WO2015001984A1 - 光電変換素子モジュールおよびその製造方法 - Google Patents
光電変換素子モジュールおよびその製造方法 Download PDFInfo
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- WO2015001984A1 WO2015001984A1 PCT/JP2014/066358 JP2014066358W WO2015001984A1 WO 2015001984 A1 WO2015001984 A1 WO 2015001984A1 JP 2014066358 W JP2014066358 W JP 2014066358W WO 2015001984 A1 WO2015001984 A1 WO 2015001984A1
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- photoelectric conversion
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- conversion element
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- 229940063789 zinc sulfide Drugs 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Classifications
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- 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
- H01G9/2004—Light-sensitive devices characterised by the electrolyte, e.g. comprising an organic electrolyte
- H01G9/2018—Light-sensitive devices characterised by the electrolyte, e.g. comprising an organic electrolyte characterised by the ionic charge transport species, e.g. redox shuttles
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B23/00—Methine or polymethine dyes, e.g. cyanine dyes
- C09B23/0008—Methine or polymethine dyes, e.g. cyanine dyes substituted on the polymethine chain
- C09B23/005—Methine or polymethine dyes, e.g. cyanine dyes substituted on the polymethine chain the substituent being a COOH and/or a functional derivative thereof
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- C09B23/00—Methine or polymethine dyes, e.g. cyanine dyes
- C09B23/0008—Methine or polymethine dyes, e.g. cyanine dyes substituted on the polymethine chain
- C09B23/005—Methine or polymethine dyes, e.g. cyanine dyes substituted on the polymethine chain the substituent being a COOH and/or a functional derivative thereof
- C09B23/0058—Methine or polymethine dyes, e.g. cyanine dyes substituted on the polymethine chain the substituent being a COOH and/or a functional derivative thereof the substituent being CN
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- C09B23/00—Methine or polymethine dyes, e.g. cyanine dyes
- C09B23/0066—Methine or polymethine dyes, e.g. cyanine dyes the polymethine chain being part of a carbocyclic ring,(e.g. benzene, naphtalene, cyclohexene, cyclobutenene-quadratic acid)
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- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B23/00—Methine or polymethine dyes, e.g. cyanine dyes
- C09B23/02—Methine or polymethine dyes, e.g. cyanine dyes the polymethine chain containing an odd number of >CH- or >C[alkyl]- groups
- C09B23/04—Methine or polymethine dyes, e.g. cyanine dyes the polymethine chain containing an odd number of >CH- or >C[alkyl]- groups one >CH- group, e.g. cyanines, isocyanines, pseudocyanines
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B23/00—Methine or polymethine dyes, e.g. cyanine dyes
- C09B23/10—The polymethine chain containing an even number of >CH- groups
- C09B23/105—The polymethine chain containing an even number of >CH- groups two >CH- groups
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- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B23/00—Methine or polymethine dyes, e.g. cyanine dyes
- C09B23/14—Styryl dyes
- C09B23/145—Styryl dyes the ethylene chain carrying an heterocyclic residue, e.g. heterocycle-CH=CH-C6H5
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09B23/00—Methine or polymethine dyes, e.g. cyanine dyes
- C09B23/14—Styryl dyes
- C09B23/148—Stilbene dyes containing the moiety -C6H5-CH=CH-C6H5
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B5/00—Dyes with an anthracene nucleus condensed with one or more heterocyclic rings with or without carbocyclic rings
- C09B5/62—Cyclic imides or amidines of peri-dicarboxylic acids of the anthracene, benzanthrene, or perylene series
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B57/00—Other synthetic dyes of known constitution
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B57/00—Other synthetic dyes of known constitution
- C09B57/008—Triarylamine dyes containing no other chromophores
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- 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
- H01G9/2059—Light-sensitive devices comprising an organic dye as the active light absorbing material, e.g. adsorbed on an electrode or dissolved in solution
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- 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
- H01G9/2068—Panels or arrays of photoelectrochemical cells, e.g. photovoltaic modules based on photoelectrochemical cells
- H01G9/2081—Serial interconnection of cells
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K39/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic radiation-sensitive element covered by group H10K30/00
- H10K39/10—Organic photovoltaic [PV] modules; Arrays of single organic PV cells
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K39/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic radiation-sensitive element covered by group H10K30/00
- H10K39/10—Organic photovoltaic [PV] modules; Arrays of single organic PV cells
- H10K39/12—Electrical configurations of PV cells, e.g. series connections or parallel connections
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
- H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
- H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/60—Organic compounds having low molecular weight
- H10K85/649—Aromatic compounds comprising a hetero atom
- H10K85/652—Cyanine dyes
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
- H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/60—Organic compounds having low molecular weight
- H10K85/631—Amine compounds having at least two aryl rest on at least one amine-nitrogen atom, e.g. triphenylamine
- H10K85/636—Amine compounds having at least two aryl rest on at least one amine-nitrogen atom, e.g. triphenylamine comprising heteroaromatic hydrocarbons as substituents on the nitrogen atom
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/60—Organic compounds having low molecular weight
- H10K85/649—Aromatic compounds comprising a hetero atom
- H10K85/655—Aromatic compounds comprising a hetero atom comprising only sulfur as heteroatom
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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
- Y02E10/542—Dye sensitized solar cells
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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
- 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
Definitions
- the present invention relates to a photoelectric conversion element module and a manufacturing method thereof.
- the general configuration of such a dye-sensitized solar cell is that a substrate, a first electrode, a semiconductor layer (photoelectric conversion layer) carrying a sensitizing dye, a hole transport layer, and a second electrode are sequentially laminated. It is a thing.
- a technology of the dye-sensitized solar cell International Publication No. 2005/078853 can be cited.
- a second electrode carrying platinum on a transparent conductive glass plate coated with fluorine-doped tin oxide is used as a counter electrode for electrolysis, and a predetermined size is provided at the center of the electrode surface.
- a photoelectric conversion element having a polymer film formed thereon and a manufacturing method thereof, and a photoelectric conversion element in which a liquid electrolyte is impregnated in the aniline electropolymerization film and a manufacturing method thereof are disclosed.
- a dye-sensitized solar cell when a dye-sensitized solar cell is actually used, it is generally a module unit in which a plurality of solar cells having the above-described configuration are combined (see, for example, JP-A-2013-12366).
- the hole transport layer in the dye-sensitized solar cell is formed by electrolytic polymerization in International Publication No. 2005/078853, and in Japanese Patent Application Laid-Open No. 2003-142168, photoelectrolytic polymerization (photoelectrochemical oxidation polymerization) is used. Forming.
- the electropolymerization method is often employed as one method for synthesizing a conductive polymer. When a voltage is applied by immersing an electrode pair in a solution in which the monomer and the supporting electrolyte are dissolved, the monomer is removed from the electrode surface. In this method, a polymer is formed by oxidation or reduction.
- electrolytic polymerization is used as a method for forming the hole transport layer from the viewpoint that pn control can be performed because counter ions in the solution can be taken in on the electrode by electrochemical doping. Adopted.
- the present inventors provide a photoelectric conversion element module capable of exhibiting sufficient power generation performance even in the form of a dye-sensitized solar cell module and a method for manufacturing the photoelectric conversion element module The purpose is to do.
- the inventors of the present application previously conducted extensive studies to improve the durability of the photoelectric conversion element.
- the polymerization of the conductive polymer precursor during the formation of the hole transport layer was performed in the presence of an oxidizing agent.
- a uniform hole transport layer can be formed by contacting the conversion layer with the conductive polymer precursor and then irradiating the sensitizing dye with light, thereby improving the durability of the photoelectric conversion element.
- the present inventors have found that a module formed by electrically connecting two or more of the photoelectric conversion elements can exhibit excellent power generation performance. Completed.
- the present invention is a photoelectric conversion element laminated in the order of a substrate, a first electrode, a semiconductor and a photoelectric conversion layer containing a sensitizing dye, a hole transport layer having a conductive polymer, and a second electrode,
- the hole transport layer polymerizes the conductive polymer precursor by irradiating the sensitizing dye with light after contacting the photoelectric conversion layer and the conductive polymer precursor in the presence of an oxidizing agent.
- the above object can be achieved by a photoelectric conversion element module formed by doing so.
- FIG. 1 10 is a photoelectric conversion element; 20 is a substrate; 30 is a first electrode; 31 is an end (connection portion with the second electrode); 40 is a buffer layer; and 50 is a photoelectric conversion layer.
- 60 is a hole transport layer; 70 is a second electrode; 71 is an end (connection portion with the first electrode); 8 is light; 100 is a photoelectric conversion element module; X is between the first electrodes Represents the distance of each.
- the 1st of this invention is the photoelectric conversion element laminated
- the hole transport layer contacts the photoelectric conversion layer and the conductive polymer precursor in the presence of an oxidizing agent, and then the sensitizing dye
- the present invention relates to a photoelectric conversion element module formed by polymerizing the conductive polymer precursor by irradiating light.
- the photoelectric conversion element module forms a hole transport layer by photochemical polymerization after contacting the photoelectric conversion layer with a solution containing a conductive polymer precursor and an oxidizing agent. Therefore, it has a uniform hole transport layer as compared with the conventional hole transport layer formed by (photo) electropolymerization, and an element with high power generation performance can be produced.
- the hole transport layer was formed by electropolymerization such as photoelectropolymerization, but it was difficult to obtain a uniform polymerized film, and there was a problem in light durability of the photoelectric conversion element.
- photochemical polymerization of an oxidative polymerizable monomer using an oxidant and a photosensitizer is also known (for example, JP-A-1-123228 and JP-A-2009-16582).
- JP-A-1-123228 and JP-A-2009-16582 since the molar ratio of the oxidizing agent to the monomer is small and the reactivity is low, it is difficult to form a sufficient film required for a photoelectric conversion element, particularly a photoelectric conversion element for a dye-sensitized solar cell.
- the sensitizing dye is excited by light irradiation, and the excited electrons are consumed by an oxidizing agent (for example, hydrogen peroxide).
- an oxidizing agent for example, hydrogen peroxide
- the sensitizing dye becomes a cationic state
- the sensitizing dye in the cationic state extracts electrons from the conductive polymer precursor
- the conductive polymer precursor becomes a cationic state.
- Polymerization is started when the conductive polymer precursor in the cationic state is triggered.
- the cationic state is increased by mixing the oxidizing agent and the conductive polymer precursor in such a ratio that the oxidizing agent is present at a high concentration with respect to the conductive polymer precursor.
- the polymerization can be started more quickly with the conductive polymer precursor in a cationic state as a trigger. Since the above process proceeds much faster than the electrolytic polymerization process, the polymerization time can be shortened, which is very advantageous for simplifying the manufacturing process. In addition, the above process can easily form a large-area hole transport layer.
- the sensitizing dye functions as a polymerization initiator and proceeds with polymerization to form a hole transport layer containing a conductive polymer, which may cause external voltage or solvation.
- a sensitizing dye is difficult to peel from the photoelectric conversion layer, and a photoelectric conversion element and a solar cell excellent in photoelectric conversion efficiency can be provided.
- the present invention it is possible to easily form a large-area hole transport layer, so when producing a module, compared to a module produced by laying a large number of small photoelectric conversion elements, The area of the portion that does not contribute to power generation can be reduced, and a photoelectric conversion element module and a solar cell with excellent photoelectric conversion efficiency can be provided.
- the photoelectric conversion element module in the method of manufacturing the photoelectric conversion element module, a substrate, a first electrode, a photoelectric conversion layer containing a semiconductor and a sensitizing dye, a hole transport layer having a conductive polymer, and a second electrode were laminated in this order.
- the photoelectric conversion layer is formed on the first electrode, and the photoelectric conversion layer is formed in the presence of an oxidizing agent.
- FIG. 1 is a schematic cross-sectional view showing an example of the photoelectric conversion element module of the present invention.
- the photoelectric conversion element module 100 is formed by electrically connecting two or more photoelectric conversion elements 10.
- each photoelectric conversion element 10 includes a substrate 20, a first electrode 30, a buffer layer 40, a photoelectric conversion layer 50, a hole transport layer 60, and a second electrode 70 that is a counter electrode.
- the photoelectric conversion layer 50 contains a semiconductor (not shown) and a sensitizing dye (not shown).
- Each photoelectric conversion element 10 has a common substrate 20, and a first electrode 30, a buffer layer 40, a photoelectric conversion layer 50, a hole transport layer 60, and a second electrode 70 are formed on the substrate 20 in this order. Is done.
- the photoelectric conversion element 10 is electrically connected to the adjacent photoelectric conversion element 10, but at this time, the connection form is not particularly limited, but is preferably connected in series. More specifically, (a) As shown in FIG. 1, in two adjacent photoelectric conversion elements 10, the end portion 31 of the first electrode 30 of one photoelectric conversion element is connected to the adjacent photoelectric conversion element 10. A form in which the end portion 71 of the second electrode 70 is connected (connected) in series is preferable.
- the end 31 of the first electrode 30 of one photoelectric conversion element is connected (connected) to the end 71 of the second electrode 70 of the adjacent photoelectric conversion element 10 via a conductive member.
- a conductive member is also preferably used.
- the form (a) is particularly preferred. That is, at least two photoelectric conversion elements adjacent to each other among the photoelectric conversion elements include one end of the first electrode of one photoelectric conversion element and one end of the second electrode of the photoelectric conversion element adjacent to the photoelectric conversion element. Are preferably connected.
- a buffer layer 40 may be formed between the first electrode 30 and the photoelectric conversion layer 50 as necessary for the purpose of preventing short circuit and sealing.
- the size of the substrate 20 is not particularly limited, and is appropriately selected according to a desired application (for example, a solar cell).
- the size of the substrate is preferably 50 to 3000 mm in length, 50 to 3000 mm in width, and 0.01 to 100 mm in thickness considering the photoelectric conversion efficiency per unit area of the module.
- the size of each photoelectric conversion element is not particularly limited.
- the photoelectric conversion elements are preferably sized so that 2 to 300, more preferably 10 to 100, photoelectric conversion elements are arranged on the substrate. Is preferred. With such a size, the photoelectric conversion element module exhibits sufficient power generation performance, and the area of the portion that does not contribute to power generation can be reduced.
- each first electrode 30 is 2 to 2 in the horizontal (long side) when the vertical (short side) is 1, considering the resistance of the oxide semiconductor and the area contributing to power generation. A ratio of 100 is preferred.
- the distance between the first electrodes (“X” in FIG. 1) is preferably as short as possible in consideration of reducing the area of the portion that does not contribute to power generation and achieving sufficient photoelectric conversion efficiency.
- the thickness is preferably 0.001 to 10 mm, more preferably 0.01 to 1 mm.
- FIG. 1 sunlight enters from the direction of the arrow 8 at the bottom of the figure, but the present invention is not limited to this form, and sunlight may enter from the top of the figure.
- the photoelectric conversion element according to the present invention has a structure in which a substrate, a first electrode, a photoelectric conversion layer, a hole transport layer, and a second electrode as a counter electrode are sequentially laminated as essential components, and two or more electrically It is connected. If necessary, a buffer layer may be formed between the substrate and the first electrode, and / or a buffer layer on the surface of the second electrode.
- a buffer layer may be formed between the substrate and the first electrode, and / or a buffer layer on the surface of the second electrode.
- the substrate according to the present invention is provided on the light incident direction side, and from the viewpoint of photoelectric conversion efficiency of the photoelectric conversion element, a transparent substrate is preferable, and a transparent conductive substrate having a first electrode formed on the surface is more preferable.
- the transmittance is more preferably 10% or more, still more preferably 50% or more, and particularly preferably 80% to 100%.
- the light transmittance is a visible wavelength region measured by a method in accordance with “Testing method of total light transmittance of plastic-transparent material” of JIS K 7361-1: 1997 (corresponding to ISO 13468-1: 1996). The total light transmittance at.
- the substrate can be appropriately selected from known materials, materials, shapes, structures, thicknesses, hardnesses, etc., but preferably has a high light transmittance as described above.
- the substrate can be roughly classified into a rigid substrate such as a glass plate and an acrylic plate, and a flexible substrate such as a film substrate.
- a rigid substrate such as a glass plate and an acrylic plate
- a flexible substrate such as a film substrate.
- a glass plate is preferable in terms of heat resistance, and the type of glass is not particularly limited.
- the thickness of the substrate is preferably from 0.1 to 100 mm, more preferably from 0.5 to 10 mm.
- TAC triacetyl cellulose
- an inorganic glass film may be used as the substrate.
- the thickness of the substrate is preferably 1 to 1000 ⁇ m, and more preferably 10
- a resin film having a transmittance of 80% or more at a visible wavelength (400 to 700 nm) can be particularly preferably applied to the present invention.
- biaxially stretched polyethylene terephthalate film preferably a biaxially stretched polyethylene terephthalate film, a biaxially stretched polyethylene naphthalate film, a polyethersulfone film, or a polycarbonate film, and biaxially stretched. More preferred are polyethylene terephthalate films and biaxially stretched polyethylene naphthalate films.
- These substrates can be subjected to a surface treatment or an easy adhesion layer in order to ensure the wettability and adhesion of the coating solution.
- the surface treatment includes surface activation treatment such as corona discharge treatment, flame treatment, ultraviolet treatment, high frequency treatment, glow discharge treatment, active plasma treatment, and laser treatment.
- examples of the easy adhesion layer include polyester, polyamide, polyurethane, vinyl copolymer, butadiene copolymer, acrylic copolymer, vinylidene copolymer, epoxy copolymer and the like.
- the first electrode according to the present invention is disposed between the substrate and the photoelectric conversion layer.
- the first electrode is provided on one surface which is opposite to the light incident direction of the substrate.
- those having a light transmittance of 80% or more, more preferably 90% or more (upper limit: 100%) are preferably used.
- the light transmittance is the same as that described in the description of the substrate.
- the material for forming the first electrode is not particularly limited, and a known material can be used.
- a known material can be used.
- silver is preferably used as the metal, and a grid-patterned film having openings or a film in which fine particles or nanowires are dispersed and applied is preferably used in order to impart light transmittance.
- the metal oxide is preferably a composite (dope) material in which one or more selected from Sn, Sb, F and Al are added to the above metal oxide. More preferably, conductive metal oxides such as In 2 O 3 (ITO) doped with Sn, SnO 2 doped with Sb, and SnO 2 (FTO) doped with F are preferably used. Is most preferred.
- the amount of the material forming the first electrode applied to the substrate is not particularly limited, but is preferably about 1 to 100 g per 1 m 2 of the substrate.
- the first electrode according to the present invention is preferably a transparent conductive substrate provided on the surface of a transparent substrate, which is a substrate.
- the substrate on which the first electrode is formed is referred to as a transparent conductive substrate (or first conductive substrate). Also referred to as one electrode substrate).
- the average thickness of the transparent conductive substrate is not particularly limited, but is preferably in the range of 0.1 mm to 5 mm.
- the surface resistance of the transparent conductive substrate is preferably 50 ⁇ / cm 2 ( ⁇ (square)) or less, more preferably 20 ⁇ / ⁇ (square) or less, and still more preferably 10 ⁇ / ⁇ ( square) or less.
- the lower limit of the surface resistance of the transparent conductive substrate is preferably as low as possible and need not be specified. However, 0.01 ⁇ / ⁇ (square) or more is sufficient.
- the preferable range of the light transmittance of the transparent conductive substrate is the same as the preferable range of the light transmittance of the substrate.
- the 2nd electrode which concerns on this invention should just have electroconductivity, and arbitrary electroconductive materials are used. Even an insulating material can be used if a conductive material layer is provided on the side facing the hole transport layer.
- the second electrode preferably has good contact with the hole transport layer.
- the second electrode preferably has a small work function difference from the hole transport layer and is chemically stable.
- a material is not particularly limited, but is a metal thin film such as gold, silver, copper, aluminum, platinum, rhodium, magnesium, indium, carbon, carbon black, a conductive polymer, a conductive metal oxide (indium -Organic conductors such as tin composite oxide, tin oxide doped with fluorine, etc.
- the average thickness of the second electrode is not particularly limited, but is preferably 10 to 1000 nm.
- the surface resistance of the second electrode is not particularly limited, but is preferably low. Specifically, the range of the surface resistance of the second electrode is preferably 80 ⁇ / ⁇ (square) or less, and more preferably 20 ⁇ / ⁇ (square) or less. In addition, since it is preferable that the lower limit of the surface resistance of the second electrode is as low as possible, it is not necessary to define the lower limit, but 0.01 ⁇ / ⁇ (square) or more is sufficient.
- buffer layer In the photoelectric conversion element according to the present invention, it is preferable to have a buffer layer positioned between the first electrode and the photoelectric conversion layer (semiconductor layer) as a short-circuit prevention means or a rectifying action.
- the buffer layer and photoelectric conversion layer according to the present invention are preferably porous as described below.
- the buffer layer has a porosity of C [%]
- the semiconductor layer has a void.
- D / C is, for example, preferably about 1.1 or more, more preferably about 5 or more, and further preferably about 10 or more.
- the upper limit of D / C is as large as possible, it is not necessary to specify in particular, but it is usually about 1000 or less. Thereby, the buffer layer and the semiconductor layer can each exhibit their functions more suitably.
- the porosity C of the buffer layer is, for example, preferably about 20% by volume or less, more preferably about 5% by volume or less, and about 2% by volume or less. Further preferred. That is, the buffer layer is preferably a dense layer. Thereby, effects, such as a short circuit prevention and a rectification effect
- the lower limit of the porosity C of the buffer layer is preferably as small as possible, it does not need to be specified in particular, but is usually about 0.05% by volume or more.
- the average thickness (film thickness) of the buffer layer is, for example, preferably about 0.01 to 10 ⁇ m, and more preferably about 0.03 to 0.5 ⁇ m. Thereby, the said effect can be improved more.
- the constituent material of the buffer layer according to the present invention is not particularly limited.
- zinc, niobium, tin, titanium, vanadium, indium, tungsten, tantalum, zirconium, molybdenum, manganese, iron, copper, nickel, iridium, rhodium , Chromium, ruthenium or oxides thereof, or perovskites such as strontium titanate, calcium titanate, barium titanate, magnesium titanate, strontium niobate, or complex oxides or oxide mixtures thereof, CdS, CdSe,
- One type or a combination of two or more types of various metal compounds such as TiC, Si 3 N 4 , SiC, and BN can also be used.
- the hole transport layer is a p-type semiconductor
- a metal when used for the buffer layer, it is preferable to use a material having a work function value smaller than that of the hole transport layer and having a Schottky contact.
- a metal oxide when used for the buffer layer, it is preferable to use a metal oxide that is in ohmic contact with the transparent conductive layer and has a conduction band energy level lower than that of the porous semiconductor layer.
- the efficiency of electron transfer from the porous semiconductor layer (photoelectric conversion layer) to the buffer layer can be improved by selecting an oxide.
- those having electrical conductivity equivalent to that of the semiconductor layer (photoelectric conversion layer) are preferable, and those mainly composed of titanium oxide are more preferable.
- the titanium oxide layer may be either anatase-type titanium oxide or rutile-type titanium oxide having a relatively high dielectric constant.
- the photoelectric conversion layer according to the present invention preferably comprises a semiconductor layer containing a semiconductor and a sensitizing dye and containing the semiconductor carrying the sensitizing dye.
- the total content of the photoelectric conversion layer 1 m 2 per dye is preferably 0.01 ⁇ 100mmol / m 2, more preferably 0.1 ⁇ 50mmol / m 2, particularly preferably at 0.5 ⁇ 20mmol / m 2 is there.
- the semiconductor according to the present invention includes a simple substance such as silicon and germanium, a compound having an element of Group 3 to Group 5, Group 13 to Group 15 of a periodic table (also referred to as an element periodic table), a metal oxide, Metal sulfide, metal selenide, metal nitride, or the like can be used.
- Preferred semiconductors include titanium oxide, tin oxide, zinc oxide, iron oxide, tungsten oxide, zirconium oxide, hafnium oxide, strontium oxide, indium, cerium, yttrium, Lanthanum, vanadium, niobium oxide or tantalum oxide, cadmium sulfide, zinc sulfide, lead sulfide, silver sulfide, antimony or bismuth sulfide, cadmium or lead selenide, cadmium And tellurium compounds.
- Other compound semiconductors include phosphides such as zinc, gallium, indium, and cadmium, gallium-arsenic or copper-indium selenides, copper-indium sulfides, and titanium nitrides. More specifically, specific examples of the semiconductor include TiO 2 , SnO 2 , Fe 2 O 3 , WO 3 , ZnO, Nb 2 O 5 , CdS, ZnS, PbS, Bi 2 S 3 , CdSe, CdTe, GaP. InP, GaAs, CuInS 2 , CuInSe 2 , Ti 3 N 4 and the like.
- TiO 2 , ZnO, SnO 2 , Fe 2 O 3 , WO 3 , Nb 2 O 5 , CdS, and PbS are preferably used, TiO 2 or Nb 2 O 5 is more preferably used, and titanium oxide (TiO 2 ) Is more preferably used.
- the semiconductor described above may be used alone, or a plurality of semiconductors may be used in combination.
- several kinds of the above-described metal oxides or metal sulfides can be used in combination, or 20% by mass of titanium nitride (Ti 3 N 4 ) may be mixed and used in the titanium oxide semiconductor.
- Ti 3 N 4 titanium nitride
- the mass ratio of the additional component to the metal oxide or metal sulfide semiconductor is preferably 30% or less.
- TiO 2 when used for the semiconductor layer, TiO 2 may be either anatase-type titanium oxide and / or rutile-type titanium oxide having a relatively high dielectric constant.
- the shape of the semiconductor according to the present invention is not particularly limited, and examples thereof include a filler shape, a particle shape, a conical shape, a columnar shape, a tubular shape, and a flat plate shape.
- a film-like layer formed by agglomerating these filler-like, particle-like, conical, columnar, tubular and other semiconductors may be used.
- a semiconductor whose surface is coated with a sensitizing dye in advance may be used, or a sensitizing dye may be coated after a semiconductor layer is formed.
- the shape of the semiconductor according to the present invention is particulate, it is a primary particle and preferably has an average particle diameter of 1 to 5000 nm, and preferably 2 to 100 nm.
- the “average particle diameter” of the semiconductor is an average particle diameter of primary particle diameters (primary average particle diameter (diameter)) when 100 or more samples are observed with an electron microscope.
- the semiconductor according to the present invention may be surface-treated using an organic base.
- the organic base include diarylamine, triarylamine, pyridine, 4-t-butylpyridine, polyvinylpyridine, quinoline, piperidine, and amidine, among which pyridine, 4-t-butylpyridine, and polyvinylpyridine are preferable.
- the semiconductor surface treatment method is not particularly limited, and a known method can be applied as it is or after being appropriately modified.
- the organic base is a liquid
- a solution (organic base solution) dissolved in an organic solvent is prepared as it is, and the semiconductor according to the present invention is added to the liquid organic base or the organic base solution at 0 to 80 ° C.
- the surface treatment of the semiconductor can be carried out by immersion for 1 minute to 24 hours.
- sensitizing dye The sensitizing dye according to the present invention is supported on a semiconductor by the above-described sensitization treatment of a semiconductor and can be photoexcited upon photoirradiation to generate an electromotive force.
- An arylamine dye is preferable, and the following general formula ( The compound represented by 1) is more preferable.
- each R 3 independently represents a hydrogen atom, a halogen atom, a substituted or unsubstituted alkyl group, a substituted or unsubstituted alkoxy group, a substituted or unsubstituted alkenyl group, substituted or unsubstituted It represents a substituted alkynyl group, a substituted or unsubstituted aryl group, an amino group (—NH 2 ), a cyano group (—CN), or a substituted or unsubstituted heterocyclic group.
- n 1, two R 3 s may be different from each other, and R 3 may be linked to other substituents to form a ring structure.
- Ar represents a divalent cyclic compound group.
- a 1 and A 2 each independently represents a single bond, a divalent saturated or unsaturated hydrocarbon group, a substituted or unsubstituted alkylene group, an arylene group, or a divalent heterocyclic group.
- Z is an organic group having an acidic group, an alkoxysilane or a halogenated silane, and is preferably an organic group containing at least one carboxyl group.
- n is 2 or more, the plurality of A 1 , A 2 , and Z may be different from each other.
- p and q are each independently an integer of 0 or more and 6 or less.
- p and q may be the same or different from each other.
- each A 1 may be the same or different from each other.
- each A 2 may be the same or different from each other.
- n is an integer of 1 or more and 3 or less, and is preferably 2.
- Ar in the general formula (1) is not particularly limited, and is preferably a divalent to tetravalent cyclic compound group, for example.
- the cyclic compound group include benzene ring, naphthalene ring, anthracene ring, thiophene ring, phenylthiophene ring, diphenylthiophene ring, imidazole ring, oxazole ring, thiazole ring, pyrrole ring, furan ring, benzimidazole ring, It is derived from an aromatic ring such as a benzoxazole ring, rhodanine ring, pyrazolone ring, imidazolone ring, pyran ring, pyridine ring or fluorene ring.
- a plurality of these aromatic rings may be used in combination, for example, a biphenyl group, a terphenyl group, a fluorenyl group, a bithiophene group, a 4-thienylphenyl group, a diphenylstyryl group, etc., and further, stilbene, 4-phenylmethylene- 2,5-cyclohexadiene, triphenylethene (eg, 1,1,2-triphenylethene), phenylpyridine (eg, 4-phenylpyridine), styrylthiophene (eg, 2-styrylthiophene), 2- (9H -Fluoren-2-yl) thiophene, 2-phenylbenzo [b] thiophene, phenylbithiophene ring, (1,1-diphenyl-4-phenyl) -1,3-butadiene, 1,4-diphenyl-1,3 -Dibutadiene,
- aromatic rings may have a substituent, such as a halogen atom (for example, fluorine, chlorine, bromine, etc.), each substituted or unsubstituted, straight chain having a carbon chain length of 1 to 24 Or a branched alkyl group (for example, methyl group, ethyl group, t-butyl group, isobutyl group, dodecyl group, octadecyl group, 3-ethylpentyl group), hydroxyalkyl group (for example, hydroxymethyl group, hydroxyethyl group)
- An alkoxyalkyl group for example, methoxyethyl group
- an alkoxy group having a carbon chain length of 1 to 18 for example, methoxy group, ethoxy group, ethoxy group, propoxy group, isopropoxy group, butoxy group, pentyloxy group, hexyloxy) Group
- aryl group eg, phenyl group, toly
- the alkyl group in the general formula (1) is preferably a linear or branched alkyl group having a carbon chain length of 1 to 30 or a cycloalkyl group having a carbon chain length of 3 to 10, and a carbon chain length of 1 It is more preferably a linear or branched alkyl group of ⁇ 24 or a cycloalkyl group of 3 to 9 carbon chain length.
- a linear or branched alkyl group having a carbon chain length of 1 to 30 is not particularly limited.
- the cycloalkyl group having a carbon chain length of 3 to 10 is not particularly limited. Examples thereof include a cyclopropyl group, a cyclobutyl group, a cyclopentyl group, a cyclohexyl group, a cycloheptyl group, a cyclooctyl group, a cyclononyl group, and a cyclodecyl group. Of these, cycloalkyl groups having a carbon chain length of 3 to 6 are preferred.
- a linear or branched alkyl group having a carbon chain length of 1 to 18 and a cycloalkyl group having a carbon chain length of 3 to 7 are preferred, and include a methyl group, an ethyl group, an n-propyl group, an n-butyl group, Straight chain alkyl groups having 1 to 6 carbon chain length such as n-pentyl group and n-hexyl group and branched alkyl groups having 3 to 6 carbon chain length such as isopropyl group and t-butyl group, and cyclopentyl group, cyclohexyl group, etc.
- a cycloalkyl group having a carbon chain length of 5 to 6 is more preferred.
- the alkoxy group in the general formula (1) is not particularly limited, and is preferably an alkoxy group having a carbon chain length of 1 to 30, and more preferably an alkoxy group having a carbon chain length of 1 to 18.
- the alkenyl group in the general formula (1) is not particularly limited, and the alkenyl group may be linear, branched or cyclic. Further, the alkenyl group preferably has 2 to 18 carbon atoms. Specific examples of the alkenyl group include vinyl group, allyl group, propenyl group, isopropenyl group, 1-butenyl group, 2-butenyl group, 3-butenyl group, 1-hexenyl group, 2-hexenyl group, and 3-hexenyl group. 4-hexenyl group, 5-hexenyl group, cyclopentenyl group, cyclohexenyl group, cyclooctenyl group and the like. Alkenyl groups other than these may be used.
- the alkynyl group in the general formula (1) is not particularly limited, and may be linear, branched or cyclic. Further, the alkynyl group preferably has 2 to 18 carbon atoms. Specific examples of the alkynyl group include ethynyl group, 2-propynyl group, 2-butynyl group and the like. Alkynyl groups other than these may be used.
- the aryl group in the general formula (1) is not particularly limited, and examples thereof include a phenyl group, a naphthyl group, a biphenyl group, a fluorenyl group, an anthryl group, a pyrenyl group, an azulenyl group, an acenaphthylenyl group, a terphenyl group, and a phenanthryl group.
- a phenyl group, a biphenyl group, and a naphthyl group are preferable.
- the heterocyclic group in the general formula (1) is not particularly limited, and is preferably a heterocyclic group containing at least one heteroatom selected from a nitrogen atom, an oxygen atom and a sulfur atom.
- a condensed heterocyclic group in which a plurality of heterocyclic rings are condensed for example, a group derived from dithieno [3,2-b: 2 ′, 3′-d] thiophene in which three thiophene rings are condensed
- a heterocyclic ring It may be a condensed heterocyclic group in which a hydrocarbon ring (non-aromatic hydrocarbon ring or aromatic hydrocarbon ring) is condensed (ortho condensation, ortho-and-peri condensation, etc.).
- the heterocyclic group may be non-aromatic or aromatic. Furthermore, in the condensed heterocyclic group in which the heterocyclic ring and the hydrocarbon ring are condensed, either the heterocyclic ring or the hydrocarbon ring may have a bond.
- heterocyclic group in the general formula (1) examples include pyrrolyl, imidazolyl, pyridyl, pyrazinyl, indolyl, quinolyl, isoquinolyl, quinazolyl, carbazolyl, carbolinyl, phenanthridinyl Group, acridinyl group, phenazinyl group, isobenzofuranyl, chromenyl group, thienyl group, thianthenyl group, morpholinyl group, isothiazolyl group, isoxazolyl group, phenoxathinyl group and the like.
- Preferred heterocyclic groups are a pyrrolyl group, an indolyl group, and a carbazolyl group.
- substituted or unsubstituted means at least one of the above-exemplified alkyl group, alkoxy group, alkenyl group, alkynyl group, aryl group, and heterocyclic group.
- This substituent is the number of carbon atoms in the above-mentioned alkyl group, alkoxy group, alkenyl group, alkynyl group, aryl group, and heterocyclic group. Substitution may be made within a range not exceeding. The same applies hereinafter.
- the substituent which exists depending on the case is not the same as the substituent. For example, when R 3 is an alkyl group, it is not further substituted with an alkyl group.
- R 3 in the general formula (1) according to the present invention include the following chemical formulas (2-A) to (2-S) as preferable groups.
- h is the degree of polymerization and is an integer of 1 to 17.
- Y represents a hydrogen atom, the above-described alkyl group, alkoxy group, alkenyl group, alkynyl group, aryl group, or heterocyclic group, preferably a hydrogen atom, An alkyl group or an alkoxy group.
- the wavy line indicates a position where it is connected to another group.
- the alkylene group in the general formula (1) is not particularly limited and may be linear or branched, and may be a methylene group, an ethylene group, a propylene group, a butylene group, an isobutylene group, a sec-butylene group, or a tert-butylene. Group, pentylene group, iso-pentylene group, hexylene group and the like.
- the arylene group in the general formula (1) is not particularly limited, and includes a phenylene group, a biphenyl-diyl group, a terphenyl-diyl group, a naphthalene-diyl group, an anthracene-diyl group, a tetracene-diyl group, a fluorene-diyl group, And phenanthrene-diyl group.
- i is the degree of polymerization and is an integer of 1 to 17.
- Y represents a hydrogen atom, the above-described alkyl group, alkoxy group, alkenyl group, alkynyl group, Represents an aryl group or a heterocyclic group, and preferably a hydrogen atom, an alkyl group, or an alkoxy group.
- Z is an organic group having an acidic group, an alkoxysilane or a halogenated silane, preferably any one of an acidic group and an Ar having an electron-withdrawing group or an electron-withdrawing ring structure. And more preferably an organic group containing at least one carboxyl group.
- the partial structure Z is substituted with Ar, Ar 1 and Ar 2 in the general formula (1), and at least one hydrogen atom (H) present in R 3 , preferably at least Ar It is substituted with a hydrogen atom (H) at the terminal of 2 .
- examples of the acidic group in the partial structure Z include a carboxyl group, a sulfo group [—SO 3 H], a sulfino group, a sulfinyl group, a phosphonic acid group [—PO (OH) 2 ], a phosphoryl group, a phosphinyl group, and a phosphono group.
- a carboxyl group a sulfo group [—SO 3 H]
- a sulfino group a sulfinyl group
- a phosphonic acid group [—PO (OH) 2 ]
- a phosphoryl group a phosphinyl group
- a phosphono group a group, thiol group, hydroxy group, phosphonyl group, alkoxysilane group, and sulfonyl group; and salts thereof.
- the acidic group a carboxyl group, a sulfo group, a phosphonic acid group, and a hydroxy group are preferable, and a carboxyl group is more preferable.
- the electron-withdrawing group include cyano group, nitro group, fluoro group, chloro group, bromo group, iodo group, perfluoroalkyl group (for example, trifluoromethyl group), alkylsulfonyl group, arylsulfonyl group, perfluoro group. Examples thereof include an alkylsulfonyl group and a perfluoroarylsulfonyl group.
- the electron-withdrawing ring structure includes a rhodanine ring, a dirhodanine ring, an imidazolone ring, a pyrazolone ring, a pyrazoline ring, a quinone ring, a pyran ring, a pyrazine ring, a pyrimidine ring, an imidazole ring, an indole ring, a benzothiazole ring, a benzoimidazole ring, Examples thereof include an oxazole ring and a thiadiazole ring.
- a rhodanine ring, a dirhodanine ring, an imidazolone ring, a pyrazoline ring, a quinone ring and a thiadiazole ring are preferable, and a rhodanine ring, a dirhodanine ring, an imidazolone ring and a pyrazoline ring are more preferable.
- These Z can effectively inject photoelectrons into a semiconductor (especially an oxide semiconductor).
- the acidic group and the electron-withdrawing group or the electron-withdrawing ring structure are oxygen atoms (O), sulfur atoms (S), selenium atoms (Se), tellurium atoms (Te), etc.
- the partial structure Z may have a charge, particularly a positive charge, and in this case, Cl ⁇ , Br ⁇ , I ⁇ , ClO 4 ⁇ , NO 3 ⁇ , SO 4 2 ⁇ , H 2 PO 4 ⁇ and the like. May have a counter ion.
- Z in the general formula (2) include the following chemical formulas (4-A) to (4-N).
- g represents the degree of polymerization and is an integer of 1 to 17.
- a sensitizing dye having a carboxyl group can be suitably used because CO 2 is not eliminated (Kolbe electrolysis) by an applied voltage even when a carboxyl group is present, and the dye does not deteriorate.
- sensitizing dye according to the present invention are shown below.
- Ar has the chemical formula (1-B), and / or R 3 has the chemical formula (2-A), the chemical formula (2-G), the chemical formula (2-J), and the chemical formula (2- K), and / or A 1 and A 2 are represented by chemical formula (3-D), chemical formula (3-I), chemical formula (3-P), chemical formula (3-Q), chemical formula (3-R) ) Is particularly preferred.
- the hole transport layer according to the present invention has a function of supplying electrons to a sensitizing dye oxidized by photoexcitation and reducing it, and transporting holes generated at the interface with the sensitizing dye to the second electrode. It is preferable that the hole transport layer can be filled not only in the layered portion formed on the porous semiconductor layer but also in the voids of the porous semiconductor layer.
- the hole transport layer according to the present invention polymerizes the conductive polymer precursor by irradiating the sensitizing dye with light after contacting the conductive polymer precursor with the photoelectric conversion layer in the presence of an oxidizing agent. It is formed by.
- the hole transport layer according to the present invention irradiates the photoelectric conversion layer with light after bringing the photoelectric conversion layer into contact with a solution containing the conductive polymer precursor and the oxidizing agent in the ratio of the following mathematical formula (1). Is preferably formed.
- [Ox] is the molar concentration of the oxidizing agent
- [M] is the molar concentration of the conductive polymer precursor.
- light irradiation photochemical polymerization of the conductive polymer precursor
- the [Ox] / [M] ratio is preferably 0.15 to 300, and more preferably 0.2 to 100.
- the sensitizing dye in the photoelectric conversion layer is irradiated with light
- electrons excited in the sensitizing dye are consumed by an oxidizing agent (for example, hydrogen peroxide solution). Therefore, the sensitizing dye becomes a cationic state, and the cationic dye extracts electrons from the conductive polymer precursor, and the conductive polymer precursor becomes a cationic state.
- Polymerization is started when the conductive polymer precursor in the cationic state becomes a trigger.
- the cationic sensitizing dye can be efficiently conducted. Since electrons are extracted from the conductive polymer precursor, the polymerization can be started more quickly with the conductive polymer precursor in a cationic state as a trigger.
- the conductive polymer precursor is a relatively low molecular weight monomer, it easily penetrates into the porous photoelectric conversion layer, and the sensitizing dye of the photoelectric conversion layer serves as an initiator for the polymerization reaction. Since it also serves as a starting point, it is considered that the amount of the polymerized conductive polymer covering the sensitizing dye is larger than the amount of the conductive polymer polymerized by electrolytic polymerization covering the sensitizing dye.
- the above process proceeds much faster than the electrolytic polymerization process, the polymerization time can be shortened, which is very advantageous for simplifying the manufacturing process.
- the above process can easily form a large-area hole transport layer.
- the hole transport layer according to the present invention has a conductive polymer formed by a photopolymerization reaction of a conductive polymer precursor using a sensitizing dye oxidized by light irradiation as a polymerization initiator. More specifically, the hole transport layer according to the present invention is a sensitizing dye produced by reacting an electron excited by irradiation of a sensitizing dye with an oxidizing agent and oxidizing the sensitizing dye. A conductive polymer obtained by polymerizing a conductive polymer precursor using a cation as a polymerization initiator is included.
- the sensitizing dye and the irradiating light for exciting the sensitizing dye and the oxidizing agent for depriving the excited electrons are present. Polymerization of the conductive polymer precursor becomes possible. Furthermore, if the level of the oxidant is higher than that of the excited sensitizing dye, electrons can be taken away. On the other hand, if the level of the oxidizing agent is too high, the conductive polymer precursor (for example, bis-EDOT) is directly oxidized and polymerized, making it difficult to form a uniform film in the vicinity of the sensitizing dye. There is sex. For this reason, it is preferable to polymerize with an oxidizing agent having an appropriate standard electrode potential.
- an oxidizing agent having an appropriate standard electrode potential.
- the oxidizing agent according to the present invention preferably has a standard electrode potential (E 0 (OX) ) (V) of ⁇ 1.5 to +2.5 V, and is ⁇ 0.5 to +2.0 V. It is more preferable to have a standard electrode potential (E 0 (OX) ) (V) of
- E 0 (OX) standard electrode potential
- the standard electrode potential of the oxidizing agent is equal to or higher than the lower limit of the above range, the polymerization can proceed more efficiently.
- the standard electrode potential of the oxidizing agent is not more than the upper limit of the above range, the reaction (reaction rate) is easily controlled, the productivity is excellent, and this is industrially preferable.
- standard electrode potential (E 0 (OX) ) (V) means a standard electrode potential (25 ° C.) in an aqueous solution.
- the oxidizing agent according to the present invention is preferably a compound that becomes a gas compound or a liquid compound by light irradiation (reduction of itself).
- the photoelectric conversion efficiency of the photoelectric conversion element obtained can be improved further.
- the “gaseous compound” means a compound that is gaseous under the conditions of 20 ° C. and 1 atm.
- the “liquid compound” means a compound that is liquid under conditions of 20 ° C. and 1 atm.
- a sensitizing dye When a sensitizing dye is irradiated with light in the presence of an oxidizing agent, electrons excited in the dye are consumed by the oxidizing agent (for example, hydrogen peroxide / hydrogen peroxide solution), and the cationic sensitizing dye is a monomer. It is thought that polymerization is initiated by extracting electrons from a certain conductive polymer precursor.
- an oxidizing agent for example, hydrogen peroxide / hydrogen peroxide solution
- peroxide examples include permanganic acid or a salt thereof, chromic acid or a salt thereof, peroxo acid or a salt thereof, oxygen acid or a salt thereof, nitric acid, sulfuric acid, and the like.
- Inorganic peroxides such as sodium peroxoborate, hypochlorous acid, hypobromous acid, hypoiodous acid, chloric acid, bromic acid, iodic acid, sodium hypochlorite, calcium hypochlorite; cumene hydro Peroxide, formic acid, performic acid, peracetic acid, perbenzoic acid, perphthalic acid, t-butyl hydroperoxide, 1,1,3,
- the metal salt examples include iron (III) tris-p-toluenesulfonate, iron (II) chloride, iron (III) chloride, iron (III) sulfate, iron (III) nitrate, silver nitrate (AgNO 3 ), citric acid Examples thereof include iron (III) and ammonium iron (III) sulfate.
- an oxidizing agent having a standard electrode potential (E 0 (OX) ) of ⁇ 0.5 to +2.0 (V) may be used.
- E 0 (OX) a standard electrode potential
- methanol (+0.588 V) may be used.
- Oxygen (+1.229 V) and the like can be used.
- hydrogen peroxide (+1.763 V), cumene hydroperoxide, formic acid (+0.034 V), iron (II) chloride ( ⁇ 0.440 V), silver nitrate (AgNO 3 ) (+0.799 V), methanol , Oxygen (+1.229 V), iron (III) tris-p-toluenesulfonate, potassium permanganate, and ozone are preferable, and hydrogen peroxide, oxygen (+1.229 V), and ozone are more preferable.
- the conductive polymer precursor according to the present invention is preferably a monomer component having a repeating unit represented by the following monomer formula 1.
- X represents S, NR, O
- R is any one of a hydrogen atom and an alkyl group
- R 1 to R 4 each independently represent a hydrogen atom, a halogen atom, Straight chain or branched alkyl group having 1 to 30 carbon atoms, cycloalkyl group having 3 to 10 carbon atoms, alkoxy group having 1 to 30 carbon atoms, polyethylene oxide group having 2 to 30 carbon atoms, or substitution Alternatively, it is an unsubstituted cyclic compound-containing group having 4 to 30 carbon atoms.
- the linear or branched alkyl group having 1 to 30 carbon atoms, the cycloalkyl group having 3 to 10 carbon atoms, and the alkoxy group having 1 to 30 carbon atoms are the same as those in the general formula (1). Therefore, it is omitted here.
- halogen atom is not particularly limited, but includes a fluorine atom, a chlorine atom, a bromine atom or an iodine atom.
- the polyethylene oxide group having 2 to 30 carbon atoms has the formula: — (CH 2 CH 2 O) x H or the formula: — (OCH 2 CH 2 ) x H [wherein x is an integer of 1 to 9] It is a group represented by Of these, x is preferably 3 to 9, and more preferably — (OCH 2 CH 2 ) 9 H.
- the cyclic compound group having 4 to 30 carbon atoms includes benzene ring, naphthalene ring, anthracene ring, thiophene ring, phenylthiophene ring, diphenylthiophene ring, imidazole ring, oxazole ring, thiazole ring, pyrrole ring, furan ring, benzine It is derived from a group in which one hydrogen element is removed from imidazole ring, benzoxazole ring, rhodanine ring, pyrazolone ring, imidazolone ring, pyran ring, pyridine ring, fluorene ring and the like.
- R 1 to R 4 in the general formula (2) according to the present invention are each independently a hydrogen atom, a halogen atom, an alkyl group having 6 to 24 carbon atoms, an alkoxy group having 1 to 18 carbon atoms, phenyl Group, biphenyl group, phenyl group substituted by alkyl group having 1 to 8 carbon atoms, biphenyl group substituted by alkyl group having 1 to 8 carbon atoms, thiophene group, bithiophene group, alkyl group having 1 to 8 carbon atoms A substituted thiophene group, a bithiophene group substituted by an alkyl group having 1 to 8 carbon atoms, a thiophene group substituted by an alkoxy group having 1 to 8 carbon atoms, or a bithiophene group substituted by an alkoxy group having 1 to 8 carbon atoms It is.
- the conductive polymer precursor according to the present invention may be any one having the above formula (1) and playing a role of polymerization. Therefore, a multimer in which the above formula (1) is combined alone or a plurality of types of repeating units may be used. Furthermore, it may be a prepolymer (including a dimer or higher multimer or a so-called oligomer) obtained by polymerizing a monomer having the above repeating unit in advance, alone or with a plurality of types of monomers, as necessary.
- the conductive polymer precursor is a prepolymer, and will be described in the synthesis method described later. However, the conductive polymer precursor is applied to the photoelectric conversion layer in the form of a prepolymer, A method of forming a conductive polymer by chemical polymerization can be simple.
- the repeating unit when the conductive polymer precursor is a multimer has the following formula:
- X and R 1 to R 4 are the same as those in the monomer formula 1, and m represents the number of bonds of the monomer.
- m 2
- m In the case of 3, it indicates a trimer.
- m is preferably an integer of 1 or more and 10 or less.
- the conductive polymer according to the present invention has the following general formula (2):
- X represents S, NR, or O
- R is a hydrogen atom or an alkyl group
- R 1 to R 4 are independently a hydrogen atom or a halogen atom.
- Preferred substituents (R 1 to R 4 ) and X in the general formula (2) are the same as those in the above repeating unit.
- the degree of polymerization of the conductive polymer according to the present invention is difficult to grasp from the polymer obtained by the synthesis method.
- the solvent solubility of the hole transport layer formed after polymerization is greatly reduced, the hole transport layer is soaked in tetrahydrofuran (THF) that can dissolve the polymer.
- THF tetrahydrofuran
- a compound conductive polymer
- THF tetrahydrofuran
- ultrasonic waves 25 kHz, 150 W, ultrasonic industry COLLECTOR CURRENT 1.5A made by ultrasonic industry 150
- the hole transport layer according to the present invention includes a conductive polymer represented by the general formula (2), and if necessary, the hole transport layer is at least selected from the group consisting of an electrolyte and an additive. One may be included as a component.
- Examples of the electrolyte include a dispersion of a redox electrolyte and a supporting electrolyte.
- a redox electrolyte I ⁇ / I 3 ⁇ series, Br ⁇ / Br 3 ⁇ series, quinone / hydroquinone series, [Co (bpy) 3 ] 2+ / [Co (bpy) 3 ] 3+ and the like are used. sell.
- the dispersion of the redox electrolyte can be obtained by a known method.
- an I ⁇ / I 3 -based electrolyte can be obtained by mixing iodide ions and iodine.
- the redox electrolyte dispersion is dispersed in a liquid electrolyte when used in a liquid form, a solid polymer electrolyte when dispersed in a solid polymer at room temperature (25 ° C.), and a gel substance. In this case, it is called a gel electrolyte.
- a liquid electrolyte is used as the hole transport layer
- an electrochemically inert solvent is used as the solvent. Examples of the solvent include acetonitrile, propylene carbonate, and ethylene carbonate.
- the electrolyte described in JP-A No. 2001-160427 is used.
- the gel electrolyte the electrolyte described in “Surface Science” Vol. 21, No. 5, pages 288 to 293 is used. , Respectively.
- lithium perchlorate LiClO 4
- lithium tetrafluoroborate lithium tetrafluoroborate
- tetrabutylammonium perchlorate Li [(CF 3 SO 2 ) 2 N] (lithium bistrifluoromethanesulfonylimide)
- Li [(CF 3 SO 2 ) 2 N] lithium bistrifluoromethanesulfonylimide)
- salts such as C 4 H 9 ) 4 NBF 4 , (nC 4 H 9 ) 4 NPF 4 , p-toluenesulfonate, dodecylbenzenesulfonate.
- polymer electrolytes described in JP-A-2000-106223 may be used as the supporting electrolyte.
- the said supporting electrolyte may be used independently and may mix and use 2 or more types.
- the polymerization catalyst is not particularly limited, but iron (III) chloride, iron (III) p-dodecylbenzenesulfonate, iron (III) methanesulfonate, iron (III) p-ethylbenzenesulfonate, iron naphthalenesulfonate. (III), and hydrates thereof.
- the sensitizing dye acts as a polymerization initiator, it is not necessary to add a polymerization catalyst, but it is necessary when it is desirable to promote the polymerization and proceed. Depending on the case, a polymerization catalyst may be added.
- the polymerization rate adjusting agent is not particularly limited as long as it has a weak complexing agent for trivalent iron ions in the polymerization catalyst and can reduce the polymerization rate so that a film can be formed.
- the polymerization catalyst is iron (III) chloride and a hydrate thereof
- an aromatic oxysulfonic acid such as 5-sulfosalicylic acid can be used.
- the polymerization catalyst is iron (III) p-dodecylbenzenesulfonate, iron (III) methanesulfonate, iron (III) p-ethylbenzenesulfonate, iron (III) naphthalenesulfonate, and hydrates thereof.
- imidazole or the like can be used.
- the reaction conditions for the above chemical polymerization vary depending on the prepolymer used, the polymerization catalyst added as necessary, the type, ratio, and concentration of the polymerization rate modifier, the thickness of the liquid film at the applied stage, and the desired polymerization rate.
- the heating temperature is preferably 25 to 120 ° C. and the heating time is preferably 1 minute to 24 hours.
- chemical polymerization is performed by light irradiation.
- the hole transport layer according to the present invention is preferably a solid hole transport layer. Therefore, the above-mentioned solid polymer electrolyte is preferably used as the material for the solid hole transport layer.
- N (PhBr) 3 SbCl 6 , NOPF 6 , SbCl 5 , I 2 , Br 2 , HClO 4 , (nC 4 H 9 ) 4 are used as necessary.
- the material contained in the hole transport layer preferably has a large band gap so as not to prevent light absorption by the sensitizing dye. Specifically, it preferably has a band cap of 2 eV or more, and more preferably has a band cap of 2.5 eV or more.
- the hole transport layer preferably has a low ionization potential in order to reduce sensitizing dye holes. Although the value of the ionization potential varies depending on the sensitizing dye to be applied, it is usually preferably 4.5 to 5.5 eV, more preferably 4.7 to 5.3 eV. *
- the average thickness of the hole transport layer according to the present invention is not easily measured when the semiconductor layer is a porous body, since it penetrates into the porous body and the gaps.
- the second of the present invention is a photoelectric conversion element in which a substrate, a first electrode, a semiconductor and a photoelectric conversion layer containing a sensitizing dye, a hole transport layer having a conductive polymer, and a second electrode are laminated in this order.
- the photoelectric conversion layer is formed on the first electrode, and a conductive polymer is formed on the photoelectric conversion layer in the presence of an oxidizing agent.
- It is a manufacturing method of a photoelectric conversion element module including forming the second electrode on and electrically connecting at least two or more of the photoelectric conversion elements.
- the hole transport layer according to the present invention is formed not by electrolytic polymerization but by chemical polymerization. Therefore, as described above, there is a problem that a sufficient amount of conductive polymer cannot be formed by polymerization under a low voltage in order not to deteriorate the sensitizing dye, and a decrease in productivity due to a long polymerization time due to polymerization under a low voltage.
- the problem is that it is difficult to form a uniform conductive polymer on the entire device because it is difficult to apply a uniform voltage in conventional electropolymerization when manufacturing a photoelectric conversion device with a large area. Can be solved by the present invention.
- the present invention it is possible to easily form a large-area hole transport layer, so when producing a module, compared to a module produced by laying a large number of small photoelectric conversion elements, The area of the portion that does not contribute to power generation can be reduced, and a photoelectric conversion element module and a solar cell with excellent photoelectric conversion efficiency can be provided.
- the manufacturing method of the photoelectric conversion element according to the present invention will be described in detail.
- the definition of the configuration in the production method of the present invention is the same as the definition of the configuration of the photoelectric conversion element module of the present invention.
- the step (1) of forming the photoelectric conversion layer on a substrate provided with a first electrode on the surface is the production of the first electrode forming the first electrode on the substrate.
- the method may be divided into a method and a method for forming a photoelectric conversion layer, and a method for forming a buffer layer after forming a first electrode on a substrate may be provided if necessary.
- a method for forming a buffer layer after forming a first electrode on a substrate may be provided if necessary.
- Method for manufacturing the first electrode As a method for producing the first electrode according to the present invention, that is, a method for forming a plurality of first electrodes (also referred to as transparent conductive layers) on one substrate, an appropriate method is used according to the material of the transparent conductive layer. You can choose the method. Examples of such a method include sputtering, CVD (vapor deposition), SPD (spray pyrolysis deposition), and vapor deposition. By these methods, a thin film made of an oxide semiconductor such as ITO, FTO, or SnO 2 is formed. If the transparent conductive layer is too thick, the light transmittance is inferior, whereas if it is too thin, the conductivity is inferior.
- CVD vapor deposition
- SPD spray pyrolysis deposition
- the transparent conductive layer preferably has a thickness range of about 0.1 to 5 ⁇ m.
- the size of the substrate is preferably 50 to 3000 mm in length, 50 to 3000 mm in width, and 0.1 to 100 mm in thickness.
- the size of each photoelectric conversion element is not particularly limited.
- the photoelectric conversion elements are preferably sized so that 2 to 300, more preferably 10 to 100, photoelectric conversion elements are arranged on the substrate. Is preferred. With such a size, the photoelectric conversion element module exhibits sufficient power generation performance, and the area of the portion that does not contribute to power generation can be reduced.
- each first electrode is 2 to 100 in the horizontal (long side) when the vertical (short side) is 1, considering the resistance of the oxide semiconductor and the area contributing to power generation. It is preferable that it is a ratio.
- the distance between the first electrodes (“X” in FIG. 1) is preferably as short as possible in consideration of reducing the area of the portion that does not contribute to power generation and achieving sufficient photoelectric conversion efficiency.
- the thickness is preferably 0.001 to 10 mm, and more preferably 0.1 to 1 mm.
- an appropriate method can be selected according to the material of a transparent conductive layer.
- Specific examples include excimer laser, YAG laser, CO 2 laser, air jet, water jet processing, etching processing, and mechanical processing.
- the transparent conductive layer can be separated into a plurality of regions.
- the pitch of the slits can be appropriately set according to the size of the cell of the photoelectric conversion element.
- Examples of the method for forming the buffer layer according to the present invention include a method in which a buffer layer precursor, which is a buffer layer forming component, is coated on the first electrode and, if necessary, heat treatment is performed. Specifically, after forming the (coating) layer of the buffer layer forming component on the (first electrode) of the transparent conductive substrate on which the first electrode according to the present invention is formed on the substrate surface, the CVD method or the firing method A method in which the reaction proceeds to form a buffer layer, a coating method using a coating solution for forming a buffer layer, a coating method by a spin coating method, or an atomic layer deposition (ALD) method is preferable.
- a buffer layer precursor which is a buffer layer forming component
- ALD atomic layer deposition
- the CVD method or baking A method in which the reaction proceeds by the method to form a buffer layer is more preferable.
- the buffer layer forming component refers to a compound that becomes a buffer layer by a chemical reaction.
- a titanium oxide precursor is preferable, and as the titanium oxide precursor, titanium oxide is more preferably generated by hydrolysis.
- titanium halides titanium trichloride, titanium tetrachloride, etc.
- orthotitanate esters methyl orthotitanate, ethyl orthotitanate, isopropyl orthotitanate, butyl orthotitanate, etc.
- titanium butoxide dimer Titanium stearate, diisopropoxy titanium distearate, tri-n-butoxy titanium monostearate, polyhydroxy titanium stearate tan acylate; titanium diisopropoxy bis (acetylacetonate), titanium tetraacetylacetonate, titanium geo Cutyloxybis (octylene glycolate), titanium diisopropoxybis (ethyl acetoacetate), titanium diisopropoxybis (triethanolaminate), titanium lac
- these titanium oxide precursors Prior to hydrolysis, these titanium oxide precursors have various ligands such as acetylacetone, aminoethanol, diethanolamine, triethanolamine, ethylenediamine, other amines, pyridinecarboxylic acid, tartaric acid, oxalic acid, lactic acid, glycolic acid, It may be mixed with other hydroxycarboxylic acid or the like to form a complex of a titanium oxide precursor, and the complex may be used for hydrolysis. Moreover, it is preferable that the titanium oxide precursor used for these baking methods is dissolved in a solvent and used as a solution.
- the solvent for dissolving the titanium oxide precursor water, alcohol (methanol, ethanol, n-propanol, isopropanol), THF and the like are preferable.
- the buffer layer forming component according to the present invention is a solution, it is preferable to contain 0.5 to 13 parts by mass of the buffer layer forming component with respect to 100 parts by mass of the solvent.
- the CVD method is called a chemical vapor deposition method, in which a gaseous source material (gas, liquid, solid) is supplied to a reaction chamber in the apparatus, and a chemical reaction (gas phase) is generated on the substrate surface.
- a gaseous source material gas, liquid, solid
- a chemical reaction gas phase
- a desired titanium oxide layer is deposited on a substrate by causing a phase reaction).
- Thermal CVD method, plasma CVD method, photo CVD method, respectively. is called.
- a buffer layer non-formation part is formed at the end of each first electrode.
- the buffer layer non-forming portion may be formed at any end portion of the first electrode, but is preferably formed continuously along one side of the first electrode.
- the buffer layer non-forming portion is used for connecting the first electrode and the second electrode in a later step.
- a method of forming the buffer layer non-forming portion a method of forming a buffer layer after arranging a covering member, a bar code method, a die coating method, a gravure coating method, an ink jet method capable of applying the buffer layer to a limited area Law.
- the width of the upper end buffer non-forming portion is preferably 0.01 to 3 mm in consideration of the photoelectric conversion efficiency per unit area of the module and the ease of forming the second electrode described later.
- the buffer layer according to the present invention is obtained by applying a coating solution for forming a buffer layer on a transparent conductive substrate and then drying or / and sintering. In general, it is preferable to dry or / and sinter immediately after applying the coating solution for forming the buffer layer on the transparent conductive substrate from the viewpoint of improving the conductivity.
- the buffer layer contains titanium oxide as long as the buffer layer has a —Ti—O— bond
- the buffer layer of the photoelectric conversion element of the present invention includes a bond layer unreacted buffer layer precursor.
- it may contain an organic substance such as an unreacted titanium oxide precursor.
- the conditions of the firing method for firing the buffer layer forming component according to the present invention to form the buffer layer are appropriately selected depending on the type of compound used.
- the firing temperature is preferably 200 to 700 ° C. 600 ° C. is more preferable.
- the firing time is preferably 0.5 to 120 minutes, more preferably 5 to 30 minutes.
- Method for forming photoelectric conversion layer [Method for Fabricating Semiconductor Layer]
- the semiconductor layer is formed on the aforementioned buffer layer.
- a suitable photoelectric conversion layer according to the present invention is obtained by aggregating a semiconductor having a sensitizing dye supported on the surface.
- a method for producing a semiconductor layer by applying or spraying a semiconductor dispersion or colloid solution (semiconductor-containing coating solution) on a conductive substrate A method (sol-gel method) in which a precursor of fine particles is applied on a conductive substrate, hydrolyzed with moisture (for example, moisture in the air), and then condensed (sol-gel method) can be used.
- the method (1) is preferred.
- the semiconductor according to the present invention is in the form of a film and is not held on a conductive substrate, it is preferable that the semiconductor layer be bonded to the conductive substrate to produce a semiconductor layer.
- a method of forming the semiconductor layer on the conductive substrate by baking using semiconductor fine particles can be given.
- the semiconductor sensitization (adsorption, filling into a porous layer, etc.) treatment with a dye is preferably performed after firing. It is particularly preferable to perform the compound adsorption treatment quickly after the firing and before the water is adsorbed to the semiconductor.
- a coating solution (semiconductor-containing coating solution) containing a semiconductor, preferably a fine powder of semiconductor, is prepared.
- the primary particle diameter is preferably 1 to 5000 nm, and more preferably 2 to 100 nm.
- the coating liquid containing the semiconductor fine powder can be prepared by dispersing the semiconductor fine powder in a solvent.
- the semiconductor fine powder dispersed in the solvent is dispersed in the form of primary particles.
- the solvent is not particularly limited as long as it can disperse the semiconductor fine powder.
- the solvent include water, an organic solvent, and a mixed solution of water and an organic solvent.
- organic solvents include alcohols such as methanol, ethanol, and isopropanol, ketones such as methyl ethyl ketone, acetone, and acetyl acetone, hydrocarbons such as hexane and cyclohexane, cellulose derivatives such as acetyl cellulose, nitrocellulose, acetylbutyl cellulose, ethyl cellulose, and methyl cellulose. Is used.
- a surfactant such as acetic acid and nitric acid
- an acid such as acetic acid and nitric acid
- a viscosity modifier such as a polyhydric alcohol such as polyethylene glycol
- a chelating agent such as acetylacetone
- the range of the concentration of the semiconductor fine powder in the solvent is preferably 0.1 to 70% by mass, and more preferably 0.1 to 30% by mass.
- the semiconductor-containing coating solution obtained as described above is applied or sprayed onto a conductive substrate, dried, etc., and then baked in air or in an inert gas to form a semiconductor layer ( (Also referred to as a semiconductor film).
- the coating method is not particularly limited, and examples thereof include known methods such as a doctor blade method, a squeegee method, a spin coating method, and a screen printing method.
- the film obtained by applying and drying a semiconductor-containing coating solution on a conductive substrate is composed of an aggregate of semiconductor fine particles, and the particle size of the fine particles corresponds to the primary particle size of the semiconductor fine powder used. It is.
- a semiconductor layer (semiconductor fine particle layer) formed on a conductive layer such as a conductive substrate in this manner generally has a low bonding strength with a conductive substrate and a bonding strength between fine particles, and a low mechanical strength. . For this reason, the semiconductor layer (semiconductor fine particle layer) is baked in order to increase the mechanical strength and form a semiconductor layer that is strongly fixed to the substrate.
- the semiconductor layer may have any structure, but is preferably a porous structure film (also referred to as a porous layer having voids).
- a porous structure film also referred to as a porous layer having voids.
- the porosity (D) of the semiconductor layer is not particularly limited, but is preferably 1 to 90% by volume, more preferably 10 to 80% by volume, and particularly preferably 20 to 70% by volume.
- the porosity (porosity) of the semiconductor layer means a porosity that is penetrable in the thickness direction of the semiconductor layer, and can be measured using a commercially available apparatus such as a mercury porosimeter (Shimadzu pore sizer 9220 type).
- the thickness of the semiconductor layer formed into a fired product film having a porous structure is not particularly limited, but is preferably at least 1 ⁇ m or more, and more preferably 2 to 30 ⁇ m. If it is such a range, it can become a semiconductor layer excellent in characteristics, such as permeability and conversion efficiency.
- the semiconductor layer may be a single layer formed of semiconductor fine particles having the same average particle diameter, or a multilayer film (layered structure) composed of semiconductor layers containing semiconductor fine particles having different average particle diameters and types. Also good.
- the firing conditions are not particularly limited. From the viewpoint of appropriately preparing the actual surface area of the fired film during the firing treatment and obtaining a fired film having the above porosity, the firing temperature is preferably lower than 900 ° C, more preferably 200 ° C to 850 ° C. The range is particularly preferably 450 ° C. to 800 ° C.
- the fine particles and the fine particle-substrate can be fixed by pressurization without performing a baking process at 250 ° C. or higher, or the substrate is Only the semiconductor layer can be heat-treated without heating.
- the firing time is preferably 10 seconds to 12 hours, more preferably 1 to 240 minutes, and particularly preferably 10 to 120 minutes.
- the firing atmosphere is not particularly limited, but usually the firing step is performed in air or in an inert gas (for example, argon, helium, nitrogen, etc.) atmosphere. The firing may be performed only once at a single temperature, or may be repeated twice or more by changing the temperature or time.
- the ratio of the actual surface area to the apparent surface area can be controlled by the particle size, specific surface area, firing temperature, and the like of the semiconductor fine particles.
- Plating or electrochemical plating using a titanium trichloride aqueous solution may be performed.
- the sensitizing dyes described above may be used alone or in combination, and other compounds (for example, US Pat. No. 4,684,537). No. 4,927,721, No. 5,084,365, No. 5,350,644, No. 5,463,057, No. 5,525,440 And compounds described in JP-A-7-249790, JP-A-2000-150007, etc.).
- the use of the photoelectric conversion element of the present invention is a solar cell to be described later
- two or more types of dyes having different absorption wavelengths are used so that the wavelength range of photoelectric conversion can be made as wide as possible to effectively use sunlight. It is preferable to use a mixture.
- the method for supporting the sensitizing dye on the semiconductor layer is not particularly limited, and a known method can be applied in the same manner or appropriately modified.
- a method in which a sensitizing dye is dissolved in an appropriate solvent and a well-dried semiconductor layer is immersed in the solution for a long time is generally used.
- a sensitizing treatment is carried out by using a plurality of sensitizing dyes in combination or other dyes in combination, a mixed solution of each dye may be prepared and used. A separate solution can be prepared and immersed in each solution in order.
- the order in which the sensitizing dye and the like are included in the semiconductor may be whatever. Or you may produce by mixing the microparticles
- the semiconductor sensitization treatment is performed by dissolving the sensitizing dye in an appropriate solvent as described above and immersing the substrate on which the semiconductor is baked in the solution.
- a substrate on which a semiconductor layer (also referred to as a semiconductor film) is formed by baking be subjected to pressure reduction treatment or heat treatment in advance to remove bubbles in the film.
- Such treatment allows the sensitizing dye to enter deep inside the semiconductor layer (semiconductor thin film), which is particularly preferable when the semiconductor layer (semiconductor thin film) is a porous structure film.
- the solvent used for dissolving the sensitizing dye is not particularly limited as long as it can dissolve the sensitizing dye and does not dissolve the semiconductor or react with the semiconductor. However, in order to prevent moisture and gas dissolved in the solvent from entering the semiconductor film and hindering sensitizing treatment such as adsorption of a sensitizing dye, it is preferable to deaerate and purify in advance.
- Solvents preferably used in dissolving the sensitizing dye include nitrile solvents such as acetonitrile, alcohol solvents such as methanol, ethanol, n-propanol, isopropanol and t-butyl alcohol, ketone solvents such as acetone and methyl ethyl ketone, diethyl Examples thereof include ether solvents such as ether, diisopropyl ether, tetrahydrofuran and 1,4-dioxane, and halogenated hydrocarbon solvents such as methylene chloride and 1,1,2-trichloroethane. These solvents may be used alone or in combination of two or more.
- acetonitrile, methanol, ethanol, n-propanol, isopropanol, t-butyl alcohol, acetone, methyl ethyl ketone, tetrahydrofuran and methylene chloride, and mixed solvents thereof such as acetonitrile / methanol mixed solvent, acetonitrile / ethanol mixed solvent, A mixed solvent of acetonitrile / t-butyl alcohol is preferred.
- the conditions for the sensitization processing according to the present invention are not particularly limited.
- the time for immersing the substrate in which the semiconductor is baked in the sensitizing dye-containing solution is deeply penetrated into the semiconductor layer (semiconductor film) to sufficiently advance adsorption and the like to sufficiently sensitize the semiconductor.
- the sensitizing treatment temperature is preferably 0 to 80 ° C., more preferably 20 to 50 ° C. .
- the sensitizing treatment time is preferably 1 to 24 hours, and more preferably 2 to 6 hours.
- the sensitization treatment at room temperature (25 ° C.) for 2 to 48 hours, particularly 3 to 24 hours.
- This effect is particularly remarkable when the semiconductor layer is a porous structure film.
- the immersion time is a value under the condition of 25 ° C., and is not limited to the above when the temperature condition is changed.
- the solution containing the dye of the present invention may be heated to a temperature that does not boil as long as the dye does not decompose.
- the preferred temperature range is 5 to 100 ° C., more preferably 25 to 80 ° C., but this is not the case when the solvent boils in the temperature range as described above.
- step (2) “Contacting the conductive polymer precursor to the photoelectric conversion layer in the presence of an oxidizing agent” in this specification)
- the step (2) in the method for producing a photoelectric conversion element according to the present invention includes a conductive polymer precursor as a precursor of the photoelectric conversion layer prepared in the step (1) and a conductive polymer constituting the hole transport layer. The body is contacted in the presence of an oxidant.
- the semiconductor layer that is a constituent element of the photoelectric conversion layer is not a porous body, a method of forming an oxidant and a conductive polymer precursor and, if necessary, the electrolyte described above on the photoelectric conversion layer, or A method in which a polymer is formed by applying a solution containing a oxidant and a monomer or prepolymer in the form of a precursor or a prepolymer, to which a solvent or an electrolyte is added, if necessary, on the photoelectric conversion layer and then polymerizing.
- the semiconductor layer that is a constituent element of the photoelectric conversion layer is a porous body
- the sensitization that is adsorbed on the surface of the semiconductor layer so that the hole transport layer covers the surface of the porous body It is preferable that the dye and the hole transport layer are in contact with each other in the presence of an oxidant.
- the precursor and the oxidant of the hole transport layer and the oxidant are added as necessary up to the inside or gaps of the porous body. It is preferable to polymerize the conductive polymer by impregnation and / or application so that the solution containing the electrolyte to be permeated and coat almost the entire surface of the porous body.
- this process (2) makes the photoelectric conversion layer produced at the said process (1) contact the solution which contains a conductive polymer precursor and an oxidizing agent in the ratio of following Numerical formula (1). preferable.
- [Ox] is the molar concentration (mol / L) of the oxidizing agent
- [M] is the molar concentration (mol / L) of the conductive polymer precursor.
- a solution containing a oxidant and a monomer or prepolymer that is a precursor of the hole transport layer and a solvent or an electrolyte as necessary is applied on the photoelectric conversion layer, and then polymerized to form a polymer. And / or impregnation and / or so that a solution containing the precursor of the hole transport layer and the oxidizing agent and an electrolyte added if necessary penetrates and covers almost the entire surface of the porous body.
- a method of coating and polymerizing the conductive polymer precursor is more preferable.
- the semiconductor layer that is a constituent element of the photoelectric conversion layer is preferably a porous body
- an impregnation method in which the photoelectric conversion layer is impregnated with a solution containing a conductive polymer precursor and an oxidizing agent is particularly preferable.
- the composition of the solution applied to or impregnated into the photoelectric conversion layer is such that the oxidizing agent is 10 to 10,000 parts by mass, the supporting electrolyte is 100 to 100,000 parts by mass, and the solvent is 5000 to 100 parts by mass with respect to 100 parts by mass of the conductive polymer precursor.
- the amount is preferably 200,000 parts by mass, more preferably 10 to 1000 parts by mass of the oxidizing agent, 500 to 10,000 parts by mass of the supporting electrolyte, and 10,000 to 1000000 parts by mass of the solvent.
- the solvent is not particularly limited as long as it can dissolve the supporting electrolyte and the monomer or multimer thereof, butylene oxide, chloroform, cyclohexanone, acetonitrile, tetrahydrofuran, propylene carbonate, dichloromethane, o-dichlorobenzene.
- the said solvent may be used individually and may be used in mixture of 2 or more types.
- a coating method when the above solution is applied to the photoelectric conversion layer to form a hole transport layer specifically, dipping, dripping, doctor blade, spin coating, brush coating, spray coating, roll coater, Air knife coating, curtain coating, wire bar coating, gravure coating, extrusion coating using a hopper described in US Pat. No. 2,681,294, and multilayer simultaneous coating methods described in US Pat. Nos. 2,761,418, 3,508,947, and 2,761791
- these various coating methods can be used.
- the coating may be repeated by repeating such coating operation.
- the number of coatings in this case is not particularly limited, and can be appropriately selected according to the desired thickness of the hole transport layer.
- step (3) “Lighting the sensitizing dye in the presence of an oxidant to polymerize the conductive polymer precursor to form a hole transport layer”
- step (3) in the method for producing a photoelectric conversion element according to the present invention, after the step (2), the sensitizing dye is irradiated with light in the presence of an oxidizing agent to polymerize the conductive polymer precursor. A hole transport layer is formed.
- a sensitizing dye in a state in which a photoelectric conversion layer is impregnated in a solution in which a solvent or an electrolyte is added as necessary in the form of a monomer or prepolymer (multimer) which is a precursor of an oxidizing agent and a hole transport layer It is preferable to irradiate light. Moreover, you may irradiate light with respect to a sensitizing dye from the outside in the state which apply
- the conditions for irradiating light to the photoelectric conversion layer are not particularly limited, but the wavelength of the irradiated light includes the absorption wavelength of the sensitizing dye. Is preferred. Specifically, it is preferable that the wavelength exceeds 400 nm. More preferably, a light source having a wavelength of more than 400 nm and not more than 1100 nm, more preferably more than 420 nm and not more than 1100 nm is used. The intensity of the light is preferably 10 ⁇ 150mW / cm 2, and more preferably 20 ⁇ 80mW / cm 2.
- the time for irradiating the sensitizing dye with light is preferably 0.1 to 30 minutes, and more preferably 0.5 to 15 minutes.
- the time for irradiating the sensitizing dye with light is preferably 0.1 to 30 minutes, and more preferably 0.5 to 15 minutes.
- the wavelength for the sensitizing dye When a wavelength of 400 nm or less is used as a wavelength for irradiating light to the sensitizing dye, titanium oxide is excited, so that a photocatalytic action works and decomposes the dye. Furthermore, although there is a slight difference depending on the dye, the longer wavelength light transmits light more deeply into the titania pores, so that the polymerization proceeds more uniformly. On the other hand, if the wavelength of the light source is too long, the dye is not absorbed and polymerization does not proceed. Therefore, the wavelength is set in the above range. In addition, the amount of light is set in the above range as the amount of light that is considered necessary for transmitting light to the depth of the pores of titanium oxide in the same manner as described above. Furthermore, as for the irradiation time, it indicates the time during which the polymerization proceeds sufficiently within the above range.
- a xenon lamp, a halogen lamp, LED, etc. are mentioned as a light source which concerns on this invention.
- the sensitizing dye adsorbed on the photoelectric conversion layer is irradiated with light, the sensitizing dye is excited by light, and the excited electrons are consumed by the oxidant.
- the dye is in a cationic state. It is considered that the sensitizing dye in the cationic state extracts electrons from the conductive polymer precursor, whereby the conductive polymer precursor is cationized and plays a role as a polymerization initiator.
- a conductive polymer can be formed by photopolymerization, so that the polymerization time can be shortened compared to electrolytic polymerization, and a sufficient amount and dense weight can be easily deposited on the surface of the photoelectric conversion layer (semiconductor layer). Combined layers can be formed. Moreover, according to the said method, the decomposition
- the temperature range for applying and / or impregnating the solution to be applied to or impregnating the photoelectric conversion layer is preferably set to a range in which the solvent does not solidify or bump, and is generally ⁇ 10 ° C. to 60 ° C. .
- step (3) after forming a hole transport layer on the photoelectric conversion layer, if necessary, a step of washing by a known method using the above solvent, and / or 25 to 150 ° C., 0.2 to You may perform the process dried on condition of 12 hours.
- step (3) if necessary, after forming a conductive polymer obtained by photopolymerization of the conductive polymer precursor and providing a hole transport layer on the surface of the photoelectric conversion layer, the photoelectric conversion layer is impregnated and / or Alternatively, a semiconductor electrode in which a hole transport layer is formed in a solution in which a solvent used for coating and at least one selected from the group consisting of the supporting electrolyte and the organic salt is mixed with a conductive polymer
- it may be immersed at ⁇ 10 to 70 ° C. for 0.1 to 2 hours. In that case, it is preferable to perform the step (4) described later after being immersed and then allowed to stand for 0.01 to 24 hours by natural drying.
- Step (4) in the method for producing a photoelectric conversion element according to the present invention is a step of forming a second electrode on the hole transport layer after the step (3).
- the second electrode forming method according to the present invention is not particularly limited, and a known method can be applied.
- a method such as vapor deposition (including vacuum vapor deposition), sputtering, coating, screen printing, or the like is preferably used.
- the photoelectric conversion element of the present invention obtained as described above can absorb light efficiently. Specifically, the absorbance (A 1000 ) at 1000 nm of the photoelectric conversion element is expressed by the following formula (2):
- a 1000 is the absorbance of the photoelectric conversion element at 1000 nm;
- FT SC is the film thickness ( ⁇ m) of the semiconductor layer.
- Step (5) in the method for producing a photoelectric conversion element according to the present invention is a process of electrically connecting at least two or more photoelectric conversion elements.
- the electrical connection method of the photoelectric conversion elements is not particularly limited, and a known method can be applied. For example, connection by a conductive paste such as silver, copper, or carbon can be mentioned, but it is preferable to connect in series. More specifically, (a) As shown in FIG. 1, in two adjacent photoelectric conversion elements 10, the end portion 31 of the first electrode 30 of one photoelectric conversion element is adjacent to the adjacent photoelectric conversion element 10. It is preferable that the end portion 71 of the second electrode 70 is connected (connected) in series.
- the end 31 of the first electrode 30 of one photoelectric conversion element is connected (connected) to the end 71 of the second electrode 70 of the adjacent photoelectric conversion element 10 via a conductive member.
- a conductive member such as a conductive paste
- the form (a) is particularly preferred. That is, in the step of electrically connecting, at least two photoelectric conversion elements adjacent to each other among the photoelectric conversion elements from the viewpoint of electric resistance reduction are the one end portion of the first electrode of one photoelectric conversion element and the photoelectric conversion element. And connecting one end of the second electrode of the adjacent photoelectric conversion element to each other.
- a conductive member such as a conductive paste
- the step (4) and the step (5) can be performed simultaneously.
- the size of the entire photoelectric conversion element module can be made more compact.
- the manufacturing process can be simplified.
- the method for forming the second electrode is not particularly limited, and a known method is applied, but the method shown in the above step (4) can be applied.
- connection between the first electrode and the second electrode of the adjacent photoelectric conversion elements is preferably a series connection.
- the photoelectric conversion element of this invention can be used especially suitably for a solar cell. Therefore, this invention also provides the solar cell characterized by having the photoelectric conversion element of this invention, or the photoelectric conversion element manufactured by the method of this invention.
- the solar cell of the present invention has the photoelectric conversion element of the present invention.
- the solar cell of the present invention comprises the photoelectric conversion element of the present invention, and has a structure in which optimal design and circuit design are performed for sunlight, and optimal photoelectric conversion is performed when sunlight is used as a light source.
- the semiconductor is dye-sensitized and can be irradiated with sunlight.
- the photoelectric conversion layer, the hole transport layer and the second electrode are housed in a case and sealed, or the whole is sealed with a resin.
- the sensitizing dye carried on the semiconductor is excited by absorbing the irradiated light or electromagnetic wave. Electrons generated by excitation move to the semiconductor, and then move to the second electrode via the first electrode and the external load, and are supplied to the hole transport layer.
- the sensitizing dye that has moved the electrons to the semiconductor is an oxidant, but is reduced by the supply of electrons from the second electrode via the polymer of the hole transport layer, thereby returning to the original state.
- the polymer of the hole transport layer is oxidized and returned to a state where it can be reduced again by the electrons supplied from the second electrode. In this way, electrons flow and a solar cell using the photoelectric conversion element of the present invention can be configured.
- a transparent conductive layer (FTO) (coating amount: 7 g / m 2 substrate) is formed on a glass substrate by sputtering fluorine-doped tin oxide (FTO) having a sheet resistance of 20 ⁇ / ⁇ (square) as a first electrode.
- FTO fluorine-doped tin oxide
- a glass substrate (first electrode substrate) was obtained.
- the size of the glass substrate was 10 mm ⁇ 15 mm ⁇ 1.0 mm, and each size of the first electrode was 10 mm ⁇ 10 mm ⁇ 0.1 ⁇ m.
- TC100 manufactured by Matsumoto Kosho
- titanium diisopropoxybis (acetylacetonate) was dropped.
- a titanium oxide paste (anatase type, primary average particle size (microscope observation average) 18 nm, ethyl cellulose dispersed in 10% acetylacetone water) was applied by a screen printing method (application area: 7 mm ⁇ 7 mm). .
- the obtained coating film was baked at 200 ° C. for 10 minutes and at 500 ° C. for 15 minutes, and a 2.5 ⁇ m-thick titanium oxide porous layer (porous semiconductor layer having a porosity (D) of 60% by volume) ) was formed.
- the sensitizing dye used was of the following structural formula having an absorption band at 350 to 650 nm.
- the conductive polymer precursor M1-1 2,2′-bis [3,4- (ethylenebisoxy) thiophene]) is 1 ⁇ 10 ⁇ 3 (mol / l)
- Li [(CF 3 SO 2 ) 2 N] was dissolved in acetonitrile at a ratio of 0.1 (mol / l) to prepare a solution, and then 30 wt% hydrogen peroxide solution was added to the solution so as to be 1 v / v%.
- the prepared semiconductor electrode was immersed. Then, photopolymerization was performed by irradiating light from a xenon lamp through a sharp cut filter (manufactured by HOYA: S-L42) for 2 minutes from the outside of the semiconductor electrode.
- the light irradiation condition was a light intensity of 22 mW / cm 2 .
- new absorption appeared at 600 to 1100 nm, and it was confirmed that the conductive polymer precursor was polymerized to form a conductive polymer.
- the semiconductor electrode on which the hole transport layer was formed by polymerization was washed with acetonitrile and then dried to obtain a hole transport layer.
- the obtained hole transport layer was a polymer film insoluble in the solvent.
- the semiconductor electrode (semiconductor electrode / hole transport layer) on which the hole transport layer was formed was replaced with Li [(CF 3 SO 2 ) 2 N] at 15 ⁇ 10 ⁇ 3 (mol / l), tert-butylpyridine.
- Li [(CF 3 SO 2 ) 2 N] at 15 ⁇ 10 ⁇ 3 (mol / l)
- tert-butylpyridine was immersed in an acetonitrile solution containing 50 ⁇ 10 ⁇ 3 (mol / l) for 10 minutes.
- gold was further deposited by 60 nm by a vacuum deposition method to form a second electrode. Thereby, a photoelectric conversion element SC-1 was obtained.
- Photoelectric conversion elements SC-2 to 5 were produced in the same manner except that the oxidizing agent was changed to iron (III) paratoluenesulfonate, AgNO 3 , cumene hydroperoxide, KMnO 4 in the production of photoelectric conversion element SC-1. .
- Photoelectric conversion element SC-6 was produced in the same manner as in the production of photoelectric conversion element SC-1, except that photopolymerization was performed in a state where oxygen was sufficiently bubbled as an oxidizing agent.
- Photoelectric conversion element SC-7 was produced in the same manner as in the production of photoelectric conversion element SC-6, except that the oxidizing agent was changed to ozone.
- Photoelectric conversion elements SC-8 and 9 were produced in the same manner as in the production of the photoelectric conversion element SC-1, except that the conductive polymer precursor was changed to M1-4 and M1-26.
- a photoelectric conversion element SC-10 was prepared in the same manner as in the production of the photoelectric conversion element SC-1, except that a light source that cut light of 400 nm or more was used.
- Photoelectric conversion element SC-11 was produced in the same manner as in the production of photoelectric conversion element SC-1, except that a light source that cut light of 400 nm or less was used.
- the semiconductor electrode contains a conductive polymer precursor M1-1 (bis-EDOT) at a rate of 1 ⁇ 10 ⁇ 3 (mol / l), and Li [( CF 3 SO 2 ) 2 N] was immersed in an acetonitrile solution (electropolymerization solution) containing 0.1 (mol / l).
- the semiconductor electrode was connected to the working electrode, the platinum wire was connected to the counter electrode, and Ag / Ag + (AgNO 3 0.01M) was connected to the reference electrode, respectively, and the holding voltage was set to ⁇ 0.16V.
- the voltage was held for 30 minutes to form the hole transport layer 51 on the surface of the semiconductor electrode.
- the obtained semiconductor electrode / hole transport layer was washed with acetonitrile and dried, and then a photoelectric conversion element SC-13 was produced in the same manner except that the hole transport layer was obtained.
- a 100 mm x 2 mm Kapton tape is pasted on each of the obtained first electrodes so as to cover the right end of the first electrode, and 15 mm x 30 mm Kapton tape is similarly attached so as to cover the upper end of the first electrode.
- TC100 manufactured by Matsumoto Kyosho
- TiN Titanium diisopropoxybis (acetylacetonate) was dropped and applied by spin coating, and then the Kapton tape was removed and heated at 450 ° C. for 8 minutes.
- buffer layers (porosity (C): 1.0 vol%) 31, 32, 33 made of a thin layer of titanium oxide having a thickness of 50 nm were formed on the transparent conductive film (FTO).
- Titanium oxide paste (anatase type, primary average particle diameter (microscope observation average) 18 nm, ethyl cellulose dispersed in 10% acetylacetone water) was screen printed on the buffer layers 31, 32, 33 (application area: 70 mm ⁇ 25 mm).
- the obtained coating film was baked at 200 ° C. for 10 minutes and at 500 ° C. for 15 minutes, and a 2.5 ⁇ m-thick titanium oxide porous layer (porous semiconductor layer having a porosity (D) of 60% by volume) ) was formed.
- the sensitizing dye used was of the following structural formula having an absorption band at 350 to 650 nm.
- the conductive polymer precursor M1-1 was dissolved in acetonitrile at a ratio of 1 ⁇ 10 ⁇ 3 (mol / l) and Li [(CF 3 SO 2 ) 2 N] at a ratio of 0.1 (mol / l). Then, after preparing the solution, 30 wt% hydrogen peroxide water was added to the solution so as to be 1 v / v%, and the produced semiconductor electrode was immersed therein. Then, the semiconductor electrode was irradiated with light passing through a sharp cut filter (manufactured by HOYA: S-L42) that cuts a wavelength of 420 nm or less from the xenon lamp for 2 minutes to perform photopolymerization.
- a sharp cut filter manufactured by HOYA: S-L42
- the light irradiation condition was a light intensity of 22 mW / cm 2 .
- new absorption appeared at 600 to 1100 nm, and it was confirmed that the conductive polymer precursor was polymerized to form a conductive polymer.
- the semiconductor electrode on which the hole transport layer was formed by polymerization was washed with acetonitrile and then dried to obtain hole transport layers 51, 52, and 53.
- the obtained hole transport layer was a polymer film insoluble in the solvent.
- the semiconductor electrode (semiconductor electrode / hole transport layer) on which the hole transport layer was formed was replaced with Li [(CF 3 SO 2 ) 2 N] at 15 ⁇ 10 ⁇ 3 (mol / l), tert-butylpyridine.
- Li [(CF 3 SO 2 ) 2 N] at 15 ⁇ 10 ⁇ 3 (mol / l), tert-butylpyridine.
- gold was further deposited by 60 nm by a vacuum deposition method to form a second electrode.
- the end of the first electrode covered with the Kapton tape is connected to the second electrode of the photoelectric conversion element adjacent to the first electrode. Vapor deposition was performed.
- a photoelectric conversion element module SM-1 was obtained.
- Example 6 A photoelectric conversion element module SM-6 was prepared in the same manner as in the production of the photoelectric conversion element module SM-1, except that photopolymerization was performed in a state where oxygen was sufficiently bubbled as an oxidizing agent.
- Photoelectric conversion element module SM-7 was produced in the same manner as in the production of photoelectric conversion element module SM-6, except that the oxidizing agent was changed to ozone.
- Photoelectric conversion element modules SM-8 and 9 were produced in the same manner as in the production of the photoelectric conversion element module SM-1, except that the conductive polymer precursor was changed to M1-4 and M1-26.
- the photoelectric conversion element module SM-10 was manufactured in the same manner as in the manufacture of the photoelectric conversion element module SM-1, except that a light source that cut light of 400 nm or more was used.
- the photoelectric conversion element module SM-11 was manufactured in the same manner as in the manufacture of the photoelectric conversion element module SM-1, except that a light source that cut light of 400 nm or less was used.
- Example 12 FTO was sputtered onto the glass substrate used in Example 1 to prepare first electrodes 201 to 210 of 90 mm ⁇ 9 mm ⁇ 100 nm.
- the distance (X) between the electrodes was 0.5 mm.
- a 100 mm ⁇ 1 mm Kapton tape is pasted on each of the obtained first electrodes so as to cover the right end of the first electrode, and 15 mm ⁇ 30 mm Kapton tape is similarly attached so as to cover the upper end of the first electrode.
- TC100 manufactured by Matsumoto Kyosho
- Titanium diisopropoxybis (acetylacetonate) was dropped and applied by spin coating, and then the Kapton tape was removed and heated at 450 ° C. for 8 minutes.
- buffer layers pH (C): 1.0 vol%) 301 to 310 made of a thin layer of titanium oxide having a thickness of 50 nm were formed on the transparent conductive film (FTO).
- a titanium oxide paste (anatase type, primary average particle diameter (microscope observation average) 18 nm, ethyl cellulose dispersed in 10% acetylacetone water) was screen printed on the buffer layer 301 to 310 (application area: 70 mm ⁇ 7. 5 mm).
- the obtained coating film was baked at 200 ° C. for 10 minutes and at 500 ° C. for 15 minutes, and a 2.5 ⁇ m-thick titanium oxide porous layer (porous semiconductor layer having a porosity (D) of 60% by volume) ) was formed.
- a photoelectric conversion element module SM-12 was produced in the same manner as in Example 1.
- the semiconductor electrode contains a conductive polymer precursor (bis-EDOT) at a rate of 1 ⁇ 10 ⁇ 3 (mol / l), and Li [(CF 3 SO 2 ) it was immersed in an acetonitrile solution containing at a ratio of 2 N] a 0.1 (mol / l) (electrolytic polymerization solution).
- the first electrode 21 was connected to the working electrode, the platinum wire was connected to the counter electrode, and Ag / Ag + (AgNO 3 0.01M) was connected to the reference electrode, respectively, and the holding voltage was set to ⁇ 0.16V.
- the voltage was maintained for 30 minutes to form the hole transport layer 51 on the surface of the semiconductor electrode.
- the working electrode was reconnected to the first electrode 22, and the voltage was maintained under the same conditions to obtain the hole transport layer 52.
- a hole transport layer 53 was obtained.
- a photoelectric conversion element module SM-13 was produced in the same manner except that a hole transport layer was obtained.
- compositions of the photoelectric conversion elements SC-1 to 11 and 13 and the photoelectric conversion element modules SM-1 to SM-13 are shown in Table 2 below.
- the photoelectric conversion element and the photoelectric conversion element module produced in the above-mentioned examples and comparative examples were converted from the xenon lamp to the AM filter (AM-1. AM-1) using the solar simulator (manufactured by Eihiro Seiki). 5) Pseudo sunlight having an intensity of 100 mW / cm 2 was irradiated. Then, the current-voltage characteristics of the photoelectric conversion element at room temperature were measured using an IV tester, and the short circuit current density (Jsc), the open circuit voltage (Voc), and the form factor (FF) were measured. . These values were applied to the following formula to determine the photoelectric conversion efficiency ⁇ c (%) of the photoelectric conversion element and the photoelectric conversion element module and the photoelectric conversion efficiency ⁇ m of the module.
- P is the incident light intensity [mW / cm 2 ]
- Voc is the open circuit voltage [V]
- Jsc is the short-circuit current density [mA ⁇ cm ⁇ 2 ]
- F.V. F. Indicates a fill factor.
- the photoelectric conversion efficiency ( ⁇ m ) of the module according to the present invention exhibits a photoelectric conversion efficiency of 65 to 75% with respect to the photoelectric conversion efficiency ( ⁇ C ) of the photoelectric conversion element of the reference example. It was.
- the photoelectric conversion efficiency ( ⁇ m ) of the module with respect to the photoelectric conversion efficiency ( ⁇ C ) of the photoelectric conversion element showed a remarkable decrease of about 17%. This is because the photoelectric conversion element is not easily affected by the sheet resistance of the first electrode because the first electrode is relatively small.
- the hole transport layer is formed by photoelectrolytic polymerization, the hole transport has an appropriate uniformity.
- the hole transport layer is strongly influenced by the sheet resistance of the first electrode when the hole transport layer is formed by photoelectrolytic polymerization. This is considered because the layer cannot be polymerized uniformly. From the above results, it can be expected that the photoelectric conversion element module according to the present invention can overcome the problem that a module having high photoelectric conversion efficiency that the conventional invention has cannot be manufactured. This is one of the characteristics of the present invention.
- a very uniform hole transport layer is formed for an electrode having a relatively large area. It can be considered that this is achieved by reducing the area of the connection portion of each photoelectric conversion element, that is, the portion that does not contribute to power generation.
- the area of the connection portion of each photoelectric conversion element that is, the portion that does not contribute to power generation Increases area. Therefore, it is considered that the module according to the present invention exhibits higher photoelectric conversion efficiency than when the photoelectric conversion elements are connected in series.
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Abstract
Description
前記正孔輸送層は、酸化剤存在下で、前記光電変換層と導電性高分子前駆体とを接触した後、前記増感色素に光を照射することにより前記導電性高分子前駆体を重合することにより形成することを特徴とする光電変換素子モジュールにより上記目的を達成できる。
本発明に係る光電変換素子モジュールの好ましい構成について、図1を参照しながら説明する。図1は、本願発明の光電変換素子モジュールの一例を示す模式断面図である。図1に示すように、光電変換素子モジュール100は、2以上の光電変換素子10が電気的に接続されてなる。ここで、各光電変換素子10は、基板20、第一電極30、バッファ層40、光電変換層50、正孔輸送層60および対極である第二電極70により構成されている。光電変換層50は、半導体(図示せず)および増感色素(図示せず)を含有する。各光電変換素子10は、共通の基板20を有し、当該基板20上に、第一電極30、バッファ層40、光電変換層50、正孔輸送層60および第二電極70がこの順で形成される。また、上述したように、光電変換素子10は、隣接する光電変換素子10と電気的に接続されるが、この際、接続形態は特に制限されないが、直列で接続されることが好ましい。より具体的には、(a)図1に示されるように、隣接する2つの光電変換素子10において、一方の光電変換素子の第一電極30の端部31が、隣接する光電変換素子10の第二電極70の端部71とが直列で連結(接続)した形態が好ましい。または、(b)一方の光電変換素子の第一電極30の端部31が、隣接する光電変換素子10の第二電極70の端部71とが導電性部材を介して連結(接続)した形態も好ましく使用される。これらのうち、(a)の形態が特に好ましい。すなわち、光電子変換素子のうちの少なくとも互いに隣接する二つの光電変換素子は、一つの光電変換素子の第一電極の一端部と前記光電変換素子と隣接する光電変換素子の第二電極の一端部とが接続されていることが好ましい。
本発明に係る基板は、光入射方向の側に設けられ、光電変換素子の光電変換効率の観点から、透明基板が好ましく、表面に第一電極が形成された透明導電性基板がより好ましく、光透過率が10%以上であることがさらに好ましく、更により好ましくは50%以上であり、特に80%~100%であることが好ましい。
本発明に係る第一電極は、基板と光電変換層との間に配置される。ここで、第一電極は、基板の光入射方向に対して反対側となる一方の面上に設けられる。第一電極としては、その光透過率が80%以上、さらに90%以上(上限:100%)のものが好ましく用いられる。光透過率は、上記基板の説明の記載と同様のものである。
本発明に係る第二電極は、導電性を有するものであればよく、任意の導電性材料が用いられる。絶縁性の物質でも、正孔輸送層に面している側に導電性物質層が設置されていれば、これも使用可能である。また、第二電極は、正孔輸送層との接触性が良いことが好ましい。第二電極は、正孔輸送層との仕事関数の差が小さく、化学的に安定であることも好ましい。このような材料としては、特に制限されないが、金、銀、銅、アルミニウム、白金、ロジウム、マグネシウム、インジウム等の金属薄膜、炭素、カーボンブラック、導電性高分子、導電性の金属酸化物(インジウム-スズ複合酸化物、酸化スズにフッ素をドープしたもの等)等の有機導電体などが挙げられる。また、第二電極の平均厚みもまた、特に制限されないが、10~1000nmであることが好ましい。また、第二電極の表面抵抗は、特に制限されないが、低いことが好ましい。具体的には、第二電極の表面抵抗の範囲は、好ましくは80Ω/□(square)以下であり、さらに好ましくは20Ω/□(square)以下である。なお、第二電極の表面抵抗の下限は、可能な限り低いことが好ましいため、特に規定する必要はないが、0.01Ω/□(square)以上であれば十分である。
本願発明に係る光電変換素子において、短絡防止手段や整流作用として、膜状(層状)をなし、第一電極と光電変換層(半導体層)との間に位置するバッファ層を有することが好ましい。
本発明に係る光電変換層は、半導体および増感色素を含有し、当該増感色素を担持した当該半導体を含有する半導体層からなることが好ましい。
本発明に係る半導体は、シリコン、ゲルマニウムのような単体、周期表(元素周期表ともいう)の第3族~第5族、第13族~第15族の元素を有する化合物、金属酸化物、金属硫化物、金属セレン化物、または金属窒化物等を使用することができる。
本発明に係る増感色素は、上記の半導体の増感処理により、半導体に担持され、かつ光照射時、光励起され起電力を生じ得るものであり、アリールアミン系色素が好ましく、下記一般式(1)で示される化合物がより好ましい。
本発明に係る正孔輸送層は、光励起によって酸化された増感色素に電子を供給して還元し、増感色素との界面で生じた正孔を第二電極へ輸送する機能を有する。正孔輸送層は、多孔質の半導体層上に形成された層状部分だけでなく、多孔質の半導体層の空隙内部に充填されうることが好ましい。
に示される繰り返し単位を有することが好ましい。
本発明の第二は、基板、第一電極、半導体および増感色素を含有する光電変換層、導電性高分子を有する正孔輸送層、ならびに第二電極の順で積層された光電変換素子が、2つ以上電気的に接続されてなる光電変換素子モジュールの製造方法において、前記第一電極上に前記光電変換層を形成することと、酸化剤存在下で前記光電変換層に導電性高分子前駆体を接触することと、前記酸化剤存在下で前記増感色素に光を照射して前記導電性高分子前駆体を重合して正孔輸送層を形成することと、前記正孔輸送層上に前記第二電極を形成することと、少なくとも2つ以上の前記光電変換素子を電気的に接続することと、を含む光電変換素子モジュールの製造方法である。
「第一電極上に光電変換層を形成すること(以下、本明細書中では工程(1)と称する)」
本発明に係る光電変換素子の製造方法において、第一電極を表面に備えた基板上に前記光電変換層を形成する工程(1)は、基板上に第一電極を形成する第一電極の製造方法と、光電変換層を形成する方法とに分けられ、必要により基板上に第一電極を形成した後、バッファ層を形成する方法を設けてもよい。以下、各方法について詳説する。
本発明に係る第一電極の製造方法、すなわち一つの基材の上に複数の第一電極(または透明導電層とも称する。)を形成する方法としては、透明導電層の材料に応じて適当な方法を選択できる。このような方法としては、例えば、スパッタ法やCVD法(気相成長法)、SPD法(スプレー熱分解堆積法)、蒸着法などが挙げられる。これらの方法により、ITO、FTO、SnO2などの酸化物半導体からなる薄膜を形成する。当該透明導電層は、厚過ぎると光透過性が劣り、一方、薄過ぎると導電性が劣ってしまうことになる。このため、光透過性と導電性の機能を両立させることを考慮すると、透明導電層は、0.1~5μm程度の膜厚範囲であることが好ましい。モジュールの単位面積当たりの光電変換効率を考慮すると当該基板の大きさは、縦50~3000mm、横50~3000mm、厚さ0.1~100mmであることが好ましい。また、各光電変換素子の大きさもまた特に制限されないが、例えば、光電変換素子が、基板上に、好ましくは2~300枚、より好ましくは10~100枚、並べられるような大きさであることが好ましい。このような大きさであれば、光電変換素子モジュールが十分な発電性能を発揮し、また、発電に寄与しない部分の面積も少なくて済む。または、各第一電極の大きさは、酸化物半導体の抵抗や発電に寄与する面積を考慮すると、縦(短いほうの辺)を1としたとき、横(長いほうの辺)が2~100の割合であることが好ましい。また、各第一電極間の距離(図1中の“X”)は発電に寄与しない部分の面積を減らし、十分な光電変換効率達成することを考慮するとなるべく短いほうが好ましいが、後の工程にある第二電極の形成を考慮すると0.001~10mmであることが好ましく、0.1~1mmであることがより好ましい。
本発明に係るバッファ層を形成する方法は、バッファ層形成成分であるバッファ層前駆体を第一電極上に被覆させて必要により熱処理を行う方法が挙げられる。具体的には、本発明に係る第一電極が基板表面に形成された透明導電性基板の(第一電極)上にバッファ層形成成分の(塗布)層を形成した後、CVD法または焼成法により反応が進行してバッファ層が形成される方法や、バッファ層形成用の塗布液を用いたインクジェット法やスピンコート法による塗布、原子層堆積(ALD)法が好ましい。なかでも、後述する本発明に係る第一電極が基板表面に形成された透明導電性基板の(第一電極)上に、バッファ層形成成分の(塗布)層を形成した後、CVD法または焼成法により反応が進行してバッファ層が形成される方法がより好ましい。ここでバッファ層形成成分とは化学反応によりバッファ層となる化合物のことをいうものである。
[半導体層の作製方法]
以下、本発明に係る光電変換層形成工程(1)における半導体層の作製方法について以下説明する。半導体層は前述のバッファ層上に形成する。また、上述したように、本発明に係る好適な光電変換層は、表面に増感色素が担持された半導体を凝集したものである。
まず、半導体、好ましくは半導体の微粉末を含む塗布液(半導体含有塗布液)を調製する。この半導体微粉末はその1次粒子径が微細な程好ましく、その1次粒子径は1~5000nmが好ましく、さらに好ましくは2~100nmである。半導体微粉末を含む塗布液は、半導体微粉末を溶媒中に分散させることによって調製することができる。
上記のようにして得られた半導体含有塗布液を、導電性基板上に塗布または吹き付け、乾燥等を行った後、空気中または不活性ガス中で焼成して、導電性基板上に半導体層(半導体膜とも言う)が形成される。ここで、塗布方法としては、特に制限されないが、ドクターブレード法、スキージ法、スピンコート法、スクリーン印刷法など公知の方法が挙げられる。
本発明に係る増感処理を行う場合、上記に記載した増感色素を単独で用いてもよいし、複数を併用してもよく、また他の化合物(例えば、米国特許第4,684,537号明細書、同4,927,721号明細書、同5,084,365号明細書、同5,350,644号明細書、同5,463,057号明細書、同5,525,440号明細書、特開平7-249790号公報、特開2000-150007号公報等に記載の化合物)と混合して用いることもできる。
本発明に係る増感処理の条件は、特に制限されない。例えば、半導体を焼成した基板を増感色素含有溶液に浸漬する時間は、半導体層(半導体膜)に深く進入して吸着等を充分に進行させ、半導体を十分に増感させることが好ましい。また、溶液中での色素の分解等により生成して分解物が色素の吸着を妨害することを抑制する観点から、増感処理温度は、0~80℃が好ましく、20~50℃がより好ましい。また、同様の観点から、増感処理時間は、1~24時間が好ましく、2~6時間がより好ましい。特に、室温(25℃)条件下で2~48時間、特に3~24時間、増感処理を行うことが好ましい。この効果は、特に半導体層が多孔質構造膜である場合において顕著である。ただし、浸漬時間については25℃条件での値であり、温度条件を変化させた場合には、上記の限りではない。
本発明に係る光電変換素子の製造方法における工程(2)は、上記工程(1)で作製した光電変換層と、正孔輸送層を構成する導電性高分子の前駆体として導電性高分子前駆体と、を酸化剤存在下で接触させる。すなわち、光電変換層の構成要素である半導体層が多孔質体でない場合は、酸化剤および導電性高分子前駆体と、必要により上記説明した電解質とを当該光電変換層上に形成する方法、または酸化剤および正孔輸送層の前駆体であるモノマーもしくはプレポリマーの形態で必要により溶媒や電解質などを添加した溶液を光電変換層上に塗布した後、重合してポリマーを形成する方法が好ましい。また、光電変換層の構成要素である半導体層が多孔質体である場合は、当該多孔質体の表面を正孔輸送層が被覆するよう、より詳細には半導体層の表面に吸着した増感色素と正孔輸送層とが酸化剤存在下で接触することが好ましく、具体的には、当該多孔質体の内部や隙間まで、前記正孔輸送層の前駆体および酸化剤と、必要より添加される電解質とを含有する溶液が浸透し、かつ当該多孔質体の表面のほぼ全面を被覆するように含浸および/または塗布により導電性高分子を重合することが好ましい。
本発明に係る光電変換素子の製造方法における工程(3)は、上記工程(2)の後、酸化剤存在下で増感色素に光を照射して前記導電性高分子前駆体を重合して正孔輸送層を形成する。すなわち、酸化剤および正孔輸送層の前駆体であるモノマーもしくはプレポリマー(多量体)の形態で必要により溶媒や電解質などを添加した溶液に光電変換層を含浸した状態で外部から増感色素に対して光を照射することが好ましい。また、当該溶液を光電変換層上に塗布した状態で外部から増感色素に対して光を照射してもよい。
本発明に係る光電変換素子の製造方法における工程(4)は、上記工程(3)の後、前記正孔輸送層上に第二電極を形成する工程である。
本発明に係る光電変換素子の製造方法における工程(5)は、少なくとも2つ以上の光電変換素子を電気的に接続する工程である。光電変換素子の電気的な接続方法は、特に制限されることはなく公知の方法が適応することができる。例えば、銀、銅、カーボンなどの導電性ペーストによる接続が挙げられるが、直列で接続されることが好ましい。より具体的には、(a)図1に示されるように、隣接する2つの光電変換素子10において、一方の光電変換素子の第一電極30の端部31は、隣接する光電変換素子10の第二電極70の端部71と直列で連結(接続)されることが好ましい。または、(b)一方の光電変換素子の第一電極30の端部31は、隣接する光電変換素子10の第二電極70の端部71と導電性部材を介して連結(接続)されることも好ましい。これらのうち、(a)の形態が特に好ましい。すなわち、電気的に接続する工程は、電気抵抗低減の観点から光電子変換素子のうちの少なくとも互いに隣接する二つの光電変換素子は、一つの光電変換素子の第一電極の一端部と前記光電変換素子と隣接する光電変換素子の第二電極の一端部とが接続することを含むことが好ましい。導電性ペーストなどの導電性部材を介して連結する場合に比べ、導電性部材による電気抵抗分のロスを抑えることが可能となり好ましい。
本願発明の光電変換素子は、太陽電池に特に好適に使用できる。したがって、本願発明は、本願発明の光電変換素子または本願発明の方法によって製造される光電変換素子を有することを特徴とする太陽電池をも提供する。
(参考例1)
ガラス基板上に第一電極としてシート抵抗20Ω /□(square)のフッ素ドープ酸化スズ(FTO)をスパッタリングして透明導電層(FTO)(塗布量:7g/m2基板)を形成し、導電性ガラス基板(第一電極基板)を得た。当該ガラス基板の大きさは10mm×15mm×1.0mm、第一電極の各大きさは10mm×10mm×0.1μmであった。得られた第一電極上に10mm×2mmのカプトンテープを第一電極の右端部を覆うように張り付けた後、TC100(マツモト交商製):チタンジイソプロポキシビス(アセチルアセトネート)を滴下して、スピンコート法により塗布した後、カプトンテープを外し、450℃で8分間加熱した。それより、透明導電膜(FTO)上に厚み50nmの酸化チタンの薄層からなるバッファ層(空孔率(C)=1.0体積%)を形成した。
光電変換素子SC-1の作製において、酸化剤をパラトルエンスルホン酸鉄(III)、AgNO3、クメンヒドロペルオキシド、KMnO4に変更した以外は同様にし、光電変換素子SC-2~5を製造した。
光電変換素子SC-1の作製において、酸化剤として酸素を十分にバブリングしている状態で光重合を行った以外は同様にし、光電変換素子SC-6を作製した。
光電変換素子SC-6の作製において、酸化剤をオゾンに変更した以外は同様にし、光電変換素子SC-7を作製した。
光電変換素子SC-1の作製において、導電性高分子前駆体をM1-4、M1-26に変更した以外は同様にし、光電変換素子SC-8、9を作製した。
光電変換素子SC-1の作製において、400nm以上の光をカットした光源を使用した以外は同様にし、光電変換素子SC-10を作製した。
光電変換素子SC-1の作製において、400nm以下の光をカットした光源を使用した以外は同様にし、光電変換素子SC-11を作製した。
光電変換素子SC-1の重合工程において、前記半導体電極を、導電性高分子前駆体M1-1(bis―EDOT)を1×10-3(mol/l)の割合で含有し、Li[(CF3SO2)2N]を0.1(mol/l)の割合で含有するアセトニトリル溶液(電解重合溶液)に浸漬した。作用極に前記半導体電極、対極に白金線、参照電極にAg/Ag+(AgNO3 0.01M)をそれぞれ接続し、保持電圧を-0.16Vとした。半導体層方向から光を照射しながら(キセノンランプ使用、光強度22mW/cm2、420nm以下の波長をカット)30分間電圧を保持して、正孔輸送層51を前記半導体電極表面に形成した。得られた半導体電極/正孔輸送層をアセトニトリルで洗浄、乾燥したのち、正孔輸送層を得た以外は同様にして、光電変換素子SC-13を作製した。
(実施例1)
ガラス基板上に第一電極としてシート抵抗20Ω/□(square)のフッ素ドープ酸化スズ(FTO)をスパッタリングして透明導電層(FTO)(塗布量:7g/m2基板)21,22,23を形成し、導電性ガラス基板(第一電極基板)を得た。当該ガラス基板の大きさは100mm×100mm×1.0mm、第一電極21,22,23の各大きさは90mm×30mm×100nmであった。得られたそれぞれの第一電極上に100mm×2mmのカプトンテープを第一電極の右端部を覆うように張り付け、同様に15mm×30mmのカプトンテープを第一電極の上端部を覆うように貼り付けた後、TC100(マツモト交商製):チタンジイソプロポキシビス(アセチルアセトネート)を滴下して、スピンコート法により塗布した後、カプトンテープを外し、450℃で8分間加熱した。それより、透明導電膜(FTO)上に厚み50nmの酸化チタンの薄層からなるバッファ層(空孔率(C):1.0体積%)31,32,33を形成した。
光電変換素子モジュールSM-1の作製において、酸化剤をパラトルエンスルホン酸鉄(III)、AgNO3、クメンヒドロペルオキシド、KMnO4に変更した以外は同様にし、光電変換素子モジュールSM-2~5を製造した。
光電変換素子モジュールSM-1の作製において、酸化剤として酸素を十分にバブリングしている状態で光重合を行った以外は同様にし、光電変換素子モジュールSM-6を作製した。
光電変換素子モジュールSM-6の作製において、酸化剤をオゾンに変更した以外は同様にし、光電変換素子モジュールSM-7を作製した。
光電変換素子モジュールSM-1の作製において、導電性高分子前駆体をM1-4、M1-26に変更した以外は同様にし、光電変換素子モジュールSM-8、9を作製した。
光電変換素子モジュールSM-1の作製において、400nm以上の光をカットした光源を使用した以外は同様にし、光電変換素子モジュールSM-10を作製した。
光電変換素子モジュールSM-1の作製において、400nm以下の光をカットした光源を使用した以外は同様にし、光電変換素子モジュールSM-11を作製した。
実施例1で用いたガラス基板上にFTOをスパッタリングし、90mm×9mm×100nmの第一電極201~210を作製した。電極間の間隔(X)は0.5mmであった。得られたそれぞれの第一電極上に100mm×1mmのカプトンテープを第一電極の右端部を覆うように張り付け、同様に15mm×30mmのカプトンテープを第一電極の上端部を覆うように貼り付けた後、TC100(マツモト交商製):チタンジイソプロポキシビス(アセチルアセトネート)を滴下して、スピンコート法により塗布した後、カプトンテープを外し、450℃で8分間加熱した。それより、透明導電膜(FTO)上に厚み50nmの酸化チタンの薄層からなるバッファ層(空孔率(C):1.0体積%)301~310を形成した。
光電変換素子モジュール1の重合工程において、前記半導体電極を、導電性高分子前駆体(bis-EDOT)を1×10-3(mol/l)の割合で含有し、Li[(CF3SO2)2N]を0.1(mol/l)の割合で含有するアセトニトリル溶液(電解重合溶液)に浸漬した。作用極に前記第一電極21、対極に白金線、参照電極にAg/Ag+(AgNO3 0.01M)をそれぞれ接続し、保持電圧を-0.16Vとした。半導体層方向から光を照射しながら(キセノンランプ使用、光強度22mW/cm2、430nm以下の波長をカット)30分間電圧を保持して、正孔輸送層51を前記半導体電極表面に形成した。得られた半導体電極/正孔輸送層をアセトニトリルで洗浄、乾燥したのち、作用極を前記第一電極22に接続し直し、同様の条件で電圧を保持し正孔輸送層52を得、さらに同様に正孔輸送層53を得た。また、正孔輸送層を得た以外は同様にして、光電変換素子モジュールSM-13を作製した。
上記実施例および比較例で作製した光電変換素子及び光電変換素子モジュールを、ソーラーシミュレータ(英弘精機製)を用いて、得られた光電変換素子とモジュールに、キセノンランプからAMフィルター(AM-1.5)を通して強度100mW/cm2の擬似太陽光を照射した。そして、I-Vテスターを用いて、光電変換素子の室温での電流-電圧特性を測定し、短絡電流密度(Jsc)、開放電圧(Voc)、および形状因子(F.F.)を測定した。これらの値を、下記式に当てはめて光電変換素子及び光電変換素子モジュールの光電変換効率ηc(%)とモジュールの光電変換効率ηmを求めた。
Claims (12)
- 基板、第一電極、半導体および増感色素を含有する光電変換層、導電性高分子を有する正孔輸送層、ならびに第二電極の順で積層された光電変換素子が、2つ以上電気的に接続されてなる光電変換素子モジュールにおいて、
前記正孔輸送層は、酸化剤存在下で、前記光電変換層と導電性高分子前駆体とを接触した後、前記増感色素に光を照射することによって前記導電性高分子前駆体を重合することにより形成することを特徴とする光電変換素子モジュール。 - 前記光電子変換素子のうちの少なくとも互いに隣接する二つの光電変換素子は、一つの光電変換素子の前記第一電極の一端部と前記光電変換素子と隣接する光電変換素子の前記第二電極の一端部とが接続されている、請求項1に記載の光電変換素子モジュール。
- 前記酸化剤が、酸素、オゾン、過酸化物または金属塩である、請求項1または2のいずれか1項に記載の光電変換素子モジュール。
- 前記増感色素は、一般式(1)
Arは、二価の環式化合物基を表し、
A1およびA2は、それぞれ独立して、単結合、2価の飽和もしくは不飽和の炭化水素基、置換もしくは未置換のアルキレン基、アリーレン基、または2価の複素環基を表し、
Zは、酸性基、アルコキシシランまたはハロゲン化シランを有する有機基であり、
p、qは、それぞれ独立して、0以上6以下の整数であり、
nは、1以上3以下の整数であり、
nが1のとき、2つのR3は互いに異なるものであってもよく、また、R3は他の置換基と連結して環構造を形成したものであってもよく、nが2以上のとき、複数のAr、A1、A2、Zは互いに異なるものであってもよい。)
で示される、請求項1~4のいずれか1項に記載の光電変換素子モジュール。 - 前記照射光の波長が前記増感色素の吸収波長を含む、請求項1~5のいずれか1項に記載の光電変換素子モジュール。
- 基板、第一電極、半導体および増感色素を含有する光電変換層、導電性高分子を有する正孔輸送層、ならびに第二電極の順で積層された光電変換素子が、2つ以上電気的に接続されてなる光電変換素子モジュールの製造方法において、
前記第一電極上に前記光電変換層を形成することと、
酸化剤存在下で前記光電変換層に導電性高分子前駆体を接触することと、
前記酸化剤存在下で前記増感色素に光を照射して前記導電性高分子前駆体を重合して正孔輸送層を形成することと、
前記正孔輸送層上に前記第二電極を形成することと、
少なくとも2つ以上の前記光電変換素子を電気的に接続することと、を含む光電変換素子モジュールの製造方法。 - 前記電気的に接続することは、一つの光電変換素子の前記第一電極の一端部と前記光電変換素子と隣接する光電変換素子の前記第二電極の一端部とを接続することを含む、請求項7に記載の光電変換素子モジュールの製造方法。
- 前記第二電極を形成することにより、少なくとも2つ以上の前記光電変換素子を電気的に接続することを特徴とする請求項8に記載の光電変換素子モジュールの製造方法。
- 前記酸化剤が、酸素、オゾン、過酸化物または金属塩である、請求項7~9のいずれか一項に記載の光電変換素子モジュールの製造方法。
- 前記照射光の波長が前記増感色素の吸収波長を含む請求項7~11のいずれか1項に記載の光電変換素子モジュールの製造方法。
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