EP0033363B1 - Procédé de revêtement d'une électrode poreuse - Google Patents
Procédé de revêtement d'une électrode poreuse Download PDFInfo
- Publication number
- EP0033363B1 EP0033363B1 EP80107001A EP80107001A EP0033363B1 EP 0033363 B1 EP0033363 B1 EP 0033363B1 EP 80107001 A EP80107001 A EP 80107001A EP 80107001 A EP80107001 A EP 80107001A EP 0033363 B1 EP0033363 B1 EP 0033363B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- electrode
- compounds
- metals
- process according
- platinum
- 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.)
- Expired
Links
- 238000000034 method Methods 0.000 title claims description 19
- 230000008569 process Effects 0.000 title claims description 13
- 238000000576 coating method Methods 0.000 title claims description 10
- 239000011248 coating agent Substances 0.000 title claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 30
- 239000002184 metal Substances 0.000 claims description 30
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 29
- 150000001875 compounds Chemical class 0.000 claims description 26
- 150000002739 metals Chemical class 0.000 claims description 16
- 230000004913 activation Effects 0.000 claims description 14
- 229910052697 platinum Inorganic materials 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 239000011148 porous material Substances 0.000 claims description 12
- -1 platinum metals Chemical class 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 238000001311 chemical methods and process Methods 0.000 claims 1
- 238000005530 etching Methods 0.000 claims 1
- 238000010792 warming Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 7
- 230000003213 activating effect Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000002270 dispersing agent Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- 229910001060 Gray iron Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- SSVFCHUBLIJAMI-UHFFFAOYSA-N platinum;hydrochloride Chemical compound Cl.[Pt] SSVFCHUBLIJAMI-UHFFFAOYSA-N 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- 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
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
-
- 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
-
- 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
Definitions
- the invention relates to a method for coating a porous electrode for electrochemical processes with an activation layer which at least partially covers the electrode surface and contains metals or compounds of metals of the platinum group.
- Electrodes for electrochemical processes e.g. B. of anodes for chlor-alkali electrotysis, from a resistant to the electrotysis products and a passivation layer forming material under the conditions of electrolysis
- numerous methods have become known, the purpose of which essentially consists of a platinum metal or platinum metal-containing compounds in an electrochemically effective degree of dispersion anchor the electrode or the electrode core mechanically.
- DE-B-1155762 it is known to galvanically coat degreased and etched titanium plates with a platinum metal and the plates in a first thermal cycle in an inert atmosphere and in a second cycle in an oxidizing atmosphere up to a temperature of approximately To heat 800 ° C.
- This treatment gives a firmly adhering activation layer and at the same time improved protection of the electrode material by converting the titanium core, which is exposed in the pores of the activation layer and has a thin barrier layer made of titanium oxide, into rutile.
- this and other known coating methods are less suitable for porous electrodes, for example for sintered electrodes according to DE-A-23 05 175 or electrodes made of titanium suboxide according to DE-B-24 05 010.
- the adhesive strength of the activation layers is particularly favorable for porous electrodes and for The large surface area of the electrode is advantageous for numerous electrochemical processes.
- the invention has for its object to provide a coating method for porous electrodes that does not have the disadvantages described, especially the comparatively large need for activating agents, and results in highly effective activation layers with small amounts of platinum metals.
- the object is achieved according to the invention with a method of the type mentioned at the outset by coating the electrode surface with a fine-grained compounds of metals of the platinum group and a suspension containing the compounds which dissolve the compounds at an elevated temperature, the fine-grained compounds of the metals having a particle diameter, that only the dispersing agent can get into the pores of the electrode, but not the fine-grained compounds, that the dispersed phase of the suspending agent is dissolved, deposited on the electrode surface by evaporation of the agent and decomposed by heating the electrode to a temperature between 250 and 350 ° C and that the cycle is repeated several times and the electrode is then heated to a temperature between 400 and 600 ° C. in an oxygen-containing atmosphere.
- the invention is based on the knowledge that particles dispersed in a suspension cannot get into pores which are only accessible through narrow hoses or channels, whereas the dispersing agent fills these pores.
- the particle diameter must therefore correspond to the pore diameter. If the electrode is heated after coating, the dispersant emerges from the pores and, because of the increasing solubility of the platinum group compounds used according to the invention, dissolves the particles concentrated at the pore entrances.
- the solution which is in a thin layer, has a relatively high toughness and is distributed evenly over the outer electrode surface and the surface of larger pores accessible from the outer surface without penetrating into narrow channel and tube pores.
- the compounds deposited by evaporation of the solvent in a uniform layer thickness are then decomposed by heating the electrode to a temperature between 250 and 350 ° C., whereby a fissured, metallic surface coating having a large specific surface is formed.
- the layer thickness of about 1 ⁇ m required for technical purposes is obtained by repeating the coating cycle several times.
- the invention provides for the heating of the coated electrode in an oxidizing atmosphere, preferably in air, to a temperature between 400 and 600 ° C.
- the main purpose of the thermal treatment is to passivate the electrode surface exposed in the pores of the activation layer and to anchor the activation layer on this surface.
- Partial oxidation of the platinum metals contained in the activation layer is not harmful, since the growth of the metal crystals is inhibited and finely dispersed layers have greater electrochemical activity.
- the treatment temperature should therefore not fall below or exceed the temperature range of 400 to 600 ° C.
- the heating time is expediently about 3 to 60 minutes and can be easily determined by simple experiments for each electrode material and each compound used as an activating agent.
- compounds of non-platinum metals are dispersed in the dispersant in addition to compounds of metals from the platinum group.
- Suitable non-platinum metals are tantalum, zirconium, niobium, aluminum and especially titanium.
- the activation layer then contains a finely dispersed mixture of platinum metals, oxides of platinum metals and oxides of non-platinum metals.
- thermally decomposable complex compounds which contain free acid, in particular compounds from the group oxotato, formiato, tartrato and citrate complexes of metals from the group ruthenium, are used as compounds of metals of the platinum group and of non-platinum metals , Rhodium, palladium, iridium and platinum and analogous compounds of non-platinum metals.
- the dispersant used according to the invention dissolves the complex compounds at elevated temperature, preferably with the electrode surface, in particular passivating layers, being formed by caustic solutions. Water and optionally aqueous oxalic acid solutions are particularly suitable for this purpose. In this process, the primer is improved without the formation of corrosive and harmful vapors as in the known use of hydrochloric acid platinum metal chloride solutions.
- electrodes In principle, all electrically conductive metals, alloys and compounds that are stable under the conditions of electrochemical processes are suitable as electrodes.
- electrodes are preferably used, e.g. B. as an anode for chlor-alkali electrolysis, passivating layers forming metals such as titanium, tantalum, zirconium and niobium and according to the invention preferably electrodes which consist at least in part of titanium suboxide.
- the electrodes according to the invention have a porosity of about 10 to 50% and are generally produced by sintering moldings from a metal powder or an oxide powder.
- the anode potential was checked with a Luggin capillary measured the saturated calomel electrode.
- Composite plates as in Example 2 were treated with a slurry of 66 parts H 2 [Ru (C 2 O 4 ) 2 ] ⁇ 2.5 H 2 O, 70 parts H 2 [Ir (C 2 O 4 ) 3 ], 100 parts Ti 2 (C 2 O 4 ) 3 .10H 2 O coated in 1,000 parts of water and 50 parts of oxalic acid, annealed and the potentials measured.
Landscapes
- 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)
Claims (7)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3004080A DE3004080C2 (de) | 1980-02-05 | 1980-02-05 | Verfahren zum Beschichten einer porösen Elektrode |
DE3004080 | 1980-02-05 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0033363A1 EP0033363A1 (fr) | 1981-08-12 |
EP0033363B1 true EP0033363B1 (fr) | 1983-08-24 |
Family
ID=6093754
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP80107001A Expired EP0033363B1 (fr) | 1980-02-05 | 1980-11-13 | Procédé de revêtement d'une électrode poreuse |
Country Status (3)
Country | Link |
---|---|
US (1) | US4431686A (fr) |
EP (1) | EP0033363B1 (fr) |
DE (1) | DE3004080C2 (fr) |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4530742A (en) * | 1983-01-26 | 1985-07-23 | Ppg Industries, Inc. | Electrode and method of preparing same |
DE3472979D1 (en) * | 1983-06-28 | 1988-09-01 | Bbc Brown Boveri & Cie | Process for manufacturing a depassivating layer and depassivating layer on an electrode for an electrochemical cell |
JPS60159185A (ja) * | 1984-01-31 | 1985-08-20 | Permelec Electrode Ltd | 電極の製造方法 |
DE3516523A1 (de) * | 1985-05-08 | 1986-11-13 | Sigri GmbH, 8901 Meitingen | Anode fuer elektrochemische prozesse |
US4912286A (en) * | 1988-08-16 | 1990-03-27 | Ebonex Technologies Inc. | Electrical conductors formed of sub-oxides of titanium |
EP0696813B1 (fr) * | 1994-08-11 | 2002-10-02 | Canon Kabushiki Kaisha | Utilisation d'une solution pour la fabrication des dispositifs émetteur d'électrons et méthode de fabrication des dispositifs émetteur d'électrons |
JPH11111273A (ja) * | 1997-09-29 | 1999-04-23 | Furukawa Battery Co Ltd:The | リチウム二次電池用極板の製造法及びリチウム二次電池 |
US20060255692A1 (en) * | 2005-03-22 | 2006-11-16 | Motohiro Yasui | Piezoelectric Actuator, Ink-Jet Head, Method Of Producing Piezoelectric Actuator, And Method Of Producing Ink-Jet Head |
US20140161972A1 (en) * | 2012-12-09 | 2014-06-12 | National Sun Yat-Sen University | Method for forming conductive film at room temperature |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US28820A (en) * | 1860-06-19 | wright | ||
NL126075C (fr) * | 1959-04-27 | |||
AT223209B (de) * | 1959-04-27 | 1962-09-10 | Ici Ltd | Verfahren zur Herstellung eines Verbundkörpers, der aus einem Trägerkörper aus Titan und einem Überzug aus Platinmetallen besteht |
USRE28820E (en) | 1965-05-12 | 1976-05-18 | Chemnor Corporation | Method of making an electrode having a coating containing a platinum metal oxide thereon |
US3778307A (en) * | 1967-02-10 | 1973-12-11 | Chemnor Corp | Electrode and coating therefor |
GB1195871A (en) * | 1967-02-10 | 1970-06-24 | Chemnor Ag | Improvements in or relating to the Manufacture of Electrodes. |
US3562008A (en) * | 1968-10-14 | 1971-02-09 | Ppg Industries Inc | Method for producing a ruthenium coated titanium electrode |
US4070504A (en) * | 1968-10-29 | 1978-01-24 | Diamond Shamrock Technologies, S.A. | Method of producing a valve metal electrode with valve metal oxide semi-conductor face and methods of manufacture and use |
LU60168A1 (fr) * | 1970-01-09 | 1971-09-22 | ||
US3684543A (en) * | 1970-11-19 | 1972-08-15 | Patricia J Barbato | Recoating of electrodes |
US3924025A (en) * | 1972-02-02 | 1975-12-02 | Electronor Corp | Method of making an electrode having a coating of cobalt metatitanate thereon |
US4032427A (en) * | 1975-11-03 | 1977-06-28 | Olin Corporation | Porous anode separator |
JPS5393179A (en) * | 1977-01-27 | 1978-08-15 | Tdk Corp | Electrode for electrolysis and its manufacture |
-
1980
- 1980-02-05 DE DE3004080A patent/DE3004080C2/de not_active Expired
- 1980-11-13 EP EP80107001A patent/EP0033363B1/fr not_active Expired
-
1982
- 1982-09-01 US US06/413,961 patent/US4431686A/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
US4431686A (en) | 1984-02-14 |
DE3004080C2 (de) | 1986-03-20 |
EP0033363A1 (fr) | 1981-08-12 |
DE3004080A1 (de) | 1981-08-13 |
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