CN86104356A - Be used for electrolytic negative electrode and preparation method thereof - Google Patents
Be used for electrolytic negative electrode and preparation method thereof Download PDFInfo
- Publication number
- CN86104356A CN86104356A CN198686104356A CN86104356A CN86104356A CN 86104356 A CN86104356 A CN 86104356A CN 198686104356 A CN198686104356 A CN 198686104356A CN 86104356 A CN86104356 A CN 86104356A CN 86104356 A CN86104356 A CN 86104356A
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- Prior art keywords
- negative electrode
- layers
- coating
- metal
- substrate
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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
-
- 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
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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)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inert Electrodes (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The present invention relates to some negative electrodes.These negative electrodes are made up of the conductive substrate that has a coating, and this coating is made up of the multiple layer metal oxide compound, and its upper layer is made up of metal oxide semiconductor, and one of middle layer or middle layer are made up of V III family metal oxide containing precious metals.These negative electrodes are specially adapted in the electrolyzer of the aqueous solution of brine electrolysis or electrolytic alkali metal halide and have used in the electrolyzer of thin film technique.
Description
The present invention relates to a kind of new negative electrode that can be used for electrolytic process.The preparation method who relates to this negative electrode simultaneously.More particularly relate to a kind of negative electrode that can be used for the electrolysis alkali metal halide aqueous solution, because its low operating potential and electrochemical properties stability in time make it noticeable especially.
This negative electrode is to belong to activatory metallic cathode classification, and it obtains by coat various activated materials at cathode substrate, and its purpose comes down in order to be reduced in hydrogen overvoltage in the alkaline medium.
English Patent 1,511,719 have described a kind of negative electrode, and it comprises the coating of a metal substrate, a cobalt and second coating of a ruthenium.
United States Patent (USP) 4,100,049 has described a kind of negative electrode, and it comprises a substrate and a coating of being made up of the mixture of metal oxide containing precious metals and metal oxide semiconductor (the especially oxide compound of zirconium).
For example at United States Patent (USP) 3,216, a kind of method of the coating that one of coating is made up of nickel-palldium alloy on nickel substrate has been described in 919; According to this patent, alloy layer is added on the substrate with Powdered, then described powdered alloy is carried out sintering.
Publication No. is 54-110,983(United States Patent (USP) NO.4,465,580) Japanese patent application has been described a kind of negative electrode of coating, this coating is made up of the particle dispersion and the activator of nickel or nickelalloy, this activator is then by platinum, ruthenium, iridium, rhodium, palladium or osmium, or the oxide compound of these metals is formed.
Publication No. is 53-010,036 Japanese patent application has been described a kind of negative electrode, this negative electrode has substrate and alloy coat of a semiconductor alloy, this alloy coat is made up of a platinum metals and a semiconductor alloy at least, if suitable, also having one is the top coat of a platinum metals at least.
The invention provides a kind of new negative electrode, this negative electrode is specially adapted to the electrolysis of the aqueous solution of alkali metal halide, and said negative electrode is made up of the conductive substrate that has a coating, and this coating is based on the oxide compound of a platinum metals.This negative electrode is characterised in that, it has the coating that a multiple layer metal oxide compound is formed, its upper layer is made up of metal oxide semiconductor basically, middle layer or be that one of middle layer is made up of the oxide compound of a precious metal in the VIII family on the periodic table of elements basically at least.Here used " basically " speech, with regard to surface and middle layer, be meant that described layer is made up of relevant metal oxide only, or by the mixed oxide composition of second metal of a relevant metal and a low ratio (for example, rate is no more than 1/10 in molar ratio).
Said semiconductor alloy is with common popular art-recognized meanings among the present invention, that is to say, it is meant 4b, 5b beyond the dechromisation in the periodic table of elements and the metal of 6b family.
More particularly, negative electrode provided by the invention comprises substrate and coating of a conduction, said coating by with one or more layers titanium and/or one or more layers ruthenium oxide (RuO of interrelating of the oxide compound of zirconium
2) form.The present invention be more particularly directed to its coating and contain RuO
2And TiO
2Negative electrode.
Special in these negative electrodes what describe is these negative electrodes, and their coating comprises, from the conductive substrate number, and one or more layers RuO
2Back to back one or more layers TiO
2, or a series of one or more layers TiO
2/ one or more layers RuO
2/ one or more layers TiO
2In these a series of coatings, insert other precious metals or nonmetal oxide layer; Or between the upper layer that conductive substrate and dielectric medium directly contact, (the Ru that increases with X
xTi
1-x) O
2The RuO that replaces some or all
2And/or TiO
2, these all belong to scope of the present invention.As the implication among the present invention, say that exactly upper layer one speech refers to the oxide skin that its surface directly contacts with ionogen, the middle layer then is meant any layer between conductive substrate and said upper layer.In more detail, the invention provides that some or all are laminar in the coating of above-mentioned oxide cathode.
As implication among the present invention, thin slice one speech refers to plane film, the part of cylinder or the part of sphere, or the combination of above-mentioned these shapes, its thickness should be engraved described thin slice on one's mind with this tetragon less than 1/10 of the mean value of tetragon two length of sides, is possible for its thickness of mean value of the said length of side between 1 and 100 micron, or rather, between 3 and 30 microns.
As what point out already, this coating is whole or partly be made up of a metal oxide containing precious metals at least, and this precious metal is meant ruthenium, rhodium, palladium, osmium, iridium and platinum.The preferential oxide compound of selecting ruthenium or above-mentioned oxide compound and the combination of one or more other metal oxide containing precious metals among the present invention.
In the coating according to negative electrode of the present invention, the mol ratio of metal oxide containing precious metals and metal oxide semiconductor generally between 10/1 and 1/10, is preferably between 1/5 and 5/1.
Can select substrate material in the electro-conductive material.Can choose easily from the generic of being made up of nickel, stainless steel and soft steel, here, this explanation does not represent that any restriction is arranged.
This substrate can be plate or thin slice, grid, sheet metal, expanded metal or the aperture plate that has or do not have some apertures or hole.According to the Technology that is adopted, above-mentioned materials is made the plane, cylinder or other Any shape are possible.
The present invention also relates to prepare the method for these negative electrodes.
The bare bones of this method is in on-chip deposition, at first at random carries out a kind of appropriate pretreatment, and the coated with metal salt deposit is heat-treated whole work-piece more then, makes it become oxidised form.
If desired, the pre-treatment of substrate preferably includes skimming treatment, then is according to the method for knowing now, removes zone of oxidation by machinery and/or chemical process.
The bare bones of present method is that the metal salt solution layer deposits on the substrate one by one.
Suppose to deposit mixed oxide, can adopt identical technology or directly deposit the settled layer that contains above-mentioned two metal-salts.Usually, take metal refining salt with solution or form of suspension.According to the character of this salt, solvent or thinner can be by water, inorganic or organic acid, or organic solvent constitutes.Preferably with an organic solvent such as dimethyl formamide, alcohol, particularly ethanol or 2-Ethylhexyl Alcohol.Usually atoms metal concentration is 3 * 10
-2And 3 between the mol, is preferably between 1 and 2 mol.
The metal-salt that can be used in the present invention generally is made up of inorganic or organic metal salt, such as, halogenide, nitrate, carbonate, vitriol, acetate or acetylacetonate.Just generate the salt of platinum and ru oxide, it will be very favourable adopting chloroplatinic acid hexahydrate and ruthenium chloride hydrate.
Can carry out the deposition of above-mentioned salt deposit according to the method for routine: substrate is immersed in these solution or the suspension, on substrate, brush with painting brush, brush or similar utensil; And use electrostatic coating method.
The preparation of solution or suspension and deposition generally are to carry out in room temperature and air.If nature suitable, can increase temperature, can make its easy dissolving for some salt, and/or this operation can be to carry out in inert nitrogen or other gas atmosphere above-mentioned salt.
The general heat treating method that adopts realizes that metal-salt transfers oxide compound to.Dry in air earlier before heat-treating, purpose is to remove part or all of solvent or thinner.Bake out temperature can be up to 200 ℃, and the temperature range of special recommendation is 100-150 ℃, generally about dozens of minutes of time length.Specifically, generally be in air, to heat-treat, its temperature changes between 200 ℃ and 1000 ℃ by used salt.A temperature that is preferably between 400 ℃ and 750 ℃ is carried out, and general every layer of time length is between 15 minutes and 1 hour.Can carry out this transition heat after each oven dry back or last oven dry handles.
Negative electrode of the present invention is characterised in that conductive coating has fabulous adhesive power on substrate.
Negative electrode of the present invention is suitable for using in the electrolyzer of the brine electrolysis or the aqueous solution.This electrolytic product is exactly the hydrogen that discharges on negative electrode.This negative electrode is particularly useful for the electrolysis (particularly sodium chloride aqueous solution) of aqueous alkali metal chloride, and the electrolysis of water, such as the electrolysis that is used in potassium hydroxide aqueous solution.Available microporous type barrier film is as the disrupter in the electrolyzer, but negative electrode of the present invention is to pay special attention to thin film technique.
Following example explanation the present invention
Example 1
Substrate is made of a nickel sheet that is of a size of 200 * 10 * 0.6 millimeter
Carry out surface treatment with silicon carbide (250 microns of average particulate diameters).
A) at 23 ℃ of preparations, 2 gram RuCl
3XHClyH
2The solution of O promptly contains about 38% metal Ru (by weight) in 2 liters ethanol.
Be coated with the nickel sheet with this solution.Carry out air oven dry (120 ℃, 30 minutes), then in air, heat-treat (500 ℃, 30 minutes).After the cooling, repeat by coating/oven dry/heat treated order again.
1.4 milligrams/centimetre have been obtained
2RuO
2Settled layer, this settled layer is laminar its mean thickness between 3 and 30 microns, demonstrates RuO when checking with X-radiocrystallgraphy method
3Structure.
B) in the time of 23 ℃, prepare the TiOCl that in 2 liters ethanol, contains 2.5 mol Ti
22.6 liters of 2HCl solution.Carry out same coating/oven dry/thermal treatment (2 layers) with the same in a, so just deposited 0.8 milligram/centimetre
2TiO
2
C) this negative electrode is in the NaOH solution of 450 grams per liters in concentration, and temperature is 85 ℃, and current density is 50A/dm
2Situation under when testing, the work potential of relative saturation mercurous chloride electrode (SCE) is-1,225 millivolt.
D) scribble RuO the porous mesh screen with according to top described method
2/ TiO
280 millimeters disks forming of nickel foil (sheet), as the negative electrode in the electrolyzer of the electrolysis NaCl aqueous solution.Adopt thin film technique.
The condition of operation is:
Current density=30A/dm
2
Temperature=85 ℃
32%NaOH solution (by weight)
Find:
During the terminal voltage of the battery that constitutes with the nickelalloy negative electrode that does not have coating when the negative electrode that relatively contains coating, this terminal voltage that contains the coated cathode electrolyzer demonstrates 300 millivolts benefit,
And after moving six days continuously, benefit still is 300 millivolts of normal values.
Example 2
The surface-treated nickel substrate has been carried out in use under the condition of example 1.
Two solution of preparation in the time of 23 ℃:
A solution: 2 gram RuCl of example 1
2XHClyH
2O is dissolved in 2 liters of solution in the ethanol.
B solution: the TiOCl in 1 liter of ethanol
21.3 liters of the solution of 2HCl wherein contain 2.5 moles of Ti/ liters.
Coating/oven dry/heat treated order according to example 1, B solution is deposited two layers on the Ni substrate, then, after the cooling, with equally according to coating/oven dry/heat treated order two layers of A solution depositions, and then deposit two layers of B solution, and handle by same procedure the back, and metal oxide deposition total amount is 1.75 milligrams/centimetre
2, comprise 0.6 milligram/centimetre
2RuO
2
Having by TiO
2, RuO
2, TiO
2The negative electrode of the coating of three formations as example 1, is tested in NaOH; The relative SCE of its work potential is-1,240 millivolt.After 40 hours, this electromotive force is-1,210 millivolt.
Example 3
A) condition of use-case 1 has been carried out surface-treated Ni substrate.
B) two solution of preparation in the time of 23 ℃:
A solution: the 2 gram RuCl of dissolving in 2 liters of ethanol of example 1
3XHClyH
2O solution.
B solution: solution 1 gram ZrOCl in 2.4 liters of ethanol/1 liter 1NHCl
28H
2The solution of O.
C) coating/oven dry/heat treated order according to example 1 deposits two layers to B solution on substrate, and then, after the cooling, equally according to coating/oven dry/heat treated order two layers of A solution depositions, and then handle two layers of B solution depositions by same procedure.
D) total amount of metal oxide is 1.8 milligrams/centimetre
2, comprise 0.7 milligram/centimetre
2RuO
2
Having ZrO
2, RuO
2, ZrO
2The negative electrode of three coatings be placed among the NaOH as example 1 and test, its work potential is-1,210 millivolt with respect to SCE; After 16 hours, electromotive force is-1,200 millivolt.
Example 4
A) nickel substrate of use-case 3, A solution and B solution.
B) coating/oven dry/heat-treating methods and the condition of pressing example 1 deposits two layers of A solution on substrate, deposits two layers of B solution again.
C) metal oxide deposition total amount is 1.2 milligrams/centimetre
2, comprise 0.7 milligram/centimetre
2RuO
2
Having RuO
2/ ZrO
2The negative electrode of two coatings is being put among the NaOH as example 1 and is being tested.Its work potential is-1,210 millivolt with respect to SCE, and after-potential was constant in 16 hours.
Claims (13)
- The negative electrode that 1, can be used for electrolyzer, it is made of the conductive substrate of a coating, and this coating is the basis with platinum group metal oxide.This negative electrode is characterised in that: it has a coating that is made of the multiple layer metal oxide compound, its upper layer is made up of metal oxide semiconductor basically, the middle layer or at least one of middle layer basically by the element phase table the VIII family a metal oxide containing precious metals form.
- According to the negative electrode of claim 1, it is characterized in that 2, upper layer and/or a middle layer or a plurality of middle layer only are made up of above-mentioned metal oxide.
- 3, according to the negative electrode of claim 1, it is characterized in that, upper layer and/or middle layer or at least one of middle layer form by the mixed oxide of second metal of above-mentioned metal and small proportion.
- According to any one negative electrode in the claim 1 to 3, it is characterized in that 4, this coating is by one or more layers ruthenium oxide (RuO 2) with one or more layers titanium and/or zirconium white gang and forming.
- According to any one negative electrode of claim 1 to 4, it is characterized in that 5, this coating comprises, from substrate, one or more layers RuO 2, be one or more layers TiO then 2And/or ZrO 2, or a series of one or more layers TiO 2And/or ZrO 2/ one or more layers RuO 2/ one or more layers TiO 2And/or ZrO 2
- According to any one negative electrode of claim 1 to 5, it is characterized in that 6, some or all oxide compounds in the coating are the thin slice state.
- According to any one negative electrode of claim 1 to 6, it is characterized in that 7, substrate is to select from nickel, stainless steel and soft steel generic.
- 8, according to the manufacture method of any one negative electrode of claim 1 to 7, it is characterized in that,, then whole lamellar body is generated the thermal treatment of oxidised form through suitable deposition of giving the enterprising row metal salt deposit of substrate of processing.
- 9, making method according to Claim 8 progressively deposits to the solution layer or the suspension layers of metal-salt on the substrate.
- 10, according to the cathode production method of claim 3, it is characterized in that: mixed oxide is formed by these metallic salts, and it is that one or more layers form deposition by the same solution of above-mentioned salt forms.
- According to Claim 8 to 10 any one methods, it is characterized in that 11, these metal-salts are to choose from the inorganic or organic salt of these metals, for example, halogenide, nitrate, carbonate, vitriol or acetate or acetylacetonate.
- 12, according to Claim 8 to 11 any one method, it is characterized in that thermal treatment is to carry out under a temperature between 200 ℃ and 1000 ℃.
- According to the method for claim 12, it is characterized in that 13,, before thermal treatment, dry that be intended that partly or entirely to remove and desolvate and thinner, said bake out temperature can reach 200 ℃ from metal-salt.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8509540 | 1985-06-24 | ||
| FR8509540A FR2583781A1 (en) | 1985-06-24 | 1985-06-24 | CATHODE FOR ELECTROLYSIS AND METHOD FOR MANUFACTURING THE SAME CATHODE |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN86104356A true CN86104356A (en) | 1986-12-24 |
Family
ID=9320572
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN198686104356A Pending CN86104356A (en) | 1985-06-24 | 1986-06-24 | Be used for electrolytic negative electrode and preparation method thereof |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP0209427A1 (en) |
| JP (1) | JPS61295386A (en) |
| KR (1) | KR890003514B1 (en) |
| CN (1) | CN86104356A (en) |
| FR (1) | FR2583781A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103255434A (en) * | 2012-02-15 | 2013-08-21 | 旭化成化学株式会社 | Electrode for electrolysis, electrolytic cell, and method for manufacturing electrode for electrolysis |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1012970B (en) * | 1987-06-29 | 1991-06-26 | 耐用电极株式会社 | Cathode for electrolysis and process for producing same |
| FR2775486B1 (en) * | 1998-03-02 | 2000-04-07 | Atochem Elf Sa | SPECIFIC CATHODE FOR USE IN THE PREPARATION OF AN ALKALINE METAL CHLORATE AND METHOD FOR THE PRODUCTION THEREOF |
| FR2852973B1 (en) * | 2003-03-28 | 2006-05-26 | Atofina | PROCESS FOR FORMING A COATING OF METAL OXIDES ON AN ELECTROCONDUCTIVE SUBSTRATE; RESULTING ACTIVE CATHODE AND USE THEREOF FOR THE ELECTROLYSIS OF ACQUEUS SOLUTIONS OF ALKALINE COIL CHORIDES. |
| EP2085501A1 (en) * | 2008-01-31 | 2009-08-05 | Casale Chemicals S.A. | High performance cathodes for water electrolysers |
| ITMI20122030A1 (en) * | 2012-11-29 | 2014-05-30 | Industrie De Nora Spa | CATODO FOR ELECTROLYTIC EVOLUTION OF HYDROGEN |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3915838A (en) * | 1968-04-02 | 1975-10-28 | Ici Ltd | Electrodes for electrochemical processes |
| NL178429C (en) * | 1974-10-29 | 1986-03-17 | Diamond Shamrock Techn | METHOD OF MANUFACTURING AN ELECTRODE SUITABLE FOR USE IN ELECTROLYTIC PROCESSES |
| US4300992A (en) * | 1975-05-12 | 1981-11-17 | Hodogaya Chemical Co., Ltd. | Activated cathode |
| JPS5927391B2 (en) * | 1976-12-15 | 1984-07-05 | 三洋電機株式会社 | Water splitting device using light energy |
| GB2083837B (en) * | 1980-08-18 | 1984-06-27 | Diamond Shamrock Corp | Manufacture of electrode with manganese dioxide coating valve metal base intermediate semiconducting layer |
-
1985
- 1985-06-24 FR FR8509540A patent/FR2583781A1/en active Pending
-
1986
- 1986-06-17 EP EP86401327A patent/EP0209427A1/en not_active Ceased
- 1986-06-24 CN CN198686104356A patent/CN86104356A/en active Pending
- 1986-06-24 JP JP61148032A patent/JPS61295386A/en active Granted
- 1986-06-24 KR KR1019860005037A patent/KR890003514B1/en not_active IP Right Cessation
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103255434A (en) * | 2012-02-15 | 2013-08-21 | 旭化成化学株式会社 | Electrode for electrolysis, electrolytic cell, and method for manufacturing electrode for electrolysis |
Also Published As
| Publication number | Publication date |
|---|---|
| KR870000455A (en) | 1987-02-18 |
| KR890003514B1 (en) | 1989-09-23 |
| JPS61295386A (en) | 1986-12-26 |
| EP0209427A1 (en) | 1987-01-21 |
| JPS6328998B2 (en) | 1988-06-10 |
| FR2583781A1 (en) | 1986-12-26 |
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