EP0021456A1 - Electrode for the electrolysis of water - Google Patents

Electrode for the electrolysis of water Download PDF

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Publication number
EP0021456A1
EP0021456A1 EP80200266A EP80200266A EP0021456A1 EP 0021456 A1 EP0021456 A1 EP 0021456A1 EP 80200266 A EP80200266 A EP 80200266A EP 80200266 A EP80200266 A EP 80200266A EP 0021456 A1 EP0021456 A1 EP 0021456A1
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Prior art keywords
surface layer
electrode
mol
titanium
catalyst
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EP80200266A
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German (de)
French (fr)
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EP0021456B1 (en
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René Dr. Dipl.-Phys. Müller
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BBC Brown Boveri AG Switzerland
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)

Abstract

Elektrode für die Wasserelektrolyse, bestehend aus einer auf einer Seite mit Rillen (2) versehenen porösen Graphitplatte (1), welche auf der anderen Seite mit einer aus Titan und Titandioxyd bestehenden dünnen Oberflächenschicht (3) versehen ist. Die Oberflächenschicht (3) ist in vorteilhafter Weise mit einem zu 20 mol-% aus Rutheniumoxyd und zu 80 mol-% aus Iridiumoxyd bestehenden Katalysator (4) dotiert.Electrode for water electrolysis, consisting of a porous graphite plate (1) provided with grooves (2) on one side, which is provided on the other side with a thin surface layer (3) made of titanium and titanium dioxide. The surface layer (3) is advantageously doped with a catalyst (4) consisting of 20 mol% of ruthenium oxide and 80 mol% of iridium oxide.

Description

Die Erfindung geht aus von einer Elektrode nach der Gattung des Anspruchs l.The invention relates to an electrode according to the preamble of claim 1.

Elektroden sowie Verfahren zu deren Herstellung sind vor allem von der für Brennstoffzellen entwickelten Technologie her bekannt (z.B. Carl Berger, Handbook of Fuel Cell Technology S. 401-406, Prentice Hall 1968; H.A. Liebhafsky and E.J. Cairns, Fuel Cells and Fuel Batteries, S. 289-294, John Wiley & Sons, 1968). Die Forderung nach genau definierten Reaktionszonen bedingt einen vielschichtigen Aufbau und spezielle Behandlungsverfahren derartiger Brennstoffzellen-Elektroden.Electrodes and processes for their production are known primarily from the technology developed for fuel cells (e.g. Carl Berger, Handbook of Fuel Cell Technology pp. 401-406, Prentice Hall 1968; HA Liebhafsky and EJ Cairns, Fuel Cells and Fuel Batteries, p 289-294, John Wiley & Sons, 1968). The requirement for precisely defined reaction zones requires a multilayer structure and special treatment processes for such fuel cell electrodes.

Für die Wasserzersetzung sind die oben beschriebenen Elektroden in ihrem Aufbau zu kompliziert und ihre Fertigungsmethoden zu aufwendig und kostspielig. Dies gilt insbesondere im Hinblick auf Herstellungsmethoden für industrielle Grossanlagen zur wirtschaftlichen Erzeugung von Wasserstoff.The structure of the electrodes described above is too complicated for water decomposition and their manufacturing methods are too complex and costly. This applies in particular with regard to manufacturing methods for large industrial plants for the economical production of hydrogen.

Elektroden für Wasserzersetzungszellen sind bereits vorgeschlagen worden (z.B. US-PS 4 039 409). Zur-Beschleunigung der elektrochemischen Reaktionen werden sie meist mit Katalysatoren dotiert.Electrodes for water decomposition cells have already been proposed (eg US Pat. No. 4,039,409). To accelerate the electrochemical reactions, they are usually used with kata dysers doped.

Die beschriebenen Elektroden lassen sowohl bezüglich ihrer mechanischen und chemischen Eigenschaften zu wünschen übrig. Das gleiche gilt bezüglich der verwendeten Katalysatoren.The described electrodes leave something to be desired in terms of their mechanical and chemical properties. The same applies to the catalysts used.

Der Erfindung liegt die Aufgabe zugrunde, eine Elektrode für die Wasserelektrolyse anzugeben, welche bei guter mechanischer und chemischer Stabilität, hoher elektrischer Leitfähigkeit und guter Durchlässigkeit für Wasser und Gas eine hohe Lebensdauer sowie die Eigenschaft besitzt, die Wasserzersetzungsreaktion katalytisch in optimaler Weise zu beschleunigen.The invention has for its object to provide an electrode for water electrolysis, which with good mechanical and chemical stability, high electrical conductivity and good permeability to water and gas has a long life and the property to catalytically accelerate the water decomposition reaction in an optimal manner.

Diese Aufgabe wird erfindungsgemäss durch die Merkmale des Anspruchs 1 gelöst.According to the invention, this object is achieved by the features of claim 1.

Es hat sich gezeigt, dass es vorteilhaft ist, als Elektrodenmaterial einen porösen, durchlässigen Werkstoff auf-Kohlenstoffbasis zu benutzen und seine dem Elektrolyt zugewandte Oberfläche durch Titan/Titandioxyd vor korrosivem Angriff zu schützen. Als Katalysator ist eine aus Platinmetalloxyden bestehende Imprägnierung, vorzugsweise eine Mischung von Rutheniumoxyd und Iridiumoxyd, vorgesehen.It has been shown that it is advantageous to use a porous, permeable carbon-based material as the electrode material and to protect its surface facing the electrolyte from corrosive attack by means of titanium / titanium dioxide. An impregnation consisting of platinum metal oxides, preferably a mixture of ruthenium oxide and iridium oxide, is provided as the catalyst.

Die Erfindung wird anhand des nachfolgenden, durch eine Figur erläuterten Ausführungsbeispiels näher beschrieben.The invention is described in more detail with reference to the following exemplary embodiment explained by a figure.

Dabei zeigt die FigurThe figure shows

den Querschnitt durch eine Elektrode.the cross section through an electrode.

1 ist eine Platte aus porösem Graphit, deren der Wasserzufuhr zugekehrte Seite mit einem Raster von Rillen 2 versehen ist. 3 stellt die aus einer Mischung von Titan und Titandioxyd bestehende elektrolytseitige Oberflächenschicht dar. 4 ist die in der Oberflächenschicht enthaltene Katalysator-Dotierung bestehend aus einer Mischung von 20 mol-% Rutheniumoxyd und 80 mol-% Iridiumoxyd. Die Platte 1 kann in ihrer Grundrissform kreisrund, quadratisch, rechteckig, sechseckig oder achteckig ausgeführt sein.1 is a plate made of porous graphite, the side facing the water supply is provided with a grid of grooves 2. 3 represents the electrolyte-side surface layer consisting of a mixture of titanium and titanium dioxide. 4 is the catalyst doping contained in the surface layer consisting of a mixture of 20 mol% ruthenium oxide and 80 mol% iridium oxide. The shape of the plate 1 can be circular, square, rectangular, hexagonal or octagonal.

Ausführungsbeispiel:Design example:

In eine fein-poröse Graphitplatte 1 von 60 mm Durchmesser und 4 mm Dicke (z.B. Qualität S 1602 von Le Carbone AG) wurden mit Hilfe eines Fräsers Rillen 2 in Form eines Rasters aus einer der Oberflächen herausgearbeitet. Bei einer gesamten Oberfläche von 28cm2 war die Breite und Tiefe der Rillen quadratischen Querschnitts je 1 mm, ihr gegenseitiger Abstand je 2 mm. Hierauf wurde die glatte Oberfläche der Platte 1, welche im Betrieb dem Feststoffelektrolyten zugewandt ist, im Vakuum von 10-5 bis 10 torr durch Glimmentladungen während 5 Minuten gereinigt. Danach wurde bei einer Aufdampfgeschwindigkeit von 10 bis 20 9/sec eine Titan-Schicht von total ca. 1000 R auf diese Oberfläche der Platte aufgedampft. Im Betrieb besteht diese Oberflächenschicht 3 dank örtlicher Oxydation zum grossen ; Teil aus Titan, zum kleineren aus Titandioxyd. Dadurch wird der darunterliegende Kohlenstoff (Graphit) der Platte 1 vor korrosivem Angriff (Oxydation durch entstehenden Sauerstoff) wirksam geschützt.In a fine-porous graphite plate 1 60 mm in diameter and 4 mm thick (eg quality S 1602 from Le Carbone AG), grooves 2 in the form of a grid were worked out from one of the surfaces with the aid of a milling cutter. With a total surface area of 28 cm 2 , the width and depth of the grooves were square in cross-section each 1 mm, their mutual spacing each 2 mm. The smooth surface of plate 1, which faces the solid electrolyte during operation, was then cleaned in a vacuum of 10 -5 to 10 torr by glow discharges for 5 minutes. A titanium layer totaling about 1000 R was then evaporated onto this surface of the plate at an evaporation rate of 10 to 20 9 / sec. In operation, this surface layer 3 is large thanks to local oxidation; Part made of titanium, the smaller one made of titanium dioxide. As a result, the underlying carbon (graphite) of the plate 1 is effectively protected against corrosive attack (oxidation by the formation of oxygen).

Die auf diese Art und Weise vorbereitete Platte 1 wurde nun während 10 sec in eine alkoholische Lösung getaucht, welche ca. 15 rel. Gew.-% Rutheniumchlorid (RuCl3) und 85 rel. Gew.-% Iridiumchlorid (IrCl3) enthielt. Nach dem Abtropfen während 1 min wurde die Platte 1 während 10 min bei einer Temperatur von 3750C in Luft oxydiert. Dieser Prozess des Eintauchens und Oxydierens wurde insgesamt 5 Mal wiederholt. Zum Schluss wurde die Platte 1 nochmals während 4 h bei einer Temperatur von 375°C in Luft oxydiert. Derart wurde auf der Plattenoberfläche die Katalysator-Dotierung 4, bestehend aus ca. 20 mol-% Rutheniumoxyd (Ru02) und 80 mol-% Iridiumoxyd gebildet. Wie sich in der Praxis gezeigt hat, weist eine derartige Oxydmischung optimale Katalysatoreigenschaften auf.The plate 1 prepared in this way was now immersed in an alcoholic solution for 10 sec. Wt .-% ruthenium chloride (RuCl3) and 85 rel. Wt .-% iridium chloride (IrCl 3 ) contained. After draining for 1 min, plate 1 was oxidized in air for 10 min at a temperature of 375 ° C. This immersion and oxidizing process was repeated 5 times in total. Finally, plate 1 was oxidized again in air for 4 h at a temperature of 375 ° C. In this way, the catalyst doping 4 consisting of approximately 20 mol% ruthenium oxide (Ru0 2 ) and 80 mol% iridium oxide was formed on the plate surface. As has been shown in practice, such an oxide mixture has optimal catalyst properties.

Die Elektrode besticht vor allem durch ihren ausserordentlich einfachen Aufbau. Zudem ist ihre Herstellung verhältnismässig billig, da Kohlenstoff (Elektrokohle, Graphit) ein preiswertes Ausgangsmaterial darstellt.The electrode is particularly impressive due to its extremely simple structure. In addition, their production is relatively cheap, since carbon (electric coal, graphite) is an inexpensive starting material.

Das beschriebene Verfahren lässt sich in besonders vorteilhafter Weise bei der Herstellung von Elektroden für Hochleistungs-Wasserzersetzungsapparate zur Herstellung von Wasserstoff anwenden. Dank der Einfachheit und Wirtschaftlichkeit des auf diese Art und Weise hergestellten Produkts eignet sich dieses vorzüglich für serienmässige, grossflächige Elektroden für industrielle Grossanlagen.The described method can be used in a particularly advantageous manner in the production of electrodes for high-performance water decomposition apparatus for the production of hydrogen. Thanks to the simplicity and economy of the product manufactured in this way, it is ideally suited for standard, large-area electrodes for large industrial plants.

Die auf diese Art hergestellten Elektroden zeichnen sich durch hohe chemische Beständigkeit und eine günstige Zersetzungsspannung aus.The electrodes manufactured in this way are characterized by high chemical resistance and a favorable decomposition voltage.

B e z e i c h n u n g s l i s t eB e z e i c h n u n g s l i s t e

  • 1 = Platte aus porösem Graphit1 = plate made of porous graphite
  • 2 = Rillen2 = grooves
  • 3 = Oberflächenschicht aus Ti/Ti02 3 = surface layer made of Ti / Ti0 2
  • 4 = Katalysator-Dotierung aus 20 Ru02/80 Ir02 (Mol-Verhältnis)4 = catalyst doping of 20 Ru0 2/80 Ir0 2 (molar ratio)

Claims (4)

1. Elektrode für die Wasserelektrolyse auf der Basis eines Verbundwerkstoffes, dadurch gekennzeichnet, dass sie aus einer porösen, auf einer Seite mit Rillen (2) versehenen Graphitplatte (1) besteht, welche auf der anderen Seite eine aus Titan und Titandioxyd bestehende dünne Oberflächenschicht (3) aufweist.1. Electrode for water electrolysis based on a composite material, characterized in that it consists of a porous graphite plate (1) provided with grooves (2) on one side, which on the other side has a thin surface layer consisting of titanium and titanium dioxide ( 3). 2. Elektrode nach Anspruch 1, dadurch gekennzeichnet, dass die aus Ti und Ti02 bestehende Oberflächenschicht (3) eine Dicke von 0,1_bis 0,5 f aufweist.2. Electrode according to claim 1, characterized in that the surface layer (3) consisting of Ti and Ti0 2 has a thickness of 0.1 to 0.5 f. 3. Elektrode nach Anspruch 1, 2 oder 3, dadurch gekennzeichnet, dass die Oberflächenschicht (3) ausserdem mit einem Katalysator (4) aus einer Mischung von Platinmetall-Verbindungen dotiert ist.3. Electrode according to claim 1, 2 or 3, characterized in that the surface layer (3) is also doped with a catalyst (4) made of a mixture of platinum metal compounds. 4. Elektrode nach Anspruch 4, dadurch gekennzeichnet, dass die Katalysator-Dotierung (4) der Oberflächenschicht (3) zu 20 mol-% aus Ru02 und zu 80 mol-% aus Ir02 besteht.4. Electrode according to claim 4, characterized in that the catalyst doping (4) of the surface layer (3) consists of 20 mol% of Ru0 2 and 80 mol% of Ir0 2 .
EP80200266A 1979-06-29 1980-03-24 Electrode for the electrolysis of water Expired EP0021456B1 (en)

Applications Claiming Priority (2)

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CH608279 1979-06-29
CH6082/79 1979-06-29

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EP0021456A1 true EP0021456A1 (en) 1981-01-07
EP0021456B1 EP0021456B1 (en) 1983-05-18

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0683247A1 (en) * 1994-05-20 1995-11-22 Bayer Ag Process for manufacturing stable graphite cathodes for the electrolysis of chlorhydric acid
EP0768390A1 (en) * 1995-09-21 1997-04-16 Karpov Institute of Physical Chemistry Electrodes and methods of preparation thereof
WO2007119130A1 (en) * 2006-04-14 2007-10-25 Toyota Jidosha Kabushiki Kaisha Fuel cell
CN106222694A (en) * 2016-08-25 2016-12-14 山东清大银光金属海绵新材料有限责任公司 The preparation method of sponge structure Alloy ternary oxide layer hydrogen evolution electrode material

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US4457824A (en) * 1982-06-28 1984-07-03 General Electric Company Method and device for evolution of oxygen with ternary electrocatalysts containing valve metals
US4707229A (en) * 1980-04-21 1987-11-17 United Technologies Corporation Method for evolution of oxygen with ternary electrocatalysts containing valve metals
JPS5937662A (en) * 1982-08-24 1984-03-01 Kureha Chem Ind Co Ltd Electrode substrate for monopolar type fuel cell with two-layer structure
US4849254A (en) * 1988-02-25 1989-07-18 Westinghouse Electric Corp. Stabilizing metal components in electrodes of electrochemical cells
US5332496A (en) * 1993-04-12 1994-07-26 Electrocom Gard, Ltd. System for performing catalytic dehalogenation of aqueous and/or non-aqueous streams
DE19844329B4 (en) * 1998-09-28 2010-06-17 Friedrich-Schiller-Universität Jena Process for the treatment of microorganisms and pollutants
US6936370B1 (en) * 1999-08-23 2005-08-30 Ballard Power Systems Inc. Solid polymer fuel cell with improved voltage reversal tolerance
US20040013935A1 (en) * 2002-07-19 2004-01-22 Siyu Ye Anode catalyst compositions for a voltage reversal tolerant fuel cell
US7241691B2 (en) * 2005-03-28 2007-07-10 Freescale Semiconductor, Inc. Conducting metal oxide with additive as p-MOS device electrode
US7510956B2 (en) * 2006-01-30 2009-03-31 Fressscale Semiconductor, Inc. MOS device with multi-layer gate stack
WO2008024465A2 (en) * 2006-08-25 2008-02-28 Bdf Ip Holdings Ltd. Fuel cell anode structure for voltage reversal tolerance
US7608358B2 (en) * 2006-08-25 2009-10-27 Bdf Ip Holdings Ltd. Fuel cell anode structure for voltage reversal tolerance
AT511433B1 (en) * 2011-11-03 2012-12-15 Pro Aqua Diamantelektroden Gmbh & Co Kg ELECTRODE, ITS USE AND ELECTROCHEMICAL CELL
CN103088362B (en) * 2012-12-13 2015-12-23 苏州赛斯德工程设备有限公司 A kind of Tubular titanium anode
PT106779A (en) * 2013-02-13 2014-08-13 José Jo O Santana Campos Rodrigues ELECTROLYTEER AND PRODUCTION PROCESS OF SYNTHESIS GAS, BY ELECTROLYSIS OF WATER, USING GRAPHITE / CARBON ELECTRODES

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FR1398388A (en) * 1963-06-10 1965-05-07 Imp Metal Ind Kynoch Ltd Electrolyser
DE1286513B (en) * 1966-03-18 1969-01-09 Bayer Ag Anode for electrolytic processes
AT313313B (en) * 1971-01-08 1974-02-11 Metallgesellschaft Ag Electrode, in particular anode, for chlor-alkali electrolysis and method for producing the electrode
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0683247A1 (en) * 1994-05-20 1995-11-22 Bayer Ag Process for manufacturing stable graphite cathodes for the electrolysis of chlorhydric acid
US5575985A (en) * 1994-05-20 1996-11-19 Bayer Aktiengesellschaft Preparation of stable graphite
CN1052038C (en) * 1994-05-20 2000-05-03 拜尔公司 Preparation of stable graphite cathodes for the electrolysis of hydrochloric acid
EP0768390A1 (en) * 1995-09-21 1997-04-16 Karpov Institute of Physical Chemistry Electrodes and methods of preparation thereof
WO2007119130A1 (en) * 2006-04-14 2007-10-25 Toyota Jidosha Kabushiki Kaisha Fuel cell
CN106222694A (en) * 2016-08-25 2016-12-14 山东清大银光金属海绵新材料有限责任公司 The preparation method of sponge structure Alloy ternary oxide layer hydrogen evolution electrode material
CN106222694B (en) * 2016-08-25 2018-01-02 山东清大银光金属海绵新材料有限责任公司 Sponge structure alloy loads the preparation method of ternary oxide layer hydrogen evolution electrode material

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DE2928911A1 (en) 1981-01-29
DE3063253D1 (en) 1983-07-07
EP0021456B1 (en) 1983-05-18
US4348268A (en) 1982-09-07

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