CN110383407B - Laminate and method for manufacturing organic solar cell - Google Patents
Laminate and method for manufacturing organic solar cell Download PDFInfo
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- CN110383407B CN110383407B CN201880016442.1A CN201880016442A CN110383407B CN 110383407 B CN110383407 B CN 110383407B CN 201880016442 A CN201880016442 A CN 201880016442A CN 110383407 B CN110383407 B CN 110383407B
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- resin
- solar cell
- based adhesive
- organic solar
- laminate
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- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
-
- 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
- Y02E10/549—Organic PV cells
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Photovoltaic Devices (AREA)
- Hybrid Cells (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention provides a laminate and a method for manufacturing an organic solar cell using the laminate, wherein the laminate prevents the occurrence of an abnormality due to heating in the manufacturing process of the organic solar cell such as film formation, fixing, printing, bonding and the like when a resin film is used as a substrate, and the organic solar cell can be efficiently manufactured. The laminate comprises, in this order, a resin film as an organic solar cell substrate, a resin-based adhesive layer containing a resin-based adhesive, and a support, wherein the material of the support is any one selected from glass, plastic, and metal, and the mass reduction ratio of the resin-based adhesive layer before and after heating is 3 mass% or less when the resin-based adhesive layer is heated at 150 ℃ for 30 minutes. The method for manufacturing an organic solar cell uses the laminate.
Description
Technical Field
The present invention relates to a laminate and a method for manufacturing an organic solar cell.
Background
In recent years, organic solar cells such as dye-sensitized solar cells and perovskite solar cells have attracted attention as photoelectric conversion elements for converting light energy into electric energy.
A dye-sensitized solar cell generally includes a working electrode (photoelectrode), a counter electrode (counter electrode), a sensitizing dye layer supported on the working electrode, and an electrolyte layer disposed between the working electrode and the counter electrode.
The perovskite type solar cell generally has a working electrode (negative electrode), a counter electrode (positive electrode), a perovskite crystal layer, an electron collecting layer, and a hole collecting layer.
In a flexible organic solar cell, a resin film is used as a substrate constituting an electrode, but the resin film is poor in handling property and difficult to position, and causes a shift in patterning and bonding, which is a factor of lowering production efficiency.
To solve this problem, for example, patent document 1 proposes that the substrate for the working electrode is held on a carrier plate via an ionic liquid.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2010-153294.
Disclosure of Invention
Problems to be solved by the invention
However, as described in patent document 1, when the substrate for the working electrode is held on the transfer plate via the ionic liquid, not only the back surface of the substrate needs to be cleaned, but also there is a problem that peeling occurs during vacuum bonding.
In contrast, the present inventors have found that when a resin film as a substrate is held on a support using a resin-based adhesive layer containing a resin-based adhesive in place of an ionic liquid, the resin film is peeled from the support when heated in a step of film formation or the like.
Accordingly, an object of the present invention is to provide a laminate which can prevent the occurrence of an abnormality due to heating in an organic solar cell manufacturing process such as film formation, fixing, printing, and bonding when a resin film is used as a substrate, and can efficiently manufacture an organic solar cell, and a method for manufacturing an organic solar cell using the laminate.
Means for solving the problems
The laminate of the present invention comprises a resin film as an organic solar cell substrate, a resin-based adhesive layer containing a resin-based adhesive, and a support in this order, wherein the material of the support is any one selected from the group consisting of glass, plastic, and metal, and when the resin-based adhesive layer is heated at 150 ℃ for 30 minutes, the mass reduction rate of the resin-based adhesive layer before and after heating is 3% by mass or less. This prevents the occurrence of an abnormality due to heating in the organic solar cell production process when the resin film is used as the substrate, and enables efficient production of the organic solar cell.
In the laminate of the present invention, when the resin-based adhesive layer is immersed in a solvent selected from ethanol and acetonitrile at 40 ℃ for 120 minutes, the mass of the resin-based adhesive eluted from the solution is preferably 3% by mass or less relative to the mass of the resin-based adhesive before immersion. This prevents the resin film from coming off the support in the impregnation step, as well as prevents the occurrence of abnormalities due to heating in the respective steps.
In the laminate of the present invention, the resin-based adhesive layer preferably has a light transmittance of 40% or more at a wavelength of 400 nm.
The laminate of the present invention preferably has a thermal shock resistance temperature of the support of 70 ℃ or higher.
The method for manufacturing an organic solar cell of the present invention uses the laminate described in any one of the above. This prevents the occurrence of an abnormality due to heating in the organic solar cell production process when the resin film is used as the substrate, and enables efficient production of the organic solar cell.
Effects of the invention
According to the present invention, it is possible to provide a laminate which can prevent the occurrence of an abnormality due to heating in the organic solar cell production process when a resin film is used as a substrate, and which can efficiently produce an organic solar cell, and a method for producing an organic solar cell using the laminate.
Drawings
Fig. 1 is a schematic cross-sectional view of an example of the laminate of the present invention.
Detailed Description
Hereinafter, embodiments of the present invention will be described. These descriptions are for the purpose of illustrating the present invention and are not intended to limit the present invention in any way.
In this specification, unless otherwise stated, numerical ranges include the lower and upper limits of their ranges. For example, 2 to 80nm includes a lower limit of 2nm and an upper limit of 80nm, and means 2nm to 80 nm.
< organic solar cell >
Before describing the laminate of the present invention and the method for manufacturing an organic solar cell using the laminate, an example of the structure of a dye-sensitized solar cell, which is a typical organic solar cell, will be described.
A dye-sensitized solar cell typically has a photoelectrode (working electrode), a counter electrode (counter electrode), and an electrolyte layer. For example, refer to Japanese patent application laid-open No. 2014-120219. The dye-sensitized solar cell may have a known functional layer such as a protective layer, an antireflection layer, or a gas barrier layer on one or both of the photoelectrode and the counter electrode. Further, a known spacer for preventing short circuit may be provided.
The photoelectrode may be any electrode capable of releasing electrons to an external circuit by receiving light, and a known photoelectrode can be used as the photoelectrode of the dye-sensitized solar cell. The photoelectrode typically includes a photoelectrode substrate, a conductive film formed on the photoelectrode substrate, a porous semiconductor fine particle layer formed on the conductive film, and a sensitizing dye layer formed by a sensitizing dye adsorbed on the surface of the semiconductor fine particle layer.
The photoelectrode substrate plays a role of supporting a porous semiconductor fine particle layer and the like and a role of a current collector. Examples of the photoelectrode substrate include a photoelectrode substrate in which a conductive film is laminated on a resin film as a substrate, which will be described later.
As the substrate, a known substrate such as a resin film or glass can be used. Examples of the resin film include resin films obtained by molding a resin composition containing a synthetic resin such as polyethylene terephthalate (PET), polyethylene naphthalate (PEN), Syndiotactic Polystyrene (SPS), polyphenylene sulfide (PPS), Polycarbonate (PC), polyarylate (PAr), Polysulfone (PSF), Polyethersulfone (PES), Polyetherimide (PEI), transparent Polyimide (PI), or cycloolefin polymer (COP).
Examples of the material constituting the conductive film include metals such as platinum, gold, silver, copper, aluminum, iridium, and titanium; conductive metal oxides such as tin oxide and zinc oxide; and a composite metal oxide such as Indium Tin Oxide (ITO) or Indium Zinc Oxide (IZO).
The porous semiconductor fine particle layer is a porous layer containing semiconductor fine particles. Since the porous layer is used, the amount of the sensitizing dye adsorbed increases, and a dye-sensitized solar cell having high conversion efficiency can be easily obtained.
Examples of the semiconductor fine particles include particles of metal oxides such as titanium oxide, zinc oxide, and tin oxide. The particle diameter of the semiconductor fine particles (average particle diameter of primary particles) is preferably 2 to 80nm, more preferably 2 to 60 nm. The particle size is small, the surface area is large, the amount of the sensitizing dye supported is large, and the electrolytic solution constituting the electrolytic solution layer can diffuse to the fine portion of the porous semiconductor fine particle layer. From the viewpoint of dispersion stability, the solid content concentration of the semiconductor fine particle dispersion is 0.1 to 60 wt%, preferably 0.5 to 40 wt%, and more preferably 1.0 to 25 wt%.
The thickness of the porous semiconductor fine particle layer is not particularly limited, but is usually 0.1 to 50 μm, preferably 5 to 30 μm, and more preferably 15 μm or less.
Further, the porous semiconductor fine particle layer may be laminated by one layer or two or more layers. The semiconductor fine particles of these layers may have different particle diameters and compositions.
The sensitizing dye layer is a layer in which a compound (sensitizing dye) capable of transferring electrons to the porous semiconductor fine particle layer by being excited by light is adsorbed on the surface of the porous semiconductor fine particle layer.
Examples of the sensitizing dye include organic dyes such as cyanine dyes, merocyanine dyes, oxonol dyes, xanthene dyes, squarylium dyes, polymethine dyes, coumarin dyes, riboflavin dyes, perylene dyes, and the like; and metal complex dyes such as phthalocyanine complexes and porphyrin complexes of metals such as iron, copper and ruthenium. Two or more dyes may be used in combination. The solvent for dissolving the sensitizing dye is not particularly limited as long as it can dissolve the sensitizing dye and does not dissolve the porous semiconductor fine particle layer or does not react with the semiconductor fine particles. In the case where the solvent is composed of only an organic solvent, it is preferable to carry out degassing and distillation purification in advance in order to remove moisture and gas present in the solvent. Preferred examples of the solvent include alcohols, nitriles, halogenated hydrocarbons, ethers, amides, esters, carbonates, ketones, hydrocarbons, aromatics, and nitromethanes. As a preferred specific example of the solvent for dissolving the sensitizing dye in the present invention, particularly preferably used solvents include methanol, ethanol, isopropanol, 1-methoxy-2-propanol, N-butanol, t-butanol, butoxyethanol, N-dimethylformamide, N-methylpyrrolidone, methyl ethyl ketone, methyl isobutyl ketone, DMSO and the like. These solvents may be used alone, or a mixed solvent of 2 or more solvents may be used.
The concentration of the sensitizing dye in the dye solution is preferably 0.01 mM-10 mM, more preferably 0.1 mM-10 mM, still more preferably 0.5 mM-8 mM, and particularly preferably 0.8 mM-6 mM. Further, the total adsorption amount of the dye is preferably per unit surface area (1 m) of the conductive support2) Is 0.01M to 100M. The amount of dye adsorbed on the semiconductor fine particles is preferably in the range of 0.001 to 1M per 1g of the semiconductor fine particles.
In the present invention, it is preferable to use a material in combination with other materials (for example, a cationic compound (for example, a tertiary ammonium compound, a quaternary ammonium compound, a pyridine compound, an imidazole compound, an acid compound (for example, a carboxylic acid compound such as cholic acid or deoxycholic acid, a phosphoric acid compound, a phosphonic acid compound, a sulfonic acid compound, etc.) in addition to the sensitizing dye, and the concentration of these compounds in the dye solution is preferably 0.1mM to 100mM, more preferably 0.5mM to 50mM, particularly preferably 1.05mM to 50 mM., based on the molar equivalent of the dye, preferably 1 molar equivalent to 1000 molar equivalents, more preferably 5 molar equivalents to 500 molar equivalents, and particularly preferably 10 molar equivalents to 100 molar equivalents.
In addition, after the sensitizing dye is adsorbed to the porous semiconductor fine particle layer, it is preferable to wash with a solvent for removing an excessive sensitizing dye solution. In this case, it is recommended to use the aforementioned solvent as the cleaning solvent. As a cleaning method, a method of spraying a solvent onto the dye-sensitized porous semiconductor fine particle layer and washing it, or a method of immersing the substrate on which the dye-sensitized porous semiconductor fine particle layer is formed in a cleaning solvent tank, may be mentioned. The substrate having the dye-sensitized porous semiconductor fine particle layer formed thereon thus obtained is further subjected to a drying treatment, whereby a photoelectrode can be obtained. The drying conditions are not particularly limited, but preferably 0.5 to 30 minutes at 30 to 150 ℃, 0.5 to 15 minutes at 40 to 120 ℃, and 0.5 to 10 minutes at 50 to 100 ℃.
The counter electrode includes a counter electrode substrate and a conductive film on the counter electrode substrate. The conductive film may have a catalyst layer thereon.
The counter electrode substrate is the same as the resin film and glass used for the photoelectrode.
Examples of the material constituting the conductive film include metals such as platinum, gold, silver, copper, aluminum, iridium, and titanium; conductive metal oxides such as tin oxide and zinc oxide; complex metal oxides such as Indium Tin Oxide (ITO) and Indium Zinc Oxide (IZO); carbon materials such as graphene, carbon nanotubes, and fullerene.
As the catalyst layer, a known catalyst layer such as a conductive polymer such as platinum or Polythiophene (PEDOT), a carbon material such as carbon black, graphene, carbon nanotube, or fullerene can be used, and for example, a catalyst layer containing carbon nanotube (a) described in japanese patent application laid-open No. 2014-120219 can be mentioned.
The electrolyte layer is a layer for separating the photoelectrode from the counter electrode and efficiently transferring charges.
The electrolyte layer is not particularly limited, and examples thereof include an electrolytic solution, a gel electrolyte, and a solid electrolyte. For example, the electrolytic solution contains a supporting electrolyte, a redox couple (a pair of chemical substances that can reversibly convert each other in the form of an oxidizing agent and a reducing agent in a redox reaction), a solvent, and the like.
Examples of the supporting electrolyte include salts containing cations such as lithium ions, imidazole ions, and quaternary ammonium ions.
The redox couple may be any one that can reduce the oxidized sensitizing dye. Examples of the redox couple include chlorine compounds, iodine compounds, bromine compounds, thallium ions (iii) and thallium ions (i), ruthenium ions (iii) and ruthenium ions (ii), copper ions (ii) and copper ions (i), iron ions (iii) and iron ions (ii), cobalt ions (iii) and cobalt ions (ii), vanadium ions (iii) and vanadium ions (ii), manganate ions and permanganate ions, ferricyanide and ferrocyanide, quinone and hydroquinone, and fumaric acid and succinic acid.
As the solvent, a known solvent for forming an electrolyte layer of a solar cell can be used. Examples of the solvent include acetonitrile, methoxyacetonitrile, 3-methoxypropionitrile, N-dimethylformamide, ethylmethylimidazole bistrifluoromethanesulfonimide, γ -butyrolactone, and propylene carbonate.
The organic solar cell may be a perovskite solar cell, in addition to the dye-sensitized solar cell. Perovskite-type solar cells typically have a perovskite crystalline layer between a working electrode and a counter electrode. Further, the perovskite crystal layer may be interposed between a hole collecting layer and an electron collecting layer. Examples of perovskite-type solar cells include perovskite-type solar cells described in, for example, japanese patent laid-open nos. 2014-049631, 2015-046583, 2016-009737, and the like.
(laminated body)
The laminate of the present invention comprises a resin film as an organic solar cell substrate, a resin-based adhesive layer containing a resin-based adhesive, and a support in this order, wherein the material of the support is any one selected from the group consisting of glass, plastic, and metal, and when the resin-based adhesive layer is heated at 150 ℃ for 30 minutes, the mass reduction rate of the resin-based adhesive layer before and after heating is 3 mass% or less. This prevents the occurrence of an abnormality due to heating in the organic solar cell production process when the resin film is used as the substrate, and enables efficient production of the organic solar cell.
The present inventors have studied and found that when a structure obtained by bonding a support and a resin film using a resin-based adhesive layer is heated, gas (gas) dissolved in the resin-based adhesive foams, whereby the bonding between the support and the resin film deteriorates, and the resin film comes off, which leads to an abnormality (for example, positioning is difficult, displacement occurs during patterning and bonding, and the production efficiency is lowered) in the production process of an organic solar cell. The present inventors have further studied and found that when the resin adhesive layer is heated at 150 ℃ for 30 minutes, the mass reduction ratio of the resin adhesive layer before and after heating is 3 mass% or less, and thus the resin film can be prevented from falling off due to heating.
In the present invention, the mass reduction ratio of the resin-based adhesive layer by heating, that is, the mass of the resin-based adhesive layer before heating is M1 and the mass of the resin-based adhesive layer after heating is M2, (M1-M2) × 100/M1 is 3 mass% or less (0 to 3 mass%). This proportion is preferably 2.4% by mass or less and 2.3% by mass or less, and more preferably 1% by mass or less and 0.6% by mass or less.
In the present invention, the mass reduction ratio of the resin-based adhesive layer due to heating was determined by the measurement method described in the examples.
Fig. 1 is a schematic diagram showing an example of a cross section of a laminate. The laminate 1 shown in fig. 1 includes a resin film 30, a resinous adhesive layer 20, and a support 10 in this order.
< support >
The material of the support is selected from any one of glass, plastic and metal. The support may be subjected to surface treatment or the like.
Examples of the glass as a material of the support include borosilicate glass, silicate glass, silica glass, alkali-free glass, and quartz glass.
Examples of the plastic material of the support include acrylic plastic, polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polytrimethylene terephthalate (PTT), polyethylene naphthalate (PEN), polyesters such as liquid crystal polyester, polyolefins such as Polyethylene (PE), polypropylene (PP), polybutylene, and polymethylpentene (PMP), cyclic olefin polymers such as cyclic olefin polymers (COP and COC), styrene resins, Polyoxymethylene (POM), Polyamide (PA), Polycarbonate (PC), polymethyl methacrylate (PMMA), polyvinyl chloride (PVC), Polyphenylene Sulfide (PPs), polyphenylene ether (PPE), modified PPE, Polyimide (PI), Polyamideimide (PAI), Polyetherimide (PEI), Polysulfone (PSU), polyethersulfone, Polyketone (PK), Polyetherketone (PEK), Polyetheretherketone (PEEK), and the like, Polyether ketone (PEKK), Polyarylate (PAR), polyether nitrile, phenol-based resin, phenoxy resin, fluorine-based resin such as polytetrafluoroethylene, and the like. The support is preferably high in heat resistance and transparency. Preferably borosilicate glass or quartz glass.
Examples of the metal as a material of the support include stainless steel, iron, aluminum, brass, and copper.
The thickness of the support body may be set to, for example, 0.5 to 10 mm.
The support preferably has a thermal shock resistance temperature of 70 ℃ or higher. Thereby, it is possible to prevent the occurrence of abnormality due to heating in each step. In the present invention, the thermal shock resistance temperature of the support is determined by measuring the critical temperature at which the support is broken when the temperature is rapidly cooled from each temperature to 0 ℃.
< resin-based adhesive layer >
The resin-based adhesive layer contains a resin-based adhesive. A known resin-based adhesive can be used as the resin-based adhesive. The resin adhesive layer may or may not have a base material. The light transmittance of the resin adhesive layer including the base material is preferably 40% or more, and more preferably 60% or more, at a wavelength of 400nm, regardless of the presence or absence of the base material.
Examples of the substrate of the resin-based adhesive layer include transparent substrates such as polyester such as polyethylene terephthalate, transparent polyimide, cycloolefin polymer (COP, COC), and thin film glass such as polymethylpentene. Particularly, it is preferable that the composition has excellent heat resistance and transparency.
In the laminate of the present invention, when the resin-based adhesive layer is immersed in a solvent containing 1 or more selected from ethanol, n-butanol, t-butanol, dimethyl sulfoxide (DMSO), dimethylformamide, and acetonitrile at 40 ℃ for 120 minutes, the mass of the resin-based adhesive that has eluted into the solution is preferably 3% by mass or less, more preferably 2.5% by mass or less, and still more preferably 1.5% by mass or less, relative to the mass of the resin-based adhesive before immersion. This prevents the occurrence of an abnormality due to heating in the production process of the organic solar cell, and also prevents the resin-based adhesive layer from being reduced in adhesive force during impregnation, thereby preventing the resin film from falling off the support during the impregnation process. The solvent used in the impregnation treatment is preferably the above-mentioned group, and the solvent used in the sensitizing dye production step may be used in the impregnation treatment as long as the resin-based adhesive layer of the present invention satisfies the above-mentioned elution conditions. Examples of the solvent include alcohols, nitriles, halogenated hydrocarbons, ethers, amides, esters, carbonates, ketones, hydrocarbons, aromatics, nitromethanes, and the like, and preferable specific examples thereof include methanol, ethanol, isopropanol, 1-methoxy-2-propanol, N-butanol, t-butanol, butoxyethanol, N-dimethylformamide, N-methylpyrrolidone, methyl ethyl ketone, methyl isobutyl ketone toluene, DMSO, and the like. These solvents may be used alone, or a mixed solvent of 2 or more solvents may be used.
In the present invention, the mass of the resin-based adhesive layer eluted in the solvent with respect to the mass of the resin-based adhesive layer before impregnation was determined using the measurement method described in the examples.
The resin-based adhesive is preferably at least 1 selected from the group consisting of silicone resin-based adhesives, acrylic resin-based adhesives, urea resin-based adhesives, melamine resin-based adhesives, phenol resin-based adhesives, vinyl acetate resin-based solvent-based adhesives, natural rubber-based solvent-based adhesives, vinyl acetate resin-based emulsion-based adhesives, vinyl acetate copolymer resin-based emulsion-based adhesives, EVA (ethylene-vinyl acetate copolymer) resin-based emulsion-based adhesives, isocyanate-based adhesives, synthetic rubber-based emulsion-based adhesives, epoxy resin-based adhesives, cyanoacrylate-based adhesives, and polyurethane-based adhesives.
In one embodiment, the resin-based adhesive is 1 or more selected from a silicone resin-based adhesive, an acrylic resin-based adhesive, and a rubber-based adhesive.
The resin-based adhesive is preferably a resin-based adhesive in which, after the laminate of the present invention is used or after the organic solar cell is produced by the production method of the present invention described below, the peeling strength of the laminate is reduced by irradiation with electromagnetic waves such as ultraviolet rays, electron beams, and radiation due to a temperature change such as heating and cooling in a peeling step (step of peeling off the support) provided as needed. These may be one kind alone, or two or more kinds may be combined. In this peeling step, the adhesive layer is heated and cooled, and irradiated with electromagnetic waves such as ultraviolet rays, electron beams, or rays, whereby the peeling strength can be reduced, and the organic solar cell or the resin film on which the electrode is formed can be more easily peeled from the support. Examples of such resin-based adhesives include an easily releasable adhesive sheet described in japanese patent laid-open nos. 2012 and 102212 and a cooling-releasable adhesive composition described in japanese patent laid-open No. 2013 and 209667, and specifically include a heat-sensitive adhesive sheet (temperature-controlled Tape (Intelimer Tape) manufactured by indian corporation and a somatalum-made SOMATAC (registered trademark) UV. In the peeling step, the stimulus may be applied at a proper timing according to the adhesive, and for example, in the case of a thermosensitive sheet, the temperature may be applied at a temperature of 0.01 to 10 hours-20 to 200 ℃, and in the case of an electromagnetic wave-peelable sheet, the electromagnetic wave containing a desired wavelength may be applied at a proper timing for 0.01 to 10 hours.
The resin-based adhesive layer formed of the resin-based adhesive may be 1 layer or 2 or more layers. In the case of 2 or more layers, the layers may be the same or different from each other.
The thickness of the resin-based adhesive layer is not particularly limited, but is, for example, preferably 1 to 150. mu.m, more preferably 1 to 100. mu.m, and still more preferably 1 to 50 μm.
< resin film >
The resin film is a member to be a substrate of the organic solar cell, such as a working electrode and a counter electrode. In the dye-sensitized solar cell, one or both of the photoelectrode substrate and the counter electrode substrate is preferably a resin film.
As the resin film, a known resin film can be used. Examples of the resin film include resin films obtained by molding a resin composition containing a synthetic resin such as polyethylene terephthalate (PET), polyethylene naphthalate (PEN), Syndiotactic Polystyrene (SPS), polyphenylene sulfide (PPS), Polycarbonate (PC), polyarylate (PAr), Polysulfone (PSF), Polyethersulfone (PES), Polyetherimide (PEI), transparent Polyimide (PI), cycloolefin polymer (COP), and polymethylpentene (PMP).
The light transmittance of the resin film at a wavelength of 400nm is preferably 40% or more, more preferably 70% or more.
The thickness of the resin film may be appropriately adjusted depending on the application. For example, 10 to 10000 μm.
The laminate may have the conductive film on the surface of the resin film.
The method of forming the laminate is not particularly limited as long as it is a method capable of obtaining a laminate having a structure of at least 3 layers including a resin film, a resin-based adhesive layer, and a support in this order as shown in fig. 1, and the method may be appropriately selected from coating, bonding, and the like. When the resin binder layer is formed by applying a resin binder, the method is not particularly limited, and a known printing method can be used. Examples thereof include spin coating, dip coating, air knife coating, shower coating, roll coating, wire bar coating, gravure coating, extrusion coating using a hopper, and multilayer simultaneous coating. In the case where the resin-based adhesive layer is formed by bonding, for example, the resin-based adhesive layer can be bonded to the support or the resin film by using a bonding apparatus.
(method for manufacturing organic solar cell)
The method for manufacturing an organic solar cell of the present invention uses the laminate described in any one of the above. This prevents the occurrence of an abnormality due to heating in the organic solar cell production process when the resin film is used as the substrate, and enables efficient production of the organic solar cell.
The method for producing an organic solar cell of the present invention is not particularly limited except for using the laminate, and a known method for producing an organic solar cell can be employed. That is, in the conventional method for manufacturing an organic solar cell, in the step of using a resin film as a substrate, the laminate of the present invention is used instead of a resin film alone, and various steps such as film formation, fixing, printing, and bonding may be performed.
Hereinafter, a method for manufacturing an organic solar cell will be described with reference to a dye-sensitized solar cell having a photoelectrode (working electrode), a counter electrode (counter electrode), and an electrolyte layer, as an example.
Examples of the steps of the method for producing an organic solar cell include a photoelectrode production step such as a step of forming a conductive film on a photoelectrode substrate, a step of forming a porous semiconductor fine particle layer on the conductive film on the photoelectrode substrate, and a step of forming a sensitizing dye layer on the porous semiconductor fine particle layer; a counter electrode manufacturing step such as a step of forming a conductive film on a counter electrode substrate, a step of forming a catalyst layer on the conductive film on the counter electrode substrate, and the like; a step of applying a sealing agent composition to the photoelectrode and/or the counter electrode, and curing the composition by irradiation with energy rays to form a sealing agent; a general process of a known method for manufacturing an organic solar cell, such as a process of disposing an electrolyte layer between a photoelectrode and a counter electrode. For example, refer to Japanese patent application laid-open No. 2014-120219.
The conductive film can be formed by forming a film on the photoelectrode substrate or the counter electrode substrate by a known method such as a sputtering method, a coating method, a vapor deposition method, a spray pyrolysis method, or a Chemical Vapor Deposition (CVD) method. CO may also be used2And YAG or the like, and the conductive film is processed to form a conductive pattern.
The porous semiconductor fine particle layer can be formed by using a known method such as a pressing method, a hydrothermal decomposition method, an electrophoretic deposition method, a binderless coating method, and an Aerosol Deposition (AD) method. For example, a porous semiconductor fine particle layer can be formed by applying a titanium oxide paste by screen printing or a Baker's coater (Baker Applicator), drying the coating film at normal temperature, and then drying the coating film by heating in a constant temperature layer of 150 ℃.
The sensitizing dye layer can be formed using, for example, a method of immersing the porous semiconductor microparticle layer in a sensitizing dye solution, a method of coating the sensitizing dye solution on the porous semiconductor microparticle layer, or the like. In the method of immersion, the porous semiconductor fine particle layer can be immersed in, for example, an ethanol solution containing a dye, thereby forming a sensitizing dye layer.
The catalyst layer can be formed by a known method. For example, in a catalyst layer containing carbon nanotubes (a) as described in japanese patent application laid-open No. 2014-120219, a dispersion containing carbon nanotubes (a) can be prepared, the dispersion is applied to a conductive film on a counter electrode substrate, and the obtained coating film is dried.
The electrolyte layer can be formed by applying a solution (electrolyte solution) containing the constituent components to the photoelectrode or by forming a cell having the photoelectrode and the counter electrode and injecting the electrolyte solution into the gap therebetween.
As the energy ray for curing the sealant, an energy ray such as ultraviolet ray, visible light, infrared ray, or electron beam can be used. Among them, ultraviolet rays and electron beams are preferable.
As the ultraviolet irradiation device, a light source having light in a range of 200 to 500nm, for example, an ultraviolet irradiation device having a high-pressure mercury lamp, an ultrahigh-pressure mercury lamp, a metal halide lamp, a gallium lamp, a xenon lamp, a carbon arc lamp, or the like can be generally used. On the other hand, when curing is performed by using an electron beam, an electron beam accelerator having an energy of 100 to 500eV can be generally used.
The curing conditions and the like may be performed under known conditions which are generally performed. The cumulative dose of the energy rays is usually 100 to 5000mJ/cm2Preferably 200 to 4000mJ/cm2。
The method of applying the sealant composition is not particularly limited, and methods such as flexographic printing, gravure printing, screen printing, inkjet printing, offset printing, or bar coating, dip coating, flow coating, spray coating, spin coating, roll coating, reverse coating, air knife coating, and dispensing can be used.
The organic solar cell module is not particularly limited in structure, and may be of a Z-type, W-type, parallel-type, collector array type, monolithic type, or the like. One or more of these modules may be combined to be connected in series or in parallel, and a plurality of these modules may be connected. In addition, current collecting electrodes, extraction electrodes, and the like may be fabricated in the module using known means. The connection method may be any known method as long as solder, a metal plate, a cable, a flat cable, a flexible base material, or the like is appropriately selected.
The method of assembling the module is not particularly limited, and the module can be manufactured by a known method such as a vacuum bonding method (One Drop Fill method: ODF method) or an end sealing method. Examples of the ODF method include the method described in international publication No. 2007/046499. As the end sealing method, for example, a method described in japanese patent application laid-open No. 2006-004827 is cited.
The ultraviolet shielding layer, the oxygen/water shielding layer, the antireflection layer, the antifouling layer, the hard coat layer, the reinforcing member, and the like may be provided around the other module or on the outer surface in a timely manner. These may be formed by any known method such as vapor deposition, coating, or sheet-like material deposition.
Examples
The present invention will be described in further detail below with reference to examples, which are intended to illustrate the present invention and are not intended to limit the present invention in any way. Unless otherwise specified, the amount to be blended represents parts by mass.
The support, resin-based adhesive, resin film, and UV curable resin used in the examples are as follows.
(support body)
Borosilicate glass: the product name TEMPAX glass (thickness 3mm) manufactured by Schottky corporation, heat shock resistance temperature 180 DEG C
(resin binder)
Silicone resin-based binder 1: silicone rubber double-sided tape 9030W (114 μm thick) manufactured by Temple corporation and 87% transmittance at wavelength of 400nm
Acrylic resin-based binder: double-sided adhesive tape 9014 (thickness 100 μm) manufactured by Temple corporation, transmittance 88% at wavelength of 400nm
Silicone resin-based binder 2: polyimide double-sided silica gel tape 4309 (110 μ M thick) manufactured by 3M corporation, light transmittance at wavelength of 400nm of 0.02%
Rubber-based adhesive: 3M double-sided adhesive tape, light transmittance at wavelength of 400nm of 1.1%
Comparative acrylic resin-based binder: acrylic double-sided tape (thickness 100 μm) manufactured by NICIBAN corporation, transmittance at wavelength of 400nm of 11%
Comparative polyvinyl alcohol resin-based binder: PVA binder (200 μm thick) manufactured by YAMATO corporation, transmittance at wavelength of 400nm of 82%
(resin film)
A resin film of an ITO film of 300nm was coated on the surface of a PEN film of 300mm in length, 210mm in width and 125 μm in thickness.
(UV curing resin)
UV curing resin: liquid polyisobutylene sealing material
Examples 1 to 4 and comparative examples 1 to 2
Using the resin-based adhesive shown in table 1, a resin film (PEN film having an ITO film) was disposed by applying the resin-based adhesive to a support, thereby forming a laminate. From the resulting laminate, 2 test pieces having dimensions of 50mm × 50mm were obtained.
< Heat test >
1 of the test pieces was left standing in a dryer at a temperature of 150 ℃ for 30 minutes. The mass reduction ratio of the resin-based adhesive layer before and after heating was calculated. The results are shown in Table 1.
< dissolution test >
The remaining 1 of the test pieces was measured at every 1cm2The sheet was immersed in a solvent (ethanol) at 40 ℃ for 120 minutes at a bath ratio of 2mL in surface area. Then, the vessel containing the solvent was allowed to stand in a reduced pressure drier (100Pa) at 150 ℃ for 1 hour. The mass of the substance (component of the resin-based adhesive layer dissolved in the solvent) remaining in the vessel after drying was measured. Then, the mass ratio of the resin-based adhesive layer eluted in the solvent to the mass of the resin-based adhesive layer before impregnation was calculated. The results are shown in Table 1.
[ Table 1]
Using the obtained laminate, an organic solar cell was produced through the following steps of organic solar cell production.
(1) Fabrication of photoelectrode
< Process for Forming porous conductor Fine particle layer (heating Process) >
An adhesive-free titanium dioxide paste (PECC-C01-06, manufactured by Peccell Technologies) was applied to the ITO surface of the laminate using a Becker coater. The obtained coating film was dried at room temperature for 10 minutes, and then further dried by heating in a constant temperature layer at 150 ℃ for 5 minutes to form a porous semiconductor fine particle layer of 7 μm.
< Process for Forming sensitizing dye layer (immersion Process) >
Dissolving the laminate with the porous semiconductor fine particle layer in a sensitizing dye at a concentration of 3X 10-1The resulting dye solution (sensitizing dye: ruthenium complex (N719, Solaronix Co., Ltd.) and solvent: ethanol) was immersed at 40 ℃ for 120 minutes to form a sensitizing dye layer.
(2) Fabrication of counter electrode
A platinum nano colloidal solution (made of a noble metal in the field) was applied on the ITO surface of the laminate by a bar coating method, and dried. Thereafter, the platinum catalyst was fixed by treatment with heated water vapor (100 ℃ C., 5 minutes), thereby forming a catalyst layer.
(3) Preparation of the electrolyte
The above components were dissolved in methoxyacetonitrile to obtain an electrolyte solution so that the concentrations of the components reached 0.05mol/L of iodine, 0.1mol/L of lithium iodide, 0.5mol/L of t-butylpyridine and 0.6mol/L of 1, 2-dimethyl-3-propylimidazolium iodide.
< step of Forming sealing agent (UV curing step) >
After a UV-curable resin as a sealant composition was drawn on a laminate having a sensitizing dye layer formed on a porous semiconductor fine particle layer by a dispensing method, an electrolytic solution was applied on the porous semiconductor fine particle layer, the prepared photoelectrode and a counter electrode were bonded under vacuum using an automatic bonding apparatus, and the UV-curable resin was cured by irradiating 100mW of metal halide lamp light from the photoelectrode side for 60 seconds, thereby forming a sealant.
The heating step, the dipping step, and the UV curing step were evaluated for the peeling of the resin film by the following criteria.
(evaluation criteria of heating step)
Evaluation A: the resin film does not fall off from the support
Evaluation B: the resin film is released from the support
(evaluation criteria for dipping step)
Evaluation A: the resin film does not fall off from the support
Evaluation B: at least 1 end of the resin film was peeled off from the support by about 5 mm.
Evaluation C: the resin film is entirely peeled off from the support
(evaluation criteria for UV curing step)
Evaluation A: curing the UV-curable resin, and bonding the photoelectrode and the counter electrode
Evaluation B: the UV-curable resin is not cured, and the photoelectrode and the counter electrode are immediately peeled off after the UV-curing process
As shown in table 1, in the examples in which the mass reduction ratio of the resin binder layer in the heating test was 3 mass% or less, the occurrence of an abnormality (falling-off) in the heating step was prevented, and the organic solar cell was efficiently produced. Further, in example 1 in which the mass ratio of the resin-based adhesive layer eluted in the solvent in the immersion test was 3 mass% or less, it was possible to prevent not only the occurrence of an abnormality due to heating but also the detachment of the resin film from the support in the immersion step.
Industrial applicability
According to the present invention, it is possible to provide a laminate which can prevent an abnormality from occurring in an organic solar cell manufacturing process when a resin film is used as a substrate, and which can efficiently manufacture an organic solar cell, and a method for manufacturing an organic solar cell using the laminate.
Description of the reference numerals
1: laminated body
10: support body
20: resin-based adhesive layer
30: resin film
Claims (4)
1. A laminate comprising, in order, a resin film as an organic solar cell substrate, a resin binder layer containing a resin binder, and a support,
the material of the support is selected from any one of glass, plastic and metal,
when the resin-based adhesive layer is heated at 150 ℃ for 30 minutes, the mass reduction ratio of the resin-based adhesive layer before and after heating is 3 mass% or less,
when the resin-based adhesive layer is immersed in a solvent containing 1 or more selected from ethanol, n-butanol, t-butanol, dimethyl sulfoxide, dimethylformamide and acetonitrile at 40 ℃ for 120 minutes, the mass of the resin-based adhesive layer eluted in the solvent is 3 mass% or less relative to the mass of the resin-based adhesive layer before immersion.
2. The laminate according to claim 1, wherein the resin-based adhesive layer has a light transmittance of 40% or more at a wavelength of 400 nm.
3. The laminate according to claim 1 or 2, wherein the support has a thermal shock resistance temperature of 70 ℃ or higher.
4. A method for manufacturing an organic solar cell, using the laminate according to any one of claims 1 to 3.
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| JP2017-065657 | 2017-03-29 | ||
| JP2017065657 | 2017-03-29 | ||
| PCT/JP2018/012555 WO2018181388A1 (en) | 2017-03-29 | 2018-03-27 | Laminate and manufacturing method of organic solar battery |
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| CN110383407A CN110383407A (en) | 2019-10-25 |
| CN110383407B true CN110383407B (en) | 2021-10-08 |
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| JP (1) | JP7264047B2 (en) |
| CN (1) | CN110383407B (en) |
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| JP2008150694A (en) * | 2006-12-20 | 2008-07-03 | Dainippon Screen Mfg Co Ltd | Plating system, plating method, and manufacturing system and manufacturing method for dye-sensitized solar cell |
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| JP2015088715A (en) | 2013-09-25 | 2015-05-07 | 富士フイルム株式会社 | Method of manufacturing organic thin-film transistor and organic thin-film transistor |
| JP2015085568A (en) | 2013-10-30 | 2015-05-07 | 株式会社リコー | Image recording method and image recording apparatus |
| JP6447389B2 (en) | 2014-10-27 | 2019-01-09 | 三菱ケミカル株式会社 | Laminate with resin / glass composite |
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2018
- 2018-03-27 WO PCT/JP2018/012555 patent/WO2018181388A1/en active Application Filing
- 2018-03-27 JP JP2019509931A patent/JP7264047B2/en active Active
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| CN103429694A (en) * | 2011-03-11 | 2013-12-04 | Dic株式会社 | Heat sealant, and laminate and solar-cell module using same |
| CN103725214A (en) * | 2012-10-11 | 2014-04-16 | 日东电工株式会社 | Laminate |
| CN104918969A (en) * | 2012-12-17 | 2015-09-16 | 株式会社可乐丽 | Rubber-containing graft polymer powder, and laminated-glass interlayer and solar-cell sealing material including same |
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| TW201903797A (en) | 2019-01-16 |
| CN110383407A (en) | 2019-10-25 |
| WO2018181388A1 (en) | 2018-10-04 |
| JPWO2018181388A1 (en) | 2020-02-06 |
| JP7264047B2 (en) | 2023-04-25 |
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