WO2008065727A1 - Procédé de fabrication d'une électrode munie d'un film de platine - Google Patents

Procédé de fabrication d'une électrode munie d'un film de platine Download PDF

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Publication number
WO2008065727A1
WO2008065727A1 PCT/JP2006/325980 JP2006325980W WO2008065727A1 WO 2008065727 A1 WO2008065727 A1 WO 2008065727A1 JP 2006325980 W JP2006325980 W JP 2006325980W WO 2008065727 A1 WO2008065727 A1 WO 2008065727A1
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WO
WIPO (PCT)
Prior art keywords
electrode
platinum
film
cathode
platinum film
Prior art date
Application number
PCT/JP2006/325980
Other languages
English (en)
Japanese (ja)
Inventor
Kazuhide Nagano
Original Assignee
Shimane Prefectural Government
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shimane Prefectural Government filed Critical Shimane Prefectural Government
Priority to JP2008546865A priority Critical patent/JP5071741B2/ja
Publication of WO2008065727A1 publication Critical patent/WO2008065727A1/fr

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Classifications

    • 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
    • H01G9/2022—Light-sensitive devices characterized by he counter electrode
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
    • 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
    • H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
    • H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
    • 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
    • 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
    • H01L31/02—Details
    • H01L31/0224—Electrodes
    • H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
    • H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • 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 method for producing an electrode having a platinum film, and more particularly to a method for producing an electrode having a platinum film useful as a counter electrode of a dye-sensitized solar cell.
  • an oxidation-reduction pair for example, I-, ⁇ , etc.
  • a counter electrode with a catalytic function As this counter electrode, a material in which a highly catalytic white metal is supported on a conductive substrate provided with a conductive film [for example, indium stannate] or SnO] is often used.
  • a sputtering method see Patent Document 1
  • a vapor deposition method see Patent Document 2
  • these methods require equipment with a large vacuum chamber when considering mass production and large area, and the productivity is low and the equipment costs are high, so the manufacturing cost is not reduced.
  • counter electrodes produced by these methods are not durable because platinum dissolves in iodine electrolyte.
  • Patent Document 3 discloses a method in which platinum particles are supported on the surface of a conductive layer by electric plating.
  • this method is considered to have a problem in durability because of low adhesion strength because platinum particles are supported by the particles.
  • this method uses a strong acid called nitric acid as the electrolytic solution, and in the electroplating under such strong acidity, a substrate using a conductive film weak in acid (for example, ITO, SnO, etc.) or a metal substrate, There are problems such as dissolution and substrate dissolution.
  • Patent Document 1 Japanese Unexamined Patent Publication No. 2000-173680
  • Patent Document 2 Japanese Unexamined Patent Publication No. 2000-36330
  • Patent Document 3 Japanese Patent Laid-Open No. 2003-36897
  • the present invention has been made to solve the above-described problems in the prior art, and a method for producing an electrode having a more excellent platinum film, particularly a platinum film useful as a counter electrode of a dye-sensitized solar cell. It is an object of the present invention to provide a method for manufacturing an electrode having the following.
  • the present inventors have performed electroplating using a platinum aqueous solution having a pH of 2 or more as an electrolytic solution, thereby providing sufficient adhesion strength on the conductive film.
  • the present invention was completed by finding that uniform and uniform platinum was formed into a film.
  • the method for producing an electrode having a platinum film of the present invention includes:
  • the present invention is characterized in that an electrode produced by the method is used as a counter electrode of a dye-sensitized solar cell.
  • an electrode by an electroplating method in an aqueous platinum solution can be used with an acid-sensitive material such as indium tin oxide (ITO), and can be selectively deposited on a conductive film in a short time.
  • ITO indium tin oxide
  • a white metal film can be formed.
  • the electroplating method is a cheaper manufacturing method compared to the conventional sputtering method and can contribute to the reduction of the manufacturing cost of the dye-sensitized solar cell.
  • the formed platinum film is superior in durability to the sputtering method, and can contribute to the production of a durable dye-sensitized solar cell.
  • FIG. 1 is a schematic cross-sectional view showing a form of an electric plating.
  • FIG. 2 is a schematic cross-sectional view showing a basic configuration when the electrode of the present invention is used as a counter electrode of a dye-sensitized solar cell.
  • FIG. 3 is a schematic cross-sectional view of an electrode used as a counter electrode of the dye-sensitized solar cell shown in FIG.
  • FIG. 4 is an electron micrograph (magnified 80,000 times) of the ITO glass conductive film surface before electroplating in Example 1.
  • FIG. 5 is an electron micrograph (100,000 times) of the ITO glass conductive film surface after electroplating in Example 1.
  • This step is a step of preparing a cathode, an anode, an electrolytic solution and a power source necessary for the production method of the present invention.
  • Electrolyte As the electrolytic solution used in the method of the present invention, a platinum aqueous solution having a pH of 2 or more is used.
  • a power suitable for electroplating can be arbitrarily used.
  • Platinum (IV) methanesulfonate [Pt (NH) (CH 2 SO 4)] and other water-soluble divalent or tetravalent
  • a valent platinum compound is particularly preferably used.
  • concentration of each platinum compound as the weight of platinum, a concentration of 0.1 to: LOgZL can be suitably used, and a concentration range of 1.5 to 2.5 gZL can be more preferably used. .
  • an additive such as hydrazine as a reducing agent or hydroxylamine salt as a stabilizer may be added.
  • the pH of the solution is 2 or more. If the pH of this solution is less than 2, even if the plating is continued until the platinum film is formed, the obtained platinum film may be peeled off immediately and good battery performance cannot be expected (patent) Reference 1, paragraph number 0031).
  • the optimum pH can be adjusted in consideration of the properties of the substrate, the deposition rate of platinum, etc., but from the viewpoint of protecting the conductive film on the substrate, the pH range of 4 to 13 is preferred. Particularly preferred is ⁇ 11 (excluding 7).
  • the pH adjusting agent nitric acid, aqueous ammonia, potassium hydroxide or the like can be preferably used.
  • the cathode used in the present invention is a substrate on which conductive films are laminated.
  • the substrate a glass substrate, a plastic substrate, a metal substrate or the like can be used, and the material of the substrate is not particularly selected. As will be described later, in particular, according to the method of the present invention, even when a metal substrate is used, it is not necessary to remove the oxide film on the surface, and electrical plating can be performed easily.
  • the metal material used for the metal substrate titanium, stainless steel, etc. are preferred from the viewpoint of corrosion resistance against iodine.
  • the conductive layer is preferably an oxide tin or indium stannate oxide (ITO) film that may contain an additive (tin oxide is preferably contained in indium oxide. Is 5 Fluorine or antimony-doped tin oxide may be used, which is preferably about 15% by weight.
  • ITO indium stannate oxide
  • These conductive layers can be laminated on the substrate by known methods such as sputtering, vapor deposition, and spin coating.
  • anode and the power source those normally used for electric plating can be used.
  • anode for example, a carbon electrode, a platinum electrode or the like can be suitably used.
  • This step is a step of performing electrical plating.
  • the bath temperature can be suitably used from room temperature to 80 ° C, more preferably from room temperature to 60 ° C.
  • current as the density in terms of deposition rate control, generally at 0. 1: more preferably preferably instrument performed by controlling the a current density LOAZdm 2 2. the 5 ⁇ 6AZdm 2 Control and do.
  • the plating time is affected by temperature, current density, etc., but from the viewpoint of catalyst performance and cost, 0.1-5 minutes, more preferably 0.25-1.0 minutes is used! I can do it.
  • a platinum film can be selectively formed on the cathode conductive film.
  • the mechanical strength is good due to adhesion and denseness, and the reflected light contributes to power generation by reflecting light from the platinum film, improving efficiency. Has the advantage of being connected.
  • This step is a step of taking out the cathode formed with the platinum film manufactured by the above steps (a) and (b).
  • the taken-out cathode can be suitably used as a counter electrode of a dye-sensitized solar cell after washing and drying.
  • FIG. 1 shows a schematic diagram of the electrical plating.
  • a substrate 6 having a conductive layer 7 laminated on one side and a counter electrode 3 were immersed in an aqueous platinum solution 2 in a container 1.
  • Example 4 As the platinum aqueous solution, except for Example 4, an aqueous solution of hexammineplatinum (IV) methanesulfonate adjusted to ⁇ .8 with aqueous ammonia (content 25% by weight) was used.
  • the concentration of hexammineplatinum (IV) methanesulfonate in the platinum aqueous solution was 6.9 g / L (2 gZL as platinum), and the liquid temperature of the platinum aqueous solution was 19 ° C.
  • a carbon electrode was used as the counter electrode.
  • the substrate 6 on which the conductive layer 7 is laminated is connected to the negative pole of the DC power source 5, and the counterpart electrode 3 is connected to the positive pole of the DC electrode 5.
  • a voltage is applied so that the current becomes 0.lAZdm 2 to l OAZdm 2
  • a platinum film 8 is selectively formed on the surface of the conductive layer 7 laminated on the substrate 6, and the counter electrode as shown in FIG. 4 can be done.
  • the counter electrode 4 was produced in each of Examples 1 to 3 and Comparative Examples 1 and 2 as follows.
  • Example 1 when electroplating is performed in a platinum aqueous solution having a pH of 2 or more, more preferably 7 or more, platinum plating can be performed without damaging the ITO even in an acid-sensitive conductive layer such as ITO. it can.
  • Example 3 a metal material having an acid film on the surface, such as titanium metal, cannot be etched unless the acid film is removed with a normal electric plating.
  • a metal material having an acid film on the surface such as titanium metal
  • electric plating can be easily performed without performing a complicated pretreatment step of removing the acid film. Since the electrical plating is selectively coated on the surface on which the conductive layer is laminated and not on the surface without the conductive layer, it is very advantageous for manufacturing the counter electrode.
  • a glass substrate in which indium tin oxide (ITO, containing approximately 10% by weight of tin oxide in indium oxide) was deposited as a conductive film was used ( Film thickness 200nm).
  • Fig. 4 shows an electron micrograph of the surface of the conductive film deposited with ITO before electroplating. [0041] The current density of the electrical plating was 5 A / dm 2 and the time was 0.5 minutes. After electroplating, the substrate on which the white metal film was formed was washed with water and dried at 110 ° C. (platinum film thickness 5 nm).
  • Fig. 5 shows an electron micrograph of the surface of the conductive film on which ITO was deposited after electroplating. Since platinum particles with no difference in the surface state before and after the plating are not observed, it is considered that platinum is uniformly deposited in the form of a film.
  • Example 1 As in Example 1, a glass substrate on which ITO was deposited as a conductive film was prepared, and an organic solvent solution (organic solvent: isopropyl alcohol) having an ITO particle concentration of 10% by mass was further spin-coated on this substrate. Then, it was dried at 110 ° C. for 5 minutes, and electroplating was performed using this as a cathode (spin coat film thickness 400 nm).
  • organic solvent organic solvent: isopropyl alcohol
  • the current density of the electrical plating was 5 A / dm 2 and the time was 0.5 minutes.
  • the substrate on which the white metal film was formed was washed with water and dried at 110 ° C. (platinum film thickness 5 nm).
  • Example 2 The same substrate as in Example 1 was prepared by depositing ITO as a conductive layer on a glass substrate, and platinum was deposited on the surface of this conductive layer using a sputtering device (Hitachi E-1030 ion sputtering). It was supported to a thickness of 20 nm.
  • a sputtering device Hagachi E-1030 ion sputtering
  • organic solvent solution organic solvent: isopropyl alcohol
  • ITO particle concentration 10% by mass with an average particle diameter of 12 nm
  • titanium metal plate As a substrate, an organic solvent solution (organic solvent: isopropyl alcohol) having an ITO particle concentration of 10% by mass with an average particle diameter of 12 nm was spin-coated on a titanium metal plate and dried at 110 ° C. for 5 minutes. (Film thickness 400nm).
  • the current density of the electrical plating was 5 A / dm 2 and the time was 0.5 minutes. After electric plating, it was washed with water and dried at 110 ° C (platinum film thickness 5 nm).
  • Example 2 As in Example 2, a titanium metal plate was used as the substrate, and platinum was supported on this surface to a thickness of 20 nm by a sputtering apparatus.
  • a hexaammineplatinum (IV) methanesulfonate aqueous solution adjusted to pH 2.1 with ammonia water (12.5 wt% contained) was used as the platinum aqueous solution. Hexa at this time The concentration of ammineplatinum (IV) methanesulfonate was 6.9 gZL (2 gZL as platinum), and the solution temperature was 19 ° C.
  • substrate use the same as in Example 1 in which ITO is deposited as a conductive film on a glass substrate, a current density of the electric plated is a 5AZdm 2, time was 5 minutes 0.5.
  • the electric plating method showed good battery performance similar to the sputtering method. Further, by adding additional ITO particles to the surface as in Example 2, the surface area can be increased and the conversion efficiency can be further improved.
  • Example 4 As a result of making the pH of the electrolytic solution acidic (2.1), the platinum film thickness was slightly thinner than that of Example 1. For this reason, the catalyst performance was slightly lower than that of Example 1.
  • iodine and lithium iodide were dissolved in 3-methoxypropio-tolyl at concentrations of 0.03M and 0.3M, respectively, to prepare an electrolyte solution.
  • the electrode of Example 2 was immersed in and held at 80 ° C. for 48 hours. Then take this A dye-sensitized solar cell as shown in Fig. 3 was prepared using the electrode as a counter electrode, and the performance was evaluated in the same manner as described above. The results are shown in Table 2.
  • the electrode produced by the method of the present invention forms a uniform film of platinum on the surface of the conductive film and has sufficient adhesion strength, and is useful as a counter electrode of a dye-sensitized solar cell. is there.
  • the platinum film can be selectively formed only in the necessary portion, so that the cost can be reduced.
  • treatment such as removal of the oxide film on the surface is not necessary, and if a conductive film is formed on the surface, electric plating can be easily performed.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Photovoltaic Devices (AREA)
  • Hybrid Cells (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

L'invention concerne un procédé de fabrication d'une électrode munie d'un film de platine, ladite électrode étant utile en tant que contre-électrode d'une cellule solaire sensibilisée par un colorant. Le procédé de fabrication d'une électrode munie d'un film de platine est caractérisé en ce qu'il comprend la réalisation successive de (a) une étape d'utilisation d'une cathode, d'une anode et d'une solution électroconductrice, ainsi que d'une alimentation électrique, un substrat comprenant un film électroconducteur étant utilisé en tant que cathode et une solution aqueuse de platine ayant une valeur de pH supérieure ou égale à 2 étant utilisée en tant que solution d'électrolyse, (b) une étape de connexion de la cathode à l'électrode négative dans l'alimentation électrique, de connexion de l'anode à l'électrode positive dans l'alimentation électrique, d'immersion des deux électrodes dans la solution d'électrolyse, d'application d'une tension entre les électrodes pour formation par électrodéposition d'un film de platine sur le film électroconducteur dans la cathode, et (c) une étape de retrait de la cathode comportant un film de platine.
PCT/JP2006/325980 2006-11-28 2006-12-26 Procédé de fabrication d'une électrode munie d'un film de platine WO2008065727A1 (fr)

Priority Applications (1)

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JP2008546865A JP5071741B2 (ja) 2006-11-28 2006-12-26 白金膜を有する電極の製造方法

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JP2006320722 2006-11-28
JP2006-320722 2006-11-28

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114182315A (zh) * 2022-02-14 2022-03-15 深圳市顺信精细化工有限公司 一种耐腐蚀组合电镀层及电镀方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002038293A (ja) * 2000-07-25 2002-02-06 Tanaka Kikinzoku Kogyo Kk 白金めっき液およびそのめっき液を用いためっき方法
JP2002298936A (ja) * 2001-03-30 2002-10-11 Fuji Xerox Co Ltd 光電変換素子、及びその製造方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001243995A (ja) * 2000-02-29 2001-09-07 Fuji Photo Film Co Ltd 光電変換素子および光電池
JP2005310722A (ja) * 2004-04-26 2005-11-04 Mitsubishi Electric Corp 色素増感型太陽電池
JP4773086B2 (ja) * 2004-12-28 2011-09-14 住友大阪セメント株式会社 色素増感型光電変換素子、色素増感型光電変換素子の製造方法、及び色素増感型光電変換素子用塗料
JP4963165B2 (ja) * 2005-03-28 2012-06-27 株式会社豊田中央研究所 色素増感型太陽電池及び色素増感型太陽電池モジュール

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002038293A (ja) * 2000-07-25 2002-02-06 Tanaka Kikinzoku Kogyo Kk 白金めっき液およびそのめっき液を用いためっき方法
JP2002298936A (ja) * 2001-03-30 2002-10-11 Fuji Xerox Co Ltd 光電変換素子、及びその製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114182315A (zh) * 2022-02-14 2022-03-15 深圳市顺信精细化工有限公司 一种耐腐蚀组合电镀层及电镀方法
CN114182315B (zh) * 2022-02-14 2022-05-17 深圳市顺信精细化工有限公司 一种耐腐蚀组合电镀层及电镀方法

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JPWO2008065727A1 (ja) 2010-03-04
JP5071741B2 (ja) 2012-11-14
TWI383529B (zh) 2013-01-21
TW200824170A (en) 2008-06-01

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