WO2011132286A1 - 透明電極上における光触媒膜の形成方法 - Google Patents
透明電極上における光触媒膜の形成方法 Download PDFInfo
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- WO2011132286A1 WO2011132286A1 PCT/JP2010/057143 JP2010057143W WO2011132286A1 WO 2011132286 A1 WO2011132286 A1 WO 2011132286A1 JP 2010057143 W JP2010057143 W JP 2010057143W WO 2011132286 A1 WO2011132286 A1 WO 2011132286A1
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- photocatalyst film
- photocatalyst
- transparent electrode
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- 229910052725 zinc Inorganic materials 0.000 description 1
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- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M14/00—Electrochemical current or voltage generators not provided for in groups H01M6/00 - H01M12/00; Manufacture thereof
-
- 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
-
- 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
Definitions
- a photocatalyst film is prepared by applying a paste containing photocatalyst particles onto a transparent conductive film of a transparent electrode and drying it. And a method of directly irradiating the same layer with a laser from the surface thereof, a method of pressurizing photocatalyst particles toward a transparent electrode, and the like are known (Non-Patent Document 1, etc.).
- the titanium oxide particles and the bonding between the transparent conductive film and the titanium oxide particles are important.
- the photocatalyst particles near the surface of the photocatalyst film can be strongly bonded to each other.
- the bond between the photocatalyst particles constituting the photocatalyst film and the transparent electrode could not be made sufficient.
- the invention according to claim 2 is characterized in that the laser is directly irradiated from the surface side of the photocatalyst film while irradiating the photocatalyst film from the transparent electrode side through the same electrode. This is a method for forming a photocatalyst film.
- a photocatalytic film is formed on a transparent conductive film in a transparent electrode composed of a transparent substrate and a transparent conductive film thereon, and then the photocatalytic film is irradiated with a laser from the transparent electrode side through the same electrode. Then, the laser is directly irradiated from the surface side of the photocatalyst film, and the additional operation of forming the photocatalyst film on the photocatalyst film and irradiating the photocatalyst film with the laser from the surface is performed at least once.
- This is a method for forming a photocatalytic film on a transparent electrode.
- the invention according to claim 5 forms a photocatalyst film on the transparent conductive film in a transparent electrode comprising a transparent substrate and a transparent conductive film thereon, and then pressurizes the photocatalyst film from the surface side with a transparent press device.
- the invention according to claim 6 is characterized in that the laser irradiation to the photocatalyst film is performed from the surface side of the photocatalyst film through the transparent press device and also from the transparent electrode side through the same electrode. This is a method for forming a photocatalytic film on a transparent electrode.
- the invention according to claim 7 is the method for forming a photocatalyst film on a transparent electrode according to any one of claims 4 to 6, wherein the pressurization of the photocatalyst film is performed while heating the photocatalyst film. is there.
- the photocatalyst particles are bonded to each other inside the photocatalyst film, and the transparent electroconductive film of the photocatalyst film and the transparent electrode Both of these bonds can be made even stronger.
- the laser is irradiated from the surface side of the photocatalyst film, and further onto the photocatalyst film
- the photocatalyst particles in the photocatalyst film are bonded to each other, and the photocatalyst film is bonded to the transparent conductive film of the transparent electrode. It can be made stronger.
- the photocatalyst particles are bonded to each other within the photocatalyst film, and the photocatalyst film and the transparent electrode
- the bond with the transparent conductive film can be further strengthened.
- a photocatalyst film is formed on a transparent conductive film, and then the photocatalyst film is pressurized from the surface side while irradiating the photocatalyst film with a laser from the surface side, thereby providing a photocatalyst.
- the bond between the photocatalyst particles inside the film and the bond between the photocatalyst film and the transparent conductive film of the transparent electrode can be strengthened, whereby a photoelectric conversion element exhibiting sufficient efficiency can be manufactured.
- a transparent conductive film can be continuously produced by using a flexible material.
- FIG. 1 is a vertical longitudinal sectional view schematically showing a method of Example 1.
- FIG. 6 is a vertical longitudinal sectional view schematically showing a method of Example 4.
- FIG. 10 is a vertical longitudinal sectional view schematically showing a method of Example 7.
- FIG. 6 is a vertical longitudinal sectional view schematically showing a method of Example 3.
- 10 is a vertical longitudinal sectional view schematically showing a method of Example 7.
- FIG. 5 is a vertical longitudinal sectional view showing a photoelectric conversion element of Reference Example 1.
- a transparent electrode composed of a transparent substrate and a transparent conductive film formed thereon will be described.
- thermoplastic resin film such as a PEN (polyethylene naphthalate) film is preferable.
- the synthetic resin may be polyethylene terephthalate, polyester, polycarbonate, polyolefin, or the like.
- the photocatalytic particles are made of a metal oxide such as titanium oxide (TiO 2), tin oxide (SnO 2), tungsten oxide (WO 3), zinc oxide (ZnO), niobium oxide (Nb 2 O 5).
- a metal oxide such as titanium oxide (TiO 2), tin oxide (SnO 2), tungsten oxide (WO 3), zinc oxide (ZnO), niobium oxide (Nb 2 O 5).
- metal compound used as a starting material for the metal oxide sol examples include metal alkoxides, metal acetylacetonates, metal carboxylates, and metal inorganic compounds such as metal nitrates, oxychlorides, and chlorides. Can be mentioned.
- titanium oxide as metal alkoxide, titanium tetramethoxide, titanium ethoxide, titanium isopropoxide, titanium butoxide, etc.
- metal acetylacetonate as titanium acetylacetonate
- metal carboxylate Titanium carboxylate, titanium nitrate, titanium oxychloride, titanium tetrachloride and the like.
- the drying is performed at room temperature for about 5 to 30 minutes. Firing is performed at a temperature of 450 to 550 ° C. for about 30 to 60 minutes.
- the laser that irradiates the photocatalyst film from the transparent electrode side is preferably visible light range (380 nm to 800 nm), specifically, Nd: YAG laser (1064 nm) infrared, and a green wavelength of 532 nm using a wavelength conversion element. Or Alexandrite laser (700-820 nm) can be applied. Note that an optical system capable of forming a short focal point is assembled at the time of laser irradiation, and the coupling effect is further improved by focusing on the interface between the transparent conductive film and the photocatalytic film.
- a laser oscillator that oscillates such a laser is equipped with a galvano scanner, and the laser irradiation position can be freely changed.
- the photocatalyst film is performed from the surface side of the photocatalyst film through a transparent press device and also from the transparent electrode side through the same electrode.
- the transparent press device is composed of a transparent body such as glass or resin.
- the photocatalyst film may be heated by a method in which an electric heater is installed inside the press apparatus or a high-temperature fluid is allowed to flow inside the press apparatus.
- the heating temperature of the photocatalytic film is preferably 150 ° C.
- Photosensitizing dyes include, for example, ruthenium complexes and iron complexes having a ligand containing a bipyridine structure, a terpyridine structure, etc., porphyrin-based and phthalocyanine-based metal complexes, and organic dyes such as eosin, rhodamine, merocyanine, and coumarin. It may be.
- an iodine-based electrolyte for example, an iodine-based electrolyte is used. Specifically, an electrolyte component such as iodine, iodide ion, or tertiary butyl pyridine is dissolved in an organic solvent such as ethylene carbonate or methoxyacetonitrile. Is exemplified.
- the electrolyte is not limited to an electrolyte and may be a solid electrolyte. Examples of the solid electrolyte include DMPImI (dimethylpropylimidazolium iodide).
- the counter electrode may be one in which a transparent conductive film is formed on a transparent substrate for a counter electrode, or one in which a sheet of metal such as aluminum, copper, or tin is provided on the same substrate.
- the counter electrode may be configured by holding a gel solid electrolyte on a mesh electrode made of metal (aluminum, copper, tin, etc.) or carbon, and conductive adhesion is performed on one side of the counter electrode substrate.
- the counter electrode may be configured by forming an agent layer so as to cover the substrate and transferring a separately formed group of brush-like carbon nanotubes to the substrate via the adhesive layer.
- the electrode provided with the dyeing photocatalyst film and the counter electrode are aligned to face each other, the gap between the electrodes is sealed with a heat-sealing film or a sealing material, and the counter electrode or the electrode is provided in advance.
- Electrolyte is injected through the holes and gaps.
- both electrodes are overlapped so that the photocatalyst film and the electrolyte layer are sandwiched therebetween, and the peripheral portions thereof are heat bonded.
- Heating may be performed by a mold, or may be performed by irradiation with an energy beam such as plasma (having a long wavelength), microwave, visible light (600 nm or more), or infrared light.
- Example 1 In FIG. 1, a paste containing titanium oxide particles as photocatalyst particles on a transparent substrate (1) composed of a polyethylene naphthalate film and a transparent electrode (3) composed of ITO on the transparent substrate (1) ( Ethanol and water with titanium oxide added), dried at room temperature for 15 minutes, baked at 150 ° C for 15 minutes, and photocatalytic film on the transparent conductive film (2) of the transparent electrode (3) (4) was formed.
- the photocatalyst film (4) was irradiated with an alexandrite laser (700-820 nm) from the transparent electrode (3) side. At that time, an optical system for forming a short focal point was assembled so that the interface between the transparent conductive film and the photocatalytic film was focused.
- the fourth photocatalyst film (10) was bonded onto the third photocatalyst film (9) by the same operation as described above.
- Example 5 In the same manner as in Example 1, a photocatalytic film (4) was formed on a transparent electrode (3) comprising a transparent substrate (1) and a transparent conductive film (2) thereon. Next, as shown in FIG. 5, while pressing the photocatalyst film (4) from the surface side with a transparent press device (12) made of a transparent glass plate, the photocatalyst film (4) is transparently pressed from the surface side. After (12), an Alexandrite laser (700-820 nm) was irradiated using a laser oscillator (5) equipped with a galvano scanner.
- a transparent press device (12) made of a transparent glass plate
- Example 6 laser irradiation to the photocatalyst film (4) is performed from the surface side of the photocatalyst film (4) through the transparent press device (12) and from the transparent electrode (3) side, an alexandrite laser (700-820 nm). ).
- Example 7 the photocatalyst film (4) was pressurized to the transparent electrode (3) using a roll-shaped press device (11) shown in FIG. 3 instead of the flat plate press device.
- a roll-shaped press device (11) shown in FIG. 3 instead of the flat plate press device.
- Other configurations are the same as those of the fourth embodiment.
- the roll-shaped press device (11) it was possible to continuously pressurize the photocatalyst film (4).
- a dye-sensitized solar cell having a thickness of several ⁇ m and a square of 100 mm was prepared, and when the power conversion efficiency was measured by irradiation with a standard light source of AM 1.5 and 100 mW / cm 2, the dyed photocatalyst film obtained in Example 1 was provided.
- conversion efficiency ⁇ 5 to 6%.
- conversion efficiency ⁇ 6 to 7%. High efficiency was obtained.
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Abstract
Description
図1において、ポリエチレン・ナフタレートフィルムからなる透明基板(1)と、その上のITOからなる透明導電膜(2)とからなる透明電極(3)に、光触媒粒子として酸化チタン粒子を含むペースト(エタノールと水に酸化チタンを添加したもの)を塗布し、室温で、15分間乾燥し、温度150℃で、15分間焼成し、透明電極(3)の透明導電膜(2)の上に光触媒膜(4)を形成した。ついで、ガルバノスキャナを備えたレーザ発振器(5)を用いて、光触媒膜(4)に透明電極(3)側からアレキサンドライトレーザ(700-820nm)を照射した。その際、短焦点を形成する光学系を組み、透明導電膜と光触媒膜との界面に焦点が合うようにした。
実施例1において、光触媒膜(4)に透明電極(3)側から同電極を経てアレキサンドライトレーザ(700-820nm)を照射しながら、同光触媒膜(4)の表面側からも直接アレキサンドライトレーザ(700-820nm)を照射した。
実施例1において、図4(a)に示すように、第1の光触媒膜(4)に透明電極(3)側から同電極を経てアレキサンドライトレーザ(700-820nm)を照射して透明電極(3)に第1の光触媒膜(4)を結合させた後、図4(b)に示すように、第1の光触媒膜(4)の上に、実施例1と同様の操作により酸化チタン粒子含有ペーストを塗布し、乾燥し、第2の光触媒膜(8)を形成した。ついで、ガルバノスキャナを備えたレーザ発振器(5)を用いて、第2の光触媒膜(8)にその表面側から直接アレキサンドライトレーザ(700-820nm)を照射して第1の光触媒膜(4)の上に第2の光触媒膜(8)を結合させた。
実施例1において、光触媒膜(4)へのレーザ照射を、同光触媒膜をその表面側から圧力50MPaで、30秒間加圧しながら行った。加圧は、図2に示すように、内部に電熱ヒータ線(6)を設けた平板状のプレス装置(7)を用いて、プレス装置温度150℃で30秒間行った。
実施例1と同様にして、透明基板(1)とその上の透明導電膜(2)とからなる透明電極(3)に、の光触媒膜(4)を形成した。ついで、図5に示すように、同光触媒膜(4)をその表面側から透明ガラス板製の透明プレス装置(12)で加圧しながら、同光触媒膜(4)にその表面側から透明プレス装置(12)を経て、ガルバノスキャナを備えたレーザ発振器(5)を用いてアレキサンドライトレーザ(700-820nm)を照射した。
実施例5において、光触媒膜(4)へのレーザ照射を、同光触媒膜(4)の表面側から透明プレス装置(12)を経て行うと共に透明電極(3)側からもアレキサンドライトレーザ(700-820nm)を用いて行った。
実施例4において、平板状のプレス装置の代わりに、図3に示すロール状のプレス装置(11)を用いて、透明電極(3)に光触媒膜(4)を加圧した。その他の構成は実施例4のものと同じである。ロール状のプレス装置(11)を用いることにより、光触媒膜(4)の加圧を連続的に行うことができた。
図6に、光増感色素で染色された光触媒膜を備えた透明電極を用いて構成した光電変換素子の例を示す。光電変換素子は、染色光触媒膜を備えた透明電極と、これに対向する対極と、両極間に配される電解質層とから主として構成されている。
(2) 透明導電膜
(3) 透明電極
(4),(8),(9),(10) 光触媒膜
(5) レーザ発振器
(6) 電熱ヒータ線
(7) 平板状のプレス装置
(11) ロール状のプレス装置
Claims (8)
- 透明基板とその上の透明導電膜とからなる透明電極において透明導電膜上に光触媒膜を形成し、ついで同光触媒膜に透明電極側から同電極を経てレーザを照射することを特徴とする、透明電極上における光触媒膜の形成方法。
- 光触媒膜に透明電極側から同電極を経てレーザを照射しながら同光触媒膜の表面側から直接レーザを照射することを特徴とする、請求項1記載の透明電極上における光触媒膜の形成方法。
- 透明基板とその上の透明導電膜とからなる透明電極において透明導電膜上に光触媒膜を形成し、ついで同光触媒膜に透明電極側から同電極を経てレーザを照射した後、同光触媒膜の表面側から直接レーザを照射し、さらにこの光触媒膜の上への光触媒膜の形成と同光触媒膜へのその表面からのレーザ照射との追加操作を少なくとも1回行うことを特徴とする、透明電極上における光触媒膜の形成方法。
- 光触媒膜へのレーザ照射を、同光触媒膜をその表面側から加圧しながら行うことを特徴とする、請求項1記載の透明電極上における光触媒膜の形成方法。
- 透明基板とその上の透明導電膜とからなる透明電極において透明導電膜上に光触媒膜を形成し、ついで同光触媒膜をその表面側から透明プレス装置で加圧しながら、同光触媒膜にその表面側から透明プレス装置を経てレーザを照射することを特徴とする、透明電極上における光触媒膜の形成方法。
- 光触媒膜へのレーザ照射を、同光触媒膜の表面側から透明プレス装置を経て行うと共に透明電極側からも同電極を経て行うことを特徴とする、請求項5記載の透明電極上における光触媒膜の形成方法。
- 光触媒膜の加圧を、同光触媒膜を加熱しながら行うことを特徴とする、請求項4~6のいずれかに記載の透明電極上における光触媒膜の形成方法。
- 透明電極への光触媒膜の加圧を、ロール状のプレス装置を用いて行い、光触媒膜の加圧を連続的に行うことを特徴とする、請求項1~7のいずれかに記載の透明電極上における光触媒膜の形成方法。
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WO2013110441A1 (de) * | 2012-01-24 | 2013-08-01 | Linde Aktiengesellschaft | Verfahren zum kaltgasspritzen |
US9527069B2 (en) | 2012-01-24 | 2016-12-27 | Linde Aktiengesellschaft | Method for cold gas spraying |
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KR20130051946A (ko) | 2013-05-21 |
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