EP1730328A2 - Procede pour realiser des revetements en oxyde d'iridium - Google Patents

Procede pour realiser des revetements en oxyde d'iridium

Info

Publication number
EP1730328A2
EP1730328A2 EP05735009A EP05735009A EP1730328A2 EP 1730328 A2 EP1730328 A2 EP 1730328A2 EP 05735009 A EP05735009 A EP 05735009A EP 05735009 A EP05735009 A EP 05735009A EP 1730328 A2 EP1730328 A2 EP 1730328A2
Authority
EP
European Patent Office
Prior art keywords
colloidal
ircl
iridium oxide
aqueous
salt
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP05735009A
Other languages
German (de)
English (en)
Inventor
Manfred Theodor Reetz
Hendrik Schulenburg
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Studiengesellschaft Kohle gGmbH
Original Assignee
Studiengesellschaft Kohle gGmbH
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 Studiengesellschaft Kohle gGmbH filed Critical Studiengesellschaft Kohle gGmbH
Publication of EP1730328A2 publication Critical patent/EP1730328A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
    • C01G55/004—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1225—Deposition of multilayers of inorganic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1241—Metallic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1283—Control of temperature, e.g. gradual temperature increase, modulation of temperature
    • 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
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound

Definitions

  • the present invention relates to a process for the production of coatings from iridium oxide, a colloidal iridium oxide and a process for the production of colloidal iridium oxide.
  • Metal oxide coated titanium electrodes are used in several electrochemical processes
  • Iridium oxide coatings in particular have proven their worth for the electrocatalysis of oxygen evolution. Iridium mixed oxides such as lrO x -SnO 2 , lrRuO x , lrO x -Ta 2 O 5 and lrO x -Sb 2 O 5 -SnO 2 can also be used for the coating.
  • Oxide-coated titanium electrodes are mostly produced by thermal decomposition of metal salts. Suitable metal salts are dissolved in water or alcohols and the electrodes are wetted with the solution. Then they are wetted
  • Electrodes typically heated at temperatures between 400 and 700 ° C.
  • the metal salts decompose under these conditions and form the corresponding metal oxides or mixed oxides. Electrodes manufactured in this way often have good mechanical stability, a satisfactory service life and show a low overvoltage for the development of oxygen.
  • the electrodes are expensive due to the high iridium load (at least 7.5 g iridium per square meter of titanium).
  • US Pat. No. 3,234,110 discloses that titanium sheets are coated with an ethanolic IrCl 4 solution and heated to 250-300 ° C. The process is repeated 4 times. The Ti / IrO x electrodes obtained can be used for the electrolysis of NaCl solutions become. No information is given about the life of the coating during the chlorine development.
  • U.S. Patent 3,926,751 describes a method of preparing Ti / IrTaO x electrodes. Titanium sheets are immersed in a solution of IrCI 3 and TaCI 5 12 to 15 times and each heated at 450 to 550 ° C. The electrodes show a lifespan of about 6000 h during the development of oxygen in 10% sulfuric acid.
  • U.S. Patents 5,294,317, 5,098,546, and 5,156,726 describe methods of making electrodes for oxygen evolution. Titanium electrodes, which are coated with mixed oxides, are produced by multiple, usually 10 times, immersion in butanolic solutions of H 2 lrCl 6 and tantalum ethoxide and subsequent firing at 500 ° C. A lifespan of more than 2000 hours is stated for the electrodes.
  • the electrode coatings described above due to the thermal decomposition of metal salts have the disadvantage that toxic gases are released when the electrodes are burned, in particular Cl 2 and HCl.
  • Titanium sheets are sandblasted, etched with 10% oxalic acid and immersed in an alcoholic ruthenium acetylacetonate / iridium acetylacetonate solution.
  • the wetted electrodes are then pyrolyzed at 400-600 ° C.
  • the wetting and pyrolysis process is repeated several times until a coating thickness of at least
  • the object of the invention was to develop a method which does not have the disadvantages described above and which enables coatings to be made from iridium oxides using low-chloride compounds.
  • a further object of the present invention was to coat titanium electrodes with low-chloride iridium oxides.
  • the present invention relates to a method for producing coatings of iridium oxide, which comprises the following steps: a) applying colloidal lRO x , where x is a number from 1 to 2, to a surface, b) drying the coated surface and c ) Firing the surface at a temperature of 300 to 1000 ° C, wherein steps a to c can be repeated until the desired layer thickness is obtained.
  • the method according to the invention becomes colloidal
  • the colloidal iridium oxide used according to the invention can be obtained in any manner known from the prior art.
  • a Brönsted base is added to an aqueous, alcoholic and / or aqueous-alcoholic solution of an Ir salt, optionally with stirring.
  • Particularly suitable Bronsted bases are alkali metal hydroxides, in particular NaOH or KOH.
  • a colloidal iridium oxide solution is formed.
  • the aqueous, alcoholic and / or aqueous-alcoholic solution of an Ir salt optionally with stirring.
  • Particularly suitable Bronsted bases are alkali metal hydroxides, in particular NaOH or KOH.
  • a colloidal iridium oxide solution is formed.
  • the a Brönsted base is added to an aqueous, alcoholic and / or aqueous-alcoholic solution of an Ir salt, optionally with stirring.
  • Particularly suitable Bronsted bases are alkali metal hydroxides, in particular NaOH or KOH.
  • Water-soluble Ir salts are preferably used to produce the colloidal iridium oxide.
  • the water-soluble Ir salts can be selected from the halides, nitrates, sulfates, acetates, acetylacetonates, the hydrates of the above and the
  • IrCl 3 xH 2 O, IrCl 4 xH 2 O, H 2 IrCl 6 xH 2 O, Na 2 IrCl 6 xH 2 O, K 2 IrCl 6 xH 2 O are particularly preferred.
  • the method according to the invention can be used for coating any surface that is stable at the firing temperature. It works particularly well for coating metal and metal oxide surfaces, in particular Ti, TiO 2 , ZnO, SnO 2 , and glass.
  • a particularly suitable area of application for the method according to the invention is the coating of Ti electrodes.
  • Such electrodes are used for the development of oxygen and chlorine or for the oxidation of organic residues in drinking water.
  • Colloidal iridium oxide as used in the process described above is new.
  • Another object of the present invention is accordingly a colloidal
  • Iridium oxide which has a particle size ⁇ 10 nm, in particular ⁇ 3 nm.
  • the colloidal iridium oxide can be obtained by adjusting an aqueous, alcoholic or aqueous-alcoholic solution of an Ir salt with stirring to a pH> 11, preferably> _12 and then adding the resulting mixture over a period of 3 to 72 hours a temperature of 0 to 100 ° C is stirred.
  • the iridium oxide obtained can be used for the production of coatings without further processing. If necessary, any undesirable soluble ingredients can be cleaned and removed by dialysis.
  • iridium chlorides are converted into iridium oxide colloids by basic hydrolysis.
  • the colloids could be produced as concentrated hydrosols without additional stabilizers.
  • the chloride concentration of the solution can be greatly reduced by dialysis. Titanium substrates can be wetted with the processed colloidal solution. The burning of the wetted electrodes leads to closed lrO x films. No or only minimal amounts of toxic gases are released during the firing process, since chloride may be bound in the form of the salts when the alkali metal hydroxides are used as Bronsted base as alkali metal chloride. Examples
  • Titanium sheets were sandblasted, transferred to deionized water and cleaned with ultrasound for 10 minutes. The sheets were then placed in hot (70-90 ° C.) 10% oxalic acid for 5 minutes and rinsed with deionized water before they were ultrasonically cleaned again.
  • the pretreated titanium sheets were immersed in the dialyzed colloidal lrO x solution and dried at 80 ° C for 5 minutes before being baked at 600 ° C for 5 minutes. This coating process was repeated 5 times. The burning process was carried out over 1 hour.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Ceramic Engineering (AREA)
  • Electrochemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Chemically Coating (AREA)
  • Paints Or Removers (AREA)

Abstract

L'invention concerne un procédé pour réaliser des revêtements en oxyde d'iridium selon les opérations suivantes: a) appliquer sur une surface de l'IrOX colloïdal, x étant un nombre de 1 à 2, b) sécher la surface ainsi recouverte et c) cuire la surface à une température allant de 300 à 1000 °C, les opérations a) à c) pouvant être répétées jusqu'à obtention de l'épaisseur de couche voulue. L'utilisation d'IrOX colloïdal comme composant de départ pour réaliser des revêtements en IrOX permet d'éviter la formation de gaz toxiques pendant la cuisson.
EP05735009A 2004-03-31 2005-03-09 Procede pour realiser des revetements en oxyde d'iridium Withdrawn EP1730328A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004015633A DE102004015633A1 (de) 2004-03-31 2004-03-31 Verfahren zur Herstellung von Beschichtungen aus Iridiumoxiden
PCT/DE2005/000399 WO2005095671A2 (fr) 2004-03-31 2005-03-09 Procede pour realiser des revetements en oxyde d'iridium

Publications (1)

Publication Number Publication Date
EP1730328A2 true EP1730328A2 (fr) 2006-12-13

Family

ID=34965127

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05735009A Withdrawn EP1730328A2 (fr) 2004-03-31 2005-03-09 Procede pour realiser des revetements en oxyde d'iridium

Country Status (5)

Country Link
US (1) US20080248195A1 (fr)
EP (1) EP1730328A2 (fr)
JP (1) JP5090901B2 (fr)
DE (1) DE102004015633A1 (fr)
WO (1) WO2005095671A2 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8022004B2 (en) 2008-05-24 2011-09-20 Freeport-Mcmoran Corporation Multi-coated electrode and method of making
US20160056409A1 (en) * 2013-03-28 2016-02-25 National Institute For Materials Science Organic el element and method for manufacturing same
US9790605B2 (en) 2013-06-27 2017-10-17 Yale University Iridium complexes for electrocatalysis
US10081650B2 (en) 2013-07-03 2018-09-25 Yale University Metal oxide-organic hybrid materials for heterogeneous catalysis and methods of making and using thereof
CN105803482A (zh) * 2016-03-17 2016-07-27 同济大学 一种电解水制氢用电解池的集电极材料的改性方法及用途
KR101773564B1 (ko) 2016-03-31 2017-08-31 유니테크 주식회사 전해반응기용 다공성 이리듐 전극의 제조방법
CN106854001B (zh) * 2016-12-19 2018-06-19 有研亿金新材料有限公司 一种三氯化铱的控制还原制备方法
CN115872466B (zh) * 2022-12-15 2023-09-08 苏州擎动动力科技有限公司 一种铱的氧化物及其制备方法

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EP0898318A2 (fr) * 1997-08-01 1999-02-24 Matsushita Electric Industrial Co., Ltd. Procédé de préparation de poudre catalytique pour électrode

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Also Published As

Publication number Publication date
JP5090901B2 (ja) 2012-12-05
WO2005095671A2 (fr) 2005-10-13
DE102004015633A1 (de) 2005-10-20
WO2005095671A3 (fr) 2006-05-11
JP2007530793A (ja) 2007-11-01
US20080248195A1 (en) 2008-10-09

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