3元ランダム共重合体(日本ポリエチレン(株)製、商品名:カーネルKJ640T、エチレン/プロピレン/ヘキセン=80/10/10質量%(88.2/7.4/4.4モル%)、結晶融解ピーク温度:53℃、結晶融解熱量:58J/g、20℃における貯蔵弾性率(E’):30MPa、平均屈折率:1.4947、MFR(温度:190℃、荷重:21.18N):5g/10min)
(A-3);エチレン-オクテンランダム共重合体(ダウ・ケミカル(株)製、商品名:アフィニティーEG8200G、密度:0.870g/cm3、エチレン/1-オクテン=68/32質量%(89/11モル%)、結晶融解ピーク温度:59℃、結晶融解熱量:49J/g、20℃における貯蔵弾性率(E’):14MPa、平均屈折率:1.4856、MFR(温度:190℃、荷重:21.18N):5g/10min)
(B-1);エチレンーオクテンブロック共重合体(ダウ・ケミカル(株)製、商品名:D910
0.05、エチレン/1-オクテン=63/37質量%(87.2/12.8モル%)、結晶融解ピーク温度:119℃、結晶融解熱量:38J/g、MFR(温度:190℃、荷重:21.18N):1g/10min)
(B-2);エチレン-オクテンブロック共重合体(ダウ・ケミカル(株)製、商品名:インフューズ9507、密度:0.866g/cm3、エチレン/オクテン=56/44質量%(83.6/16.4モル%)、結晶融解ピーク温度:123℃、結晶融解熱量:21J/g、20℃における貯蔵弾性率(E’):12MPa、平均屈折率:1.4828、MFR(温度:190℃、荷重:21.18N):5g/10min)
(B-3);エチレンーオクテンブロック共重合体(ダウ・ケミカル(株)製、商品名:インフューズ9000、密度:0.875g/cm3、エチレン/1-オクテン=65/35質量%(88/12モル%)、結晶融解ピーク温度:122℃、結晶融解熱量:44J/g、20℃における貯蔵弾性率(E’):27MPa、平均屈折率:1.4899、MFR(温度:190℃、荷重:21.18N):0.5g/10min)
(I)層に(X-1)と(W-1)を、質量比95:5の割合で混合した樹脂組成物、また、(II)層として(A-1)と(B-1)を、質量比95:5の割合で混合した樹脂組成物をそれぞれ用いて、(I)層/(II)層/(I)層の積層構成となるように、同方向二軸押出機を用いたTダイ法にて樹脂温180~220℃にて共押出成形した後、20℃のキャストロールで急速製膜し、各層厚みが(I)/(II)/(I)=0.09mm/0.27mm/0.09mmであるシートを得た。得られたシートを用いて各特性を評価した結果を表1に示す。
実施例1において、積層構成を(I)層/(II)層にし、各層厚みが(I)/(II)=0.09mm/0.36mmになるように変更した以外は、実施例1と同様にしてシートを得た。得られたシートを用いて各特性を評価した結果を表1に示す。
実施例1において、(II)層として(A-1)と(B-1)を、質量比80:20の割合で混合した樹脂組成物を用いて、各層厚みが(I)/(II)/(I)=0.045mm/0.36mm/0.045mmとなるように変更した以外は、実施例1と同様にしてシートを得た。得られたシートを用いて各特性を評価した結果を表1に示す。
実施例3において、(I)層の(X-1)と(W-1)との質量比を90:10の割合で混合した樹脂組成物に、(II)層として(A-2)と(B-1)を、質量比95:5の割合で混合した樹脂組成物にそれぞれ変更した以外は、実施例3と同様にしてシートを得た。得られたシートを用いて各特性を評価した結果を表1に示す。
(X-1)と(W-1)を、質量比95:5の割合で混合した樹脂組成物を用いて、Tダイ法にて樹脂温180~220℃にて押出成形した後、20℃のキャストロールで急速製膜し、厚みが0.45mmである単層のシートを得た。得られたシートを用いて各特性を評価した結果を表1に示す。
実施例1において、(II)層を(A-1)100質量部の樹脂組成物に変更した以外は、実施例1と同様にしてシートを得た。得られたシートを用いて各特性を評価した結果を表1に示す。
(A-1)の樹脂組成物にシランカップリング剤(モメンティブ社製、商品名:SILQUEST)を0.5質量部加えてドライブレンドした樹脂組成物に変更した以外は、比較例1と同様にして単層のシートを得た。得られたシートを用いて各特性を評価した結果を表1に示す。
真空ラミネーター((株)エヌ・ピー・シー製、商品名:LM30×30)を用いて、熱板温度:150℃、加工時間:10分(内訳、真空引き:3分、プレス:7分)、圧着速度:急速の条件で、熱板側から順に、上部保護材として厚みが3mmの白板ガラス(旭硝子(株)製、商品名:ソライト)、実施例1で採取した厚みが0.45mmのシート(封止材)、厚みが0.4mmの太陽電池セル(フォトワット社製、型式:101×101MM)、実施例1で採取した厚みが0.45mmのシート(封止材)、下部保護材として厚みが0.125mmの耐候性PETフィルム(東レ(株)製、商品名:ルミラーX10S)の5層を真空プレスして太陽電池モジュール(サイズ:150mm×150mm)を作製した。得られた太陽電池モジュールは透明性や外観などに優れるものであった。
(I)層として、(X-3)と(Y-1)を、質量比70:30の割合で混合した樹脂組成物、また、(II)層として、(A-3)と(B-3)を、質量比95:5の割合で混合した樹脂組成物をそれぞれ用いて、(I)層/(II)層/(I)層の積層構成となるように、同方向二軸押出機を用いたTダイ法にて樹脂温180~200℃にて共押出成形した後、20℃のキャストロールで急冷製膜し、各層厚みが(I)/(II)/(I)=0.09mm/0.27mm/0.09mmであるシートを得た。得られたシートを用いて各特性を評価した結果を表2に示す。
実施例6において、(I)層として、(X-3)と(Y-1)と(W-1)を質量比85:13:2の割合で混合した樹脂組成物、また、(II)層として、(A-3)と(B-2)を質量比80:20の割合で混合した樹脂組成物に変更した以外は、実施例6と同様にしてシートを得た。得られたシートを用いて各特性を評価した結果を表2に示す。
実施例6において、(II)層として、(A-2)と(B-3)を質量比95:5の割合で混合した樹脂組成物に変更し、さらに各層厚みが(I)/(II)/(I)=0.045mm/0.36mm/0.045mmとなるように変更した以外は、実施例6と同様にしてシートを得た。得られたシートを用いて各特性を評価した結果を表2に示す。
実施例6において、(I)層として、(X-3)と(X-2)と(Y-1)を質量比90:5:5の割合で混合した樹脂組成物に変更し、さらに各層厚みが(I)/(II)/(I)=0.045mm/0.36mm/0.045mmとなるように変更した以外は、実施例6と同様にしてシートを得た。得られたシートを用いて各特性を評価した結果を表2に示す。
実施例6において、(II)層を構成する樹脂組成物を(A-3)のみに変更した以外は、実施例6と同様にしてシートを得た。得られたシートを用いて各特性を評価した結果を表2に示す。
真空ラミネーター(日清紡社製、商品名:PVL0505S)を用いて、熱板温度:150℃、加工時間:10分(内訳、真空引き:3分、プレス:7分)、圧着速度:急速の条件で、熱板側から順に、上部保護材として厚みが3mmの白板ガラス(旭硝子(株)製、商品名:ソライト)、実施例1で採取した厚みが0.45mmのシート(封止材)、厚みが0.4mmの太陽電池セル(フォトワット社製、型式:101×101MM)、実施例7で採取した厚みが0.45mmのシート(封止材)、下部保護材として厚みが0.125mmの耐候性PETフィルム(東レ(株)製、商品名:ルミラーX10S)の5層を真空プレスして太陽電池モジュール(サイズ:150mm×150mm)を作製した。得られた太陽電池モジュールは透明性や外観などに優れるものであった。
実施例9において得られたシートに、照射強度:300W、照射スピード:10m/minの条件(コロナ処理量:60W・min/m2)で、封止材にコロナ処理を行なった後、厚み3.2mm、縦150mm、横150mmのエンボス付白板ガラス(旭硝子社製、商品名:ソライト)と厚み0.33mmのフッ素系バックシート(Cybrid社製、濡れ指数:42mN/m、易接着層無し、PVdF/PET/PVdF積層体)の間に厚み0.012mm、縦90mm、横150mmのPETフィルム(三菱樹脂(株)製、商品名:ダイアホイル)とコロナ処理をした厚みが0.45mmのシート状の封止材を重ね、ガラスと封止材の間にPETフィルムできっかけをつくり、真空ラミネーター(日清紡社製、商品名:PVL0505S)を用い、温度150℃、真空3分、プレス7分の条件で積層した試料を作製した後、幅10mmの試験片を作製し、引張試験機(INTESCO社製、商品名:200X)のチャックにガラスを挟み、もう一方のチャックにバックシートと封止材を取り付け、角度180度、引張速度50mm/minの条件で接着力を評価した。また、実施例9において得られたシートにコロナ処理をせずに作製したサンプルを用いて、前述した手法で接着力を評価し、コロナ処理の効果を比較した。結果を表3に示す。
実施例11において、実施例7で得られたシートに変更した以外は実施例11と同様にして接着力を評価した。結果を表3に示す。
12A,12B・・・封止樹脂層
14A,14B・・・太陽電池素子
16・・・バックシート
18・・・ジャンクションボックス
20・・・配線
Claims (10)
- 少なくとも、接着層((I)層)と、下記(a)の条件を満足するエチレン-α-オレフィンランダム共重合体(A)と下記(b)の条件を満足するエチレン-α-オレフィンブロック共重合体(B)を含有する樹脂組成物(C)からなる層((II)層)とを有する太陽電池封止材。
(a)示差走査熱量測定における加熱速度10℃/分で測定される結晶融解熱量が0~70J/g
(b)示差走査熱量測定における加熱速度10℃/分で測定される結晶融解ピーク温度が100℃以上であり、かつ、結晶融解熱量が5~70J/g - 前記(I)層が、ポリオレフィン系樹脂を主成分とする樹脂組成物からなることを特徴とする請求項1に記載の太陽電池封止材。
- 前記(I)層が、紫外線吸収剤及び/または耐候安定剤を含有することを特徴とする請求項1又は2に記載の太陽電池封止材。
- 前記(I)層が、ポリエチレン系樹脂(X)、及びシラン変性エチレン系樹脂(Y)を含有し、かつ下記(a)の条件を満足する樹脂組成物(Z)からなる(I)層であることを特徴とする請求項1~3のいずれか1項に記載の太陽電池封止材。
(a)示差走査熱量測定における加熱速度10℃/分で測定される結晶融解熱量が0~70J/g - 前記ポリエチレン系樹脂(X)と前記シラン変性エチレン系樹脂(Y)との平均屈折率の差の絶対値が0.0100以下であることを特徴とする請求項4記載の太陽電池封止材。
- 前記エチレン-α-オレフィンブロック共重合体(B)がエチレン-オクテンマルチブロック共重合体であることを特徴とする請求項1~5のいずれか1項に記載の太陽電池封止材。
- 前記エチレン-α-オレフィンランダム共重合体(A)と前記エチレン-α-オレフィンブロック共重合体(B)を構成するα-オレフィンの種類が同一であることを特徴とする請求項1~6のいずれか1項に記載の太陽電池封止材。
- 前記ポリエチレン系樹脂(X)、前記シラン変性エチレン系樹脂(Y)、前記エチレン-α-オレフィンランダム共重合体(A)及び前記エチレン-α-オレフィンブロック共重合体(B)の各々を構成するα-オレフィンの種類が同一であることを特徴とする請求項4~7のいずれか1項に記載の太陽電池封止材。
- 動的粘弾性測定における振動周波数10Hz、温度20℃の貯蔵弾性率(E´)が10~100MPa、示差走査熱量測定における加熱速度10℃/分で測定される結晶融解ピーク温度が110~145℃、及び全光線透過率85%以上であることを特徴とする請求項1~8のいずれか1項に記載の太陽電池封止材。
- 請求項1~9のいずれか1項に記載の太陽電池封止材を用いて作製された太陽電池モジュール。
Priority Applications (6)
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RU2013114380/04A RU2592608C2 (ru) | 2010-08-30 | 2011-07-28 | Материал для герметизации солнечных батарей и модуль солнечной батареи, изготовленный с его использованием |
CA2809757A CA2809757A1 (en) | 2010-08-30 | 2011-07-28 | Solar cell sealing material and solar cell module produced by using same |
CN201180040002.8A CN103081121B (zh) | 2010-08-30 | 2011-07-28 | 太阳能电池封装材料及使用其制成的太阳能电池组件 |
KR1020137005006A KR20130111536A (ko) | 2010-08-30 | 2011-07-28 | 태양 전지 봉지재 및 그것을 이용하여 제작된 태양 전지 모듈 |
EP11821482.4A EP2613361A4 (en) | 2010-08-30 | 2011-07-28 | SOLAR CELL TEMPERATURE MATERIAL AND SOLAR CELL MODULE MANUFACTURED THEREOF |
US13/819,170 US20130213476A1 (en) | 2010-08-30 | 2011-07-28 | Solar cell sealing material and solar cell module produced by using same |
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JP2010192643A JP5654804B2 (ja) | 2010-08-30 | 2010-08-30 | 太陽電池封止材及びそれを用いて作製された太陽電池モジュール |
JP2010-192643 | 2010-08-30 | ||
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US (1) | US20130213476A1 (ja) |
EP (1) | EP2613361A4 (ja) |
KR (1) | KR20130111536A (ja) |
CN (1) | CN103081121B (ja) |
CA (1) | CA2809757A1 (ja) |
MY (1) | MY165895A (ja) |
RU (1) | RU2592608C2 (ja) |
TW (1) | TWI538922B (ja) |
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JP2013214559A (ja) * | 2012-03-30 | 2013-10-17 | Mitsubishi Plastics Inc | 太陽電池用表面保護シート・封止材積層体 |
JP2013212600A (ja) * | 2012-03-30 | 2013-10-17 | Mitsubishi Plastics Inc | 積層防湿フィルム |
JP2014003055A (ja) * | 2012-06-15 | 2014-01-09 | Jnc Corp | 太陽電池用封止材 |
EP2860766A4 (en) * | 2012-06-07 | 2016-02-10 | Mitsubishi Plastics Inc | SOLAR BATTERY MODULE AND METHOD FOR MANUFACTURING THE SAME |
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- 2011-07-28 CN CN201180040002.8A patent/CN103081121B/zh not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
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TWI538922B (zh) | 2016-06-21 |
RU2013114380A (ru) | 2014-10-10 |
CN103081121A (zh) | 2013-05-01 |
CN103081121B (zh) | 2016-06-08 |
TW201219423A (en) | 2012-05-16 |
CA2809757A1 (en) | 2012-03-08 |
MY165895A (en) | 2018-05-18 |
EP2613361A4 (en) | 2015-02-18 |
EP2613361A1 (en) | 2013-07-10 |
US20130213476A1 (en) | 2013-08-22 |
RU2592608C2 (ru) | 2016-07-27 |
KR20130111536A (ko) | 2013-10-10 |
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