CN108866610A - A kind of electrolytic anode - Google Patents
A kind of electrolytic anode Download PDFInfo
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- CN108866610A CN108866610A CN201810558389.XA CN201810558389A CN108866610A CN 108866610 A CN108866610 A CN 108866610A CN 201810558389 A CN201810558389 A CN 201810558389A CN 108866610 A CN108866610 A CN 108866610A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
A kind of electrolytic anode is formed in the multiple layer metal transition zone of described matrix any surface including matrix, by magnetron sputtering method and is formed in the catalyst layer of the multiple layer metal transition layer surface；Described matrix is valve metal or valve metal alloy, and the valve metal is selected from one of titanium, tantalum, niobium, zirconium, hafnium, vanadium, molybdenum and tungsten；The material of the intermediate metal is titanium, tantalum, niobium, zirconium, hafnium, vanadium, molybdenum or tungsten；The catalyst layer is element containing catalytic activity and the oxide skin(coating) for being catalyzed stable element, the catalytic activity element is selected from one of iridium, platinum, osmium, rhodium, palladium and ruthenium or a variety of, and the catalysis stable element is selected from one of titanium, tantalum, niobium, tungsten and zirconium or a variety of.The composition metal transition zone binding force being achieved in that is strong, thermal stability with higher, has good protective effect to matrix.In addition, target used in magnetron sputtering is monometallic, coating ratio and the inconsistent situation of target ratio are avoided relative to alloy target material.
Description
Technical field
The invention belongs to electrolysis electrode manufacturing fields, are related to a kind of anode, and in particular to a kind of electrolytic anode.
Background technique
It needs in copper foil production or during steel electroplating zinc, electrotinning to use Ni―Ti anode as oxygen evolution reaction electricity
Pole.Catalyst layer of the Ni―Ti anode usually by matrix and coated in matrix surface forms, and matrix generallys use valve-type metal titanium
Matter, catalyst layer are several microns of thick metal oxide containing precious metals (being mainly made of the mixture of yttrium oxide and tantalum oxide).
Every square metre is trained since the current density that Ni―Ti anode passes through in use reaches nearly Wan An, electrode surface is urged
Agent layer has often been not used, just between catalyst layer and Titanium base formed one layer insulation oxide skin(coating) or electrolyte into
Enter coat inside and substrate occurs corrosion reaction and forms gap, is obstructed so as to cause electric current output, oxygen evolution potential increases.Pass through increasing
This trend can effectively be slowed down by adding the mode of middle layer.Although titanium or/and tantalum pentoxide are common middle layers known in the art,
But under high current densities, remain difficult to get a desired effect；For another example Authorization Notice No. is CN 101550557B, CN
The Chinese invention patents such as 101550558B, which are disclosed, plates one layer of titanium tantalum alloy on matrix titanium surface using the mode of arc ion plating
Middle layer, and so that metal tantalum therein is formed oxidation state by heat-agglomerating.But since arc ions depositing process exists
Drop phenomenon, and be difficult to avoid, it be easy to cause the defect of middle layer；And target is titanium tantalum alloy, the ratio of coating often with
The ratio of target has deviation, and greatly, processing difficulties are expensive, and the recovery value of target is little for the two fusing point difference；Also there is packet
The mode for including plasma or electric-arc thermal spray coating forms tens microns thick of the middle layer containing tantalum or tantalum alloy, bright but there are coatings
Blocked up defect is shown, causes the waste of raw material, and its porosity is also higher (disclosed in JP 05-033177A etc.).
Summary of the invention
A kind of electrolytic anode is provided the invention aims to overcome the deficiencies in the prior art.
In order to solve the above technical problems, a kind of technical solution that the present invention takes is：A kind of electrolytic anode, it includes base
Body, the multiple layer metal transition zone that described matrix any surface is formed in by magnetron sputtering method and it is formed in the multiple layer metal
The catalyst layer of transition layer surface；Described matrix be valve metal or valve metal alloy, the valve metal be selected from titanium, tantalum, niobium,
One of zirconium, hafnium, vanadium, molybdenum and tungsten；The material of the intermediate metal is titanium, tantalum, niobium, zirconium, hafnium, vanadium, molybdenum or tungsten；It is described to urge
Agent layer be element containing catalytic activity and be catalyzed stable element oxide skin(coating), the catalytic activity element be selected from iridium, platinum,
One of osmium, rhodium, palladium and ruthenium are a variety of, and the catalysis stable element is selected from one of titanium, tantalum, niobium, tungsten and zirconium or more
Kind.
Optimally, the material of described matrix is Titanium.
Further, the catalyst layer is presoma of the coating containing the catalytic activity element and catalysis stable element
Solution is formed after dry through sintering.
Further, the material of the intermediate metal is tantalum or titanium, and the material of intermediate metal described in adjacent two layers
It is different；It is preferred that being adjacent to tantalum layer with matrix, titanium layer is adjacent to catalyst layer.
Optimally, the magnetron sputtering method is：Under conditions of argon gas, vacuum, the material with the intermediate metal is
Target carries out magnetron sputtering in described matrix any surface.The parameter of above-mentioned magnetron sputtering method is preferably：The magnetic control splashes
Target and the workpiece distance penetrated are 30~100mm, sputtering time is 1~40min, Dc source power is 100~500W and true
Reciprocal of duty cycle≤0.5Pa.Further, when carrying out magnetron sputtering, temperature≤500 DEG C of described matrix are controlled.Further, by institute
It states matrix to be cleaned, obtains roughness after sandblasting or/and etching after and be 3~12 μm of surface, then carry out magnetron sputtering.
Optimally, every layer of transition zone with a thickness of 0.1~5 μm.
Optimally, catalytic activity constituent content described in the catalyst layer is 5~50g/m2。
The invention has the beneficial effects that：Electrolytic anode of the present invention, by using magnetron sputtering method in catalyst layer and
Form the intermediate metal of multilayer monometallic composition between matrix, the material of the intermediate metal be titanium, tantalum, niobium, zirconium, hafnium, vanadium,
Molybdenum or tungsten, defect caused by the transition zone being achieved in that is fine and close and corrosion-resistant, dripless, binding force is strong, higher thermal stability
Can, to have good protective effect to matrix.In addition, target used in magnetron sputtering is monometallic, relative to alloys target
Material avoids coating ratio and the inconsistent situation of target ratio, and corresponding price is more competitive and recycling and reusing valence
Value.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of electrolytic anode in embodiment 1；
Fig. 2 is the section SEM figure of electrolytic anode in embodiment 3；
Fig. 3 is the section SEM figure in comparative example 1 after electrolytic anode failure.
Specific embodiment
Electrolytic anode of the present invention, it includes matrix, the multilayer for being formed in by magnetron sputtering method described matrix any surface
Intermediate metal and the catalyst layer for being formed in the multiple layer metal transition layer surface；Described matrix is valve metal or valve metal
Alloy, the valve metal are selected from one of titanium, tantalum, niobium, zirconium, hafnium, vanadium, molybdenum and tungsten；The material of the intermediate metal is
Titanium, tantalum, niobium, zirconium, hafnium, vanadium, molybdenum or tungsten；The catalyst layer is element containing catalytic activity and the oxide for being catalyzed stable element
Layer, the catalytic activity element are selected from one of iridium, platinum, osmium, rhodium, palladium and ruthenium or a variety of, and the catalysis stable element is
Selected from one of titanium, tantalum, niobium, tungsten and zirconium or a variety of.It is formed between catalyst layer and matrix by using magnetron sputtering method
The intermediate metal of multilayer monometallic composition, the material of the intermediate metal are titanium, tantalum, niobium, zirconium, hafnium, vanadium, molybdenum or tungsten, in this way
Defect caused by the transition zone of acquisition is fine and close and corrosion-resistant, dripless, binding force is strong, higher thermal stability, thus to base
Body has good protective effect.In addition, target used in magnetron sputtering is monometallic, coating is avoided relative to alloy target material
Ratio and the inconsistent situation of target ratio, and corresponding price is more competitive and recycling and reusing value.
The material of above-mentioned matrix is usually Titanium, has lower cost while meeting service performance.It is described to urge
Agent layer is usually to coat the precursor solution containing the catalytic activity element and catalysis stable element (it is molten to can be mixing
Liquid), it is formed after dry through sintering；Sintering temperature is usually 400~600 DEG C, sintering time is usually 10~30min；Finally urge
Catalytic activity constituent content is preferably 5~50g/m in agent layer2, generally for catalytic activity element in guarantee catalyst layer
Be uniformly distributed, final catalyst layer repeat it is above-mentioned coating, sintering process repeatedly (5~20 times) and obtain.Phase
The material of adjacent double layer of metal transition zone is different, and material is usually tantalum or titanium；It is further preferred that tantalum layer is adjacent to matrix, with catalysis
Oxidant layer is adjacent to titanium layer.The thickness of every layer of intermediate metal is preferably 0.1~5 μm.Above-mentioned magnetron sputtering method is：In argon gas, very
Under conditions of sky, magnetron sputtering is carried out in described matrix any surface using the material of the intermediate metal as target；Tool
Body parameter is preferably：Target and the workpiece distance of the magnetron sputtering are 30~100mm, sputtering time is 1~40min, direct current
Power is 100~500W and vacuum degree≤0.5Pa.Further, when carrying out magnetron sputtering, the temperature of described matrix is controlled
≤ 500 DEG C of degree.Further, described matrix is cleaned, obtaining roughness after sandblasting or/and etching after is 3~12 μ
The surface of m, then magnetron sputtering is carried out, to improve the bond strength of layer intermediate metal.
The preferred embodiment of the invention is described in detail below in conjunction with attached drawing：
Embodiment 1
The present embodiment provides a kind of electrolytic anodes, as shown in Figure 1, it includes matrix 1, catalyst layer 2, intermediate metal 3
With intermediate metal 3 '；Intermediate metal 3 is formed in the upper surface of matrix 1 by magnetron sputtering method, and intermediate metal 3 ' is logical
Cross the outer surface that magnetron sputtering method is formed in intermediate metal 3；Catalyst layer 2 is then formed on the surface of intermediate metal 3 '；
Its preparation process is specially：
Industrially pure titanium plate surface is cut into 35mm × 35mm × 1mm size, 10% grass of boiling after blasting treatment
The Titanium base that roughness Ra is 3~12 μm is obtained after acid solution soak acid-cleaning 1 hour；
Then Titanium base is placed in JGP045CA circle single chamber magnetic control sputtering system, control titanium-based temperature is 300 DEG C
Magnetron sputtering is carried out, parameter is：Working gas is commercially available high-purity argon gas, vacuum degree 0.3Pa, Dc source power are
200W, target-substrate distance 50mm；It is first sputtered 20 minutes using tantalum target, forms 2 μm of tantalum layer (i.e. intermediate metal 3)；Then adopt
With titanium target as sputter 2 minutes, the titanium layer (i.e. intermediate metal 3 ') of 100nm is formed；
Then coating the butanol solution of chloro-iridic acid and tantalic chloride on titanium layer surface, (concentration of chloro-iridic acid is 0.23mol/
L, Ir and Ta molar ratio are 65: 35), in 120 DEG C of drying half an hour, being subsequently placed in 500 DEG C of air electric furnaces and carry out heat treatment 20
Minute；It is so repeated 15 times, obtaining catalyst layer 2, (iridium content reaches 15g/m in catalyst layer 22)。
Embodiment 2
The present embodiment provides a kind of electrolytic anode, it with it is almost the same in embodiment 1, unlike：Intermediate metal
3 ' use titanium target as sputter 4 minutes, form the titanium layer of 200nm.
Embodiment 3
The present embodiment provides a kind of electrolytic anode, it with it is almost the same in embodiment 1, unlike：Intermediate metal
3 ' use titanium target as sputter 10 minutes, form the titanium layer of 500nm.Sample section stereoscan photograph such as Fig. 2.
Comparative example 1
The present embodiment provides a kind of electrolytic anode, in Titanium base processing method and catalyst layer and embodiment 1 basic one
It causes, unlike：Butanol solution 3 times containing butyl titanate and tantalic chloride are coated on 1 surface of matrix, it is thick to obtain 500nm
Oxide skin(coating) (concentration of butyl titanate is that the molar ratio of 0.1mol/L, Ti and Ta are 95: 5), after drying 500 DEG C be sintered
Form titanium tantalum pentoxide transition zone.
Comparative example 2
The present embodiment provides a kind of electrolytic anode, it with it is almost the same in embodiment 1, unlike：Intermediate metal
3 ' use titanium target as sputter 1 minute, form the titanium layer of 50nm.
Comparative example 3
The present embodiment provides a kind of electrolytic anode, it with it is almost the same in embodiment 1, unlike：Only with included a tantalum target
Material sputters 20 minutes, forms 2 μm of tantalum layer.
Comparative example 4
The present embodiment provides a kind of electrolytic anode, it with it is almost the same in embodiment 1, unlike：Only with titanium target
Material sputters 40 minutes, forms 2 μm of titanium layer.
Comparative example 5
The present embodiment provides a kind of electrolytic anode, it with it is almost the same in embodiment 1, formed using magnetron sputtering method
Layer is crossed, the difference is that the transition zone is that application reference number is used by example 1 in 200910133002.7 Chinese invention patent
The alloy-layer that titanium tantalum weight ratio is 60: 40 is obtained, with a thickness of 2 μm.
The electrolytic anode obtained in embodiment 1-3, comparative example 1-5 is subjected to accelerating lifetime testing respectively：In 60 DEG C, H25O4
Constant-current electrolysis (current density 30kA/m is carried out in aqueous solution (concentration 1.0mol/L)2), 1V is risen as the service life using voltage
Terminal, the result is shown in tables 1.
The accelerating lifetime testing table of electrolytic anode in 1 embodiment 1-3 of table, comparative example 1-5
From table 1 it follows that using this composition metal middle layer electrolytic anode accelerated aging duration considerably beyond
Traditional titanium tantalum pentoxide middle layer.Cross-section diagram in comparative example 1 after sample fails is as shown in figure 3, Titanium base has been corroded.
When (similarly in 50nm or less), the service life is lower, this is because metal mistake in 50nm for the thickness of titanium layer in intermediate metal
It is too thin intolerant to thermal oxide to cross layer.Therefore needing the layer of titanium metal of plating to reach certain thickness can guarantee that tantalum layer is not oxidized, together
When the oxide that can be formed in catalyst manufacturing process of titanium layer itself also there is good corrosion resistance.In comparative example 4
Titanium layer, which is easily corroded, is making the disadvantages of catalyst layer is then easily oxidized with tantalum pure in comparative example 3, thus is all unable to reach best
Protecting effect.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of electrolytic anode, it is characterised in that：It includes matrix, is formed in described matrix any surface by magnetron sputtering method
Multiple layer metal transition zone and be formed in the catalyst layer of the multiple layer metal transition layer surface；Described matrix be valve metal or
Valve metal alloy, the valve metal are selected from one of titanium, tantalum, niobium, zirconium, hafnium, vanadium, molybdenum and tungsten；The intermediate metal
Material is titanium, tantalum, niobium, zirconium, hafnium, vanadium, molybdenum or tungsten；The catalyst layer is element containing catalytic activity and the oxygen for being catalyzed stable element
Compound layer, the catalytic activity element are selected from one of iridium, platinum, osmium, rhodium, palladium and ruthenium or a variety of, the stable member of the catalysis
Element is selected from one of titanium, tantalum, niobium, tungsten and zirconium or a variety of.
2. electrolytic anode according to claim 1, it is characterised in that：The material of described matrix is Titanium.
3. electrolytic anode according to claim 1 or 2, it is characterised in that：The catalyst layer is that coating is urged containing described
Change active element and be catalyzed the precursor solution of stable element, is formed after dry through sintering.
4. electrolytic anode according to claim 1 or 2, it is characterised in that：The material of the intermediate metal be tantalum or titanium,
And the material of intermediate metal described in adjacent two layers is different.
5. electrolytic anode according to claim 1, which is characterized in that the magnetron sputtering method is：In argon gas, the item of vacuum
Under part, magnetron sputtering is carried out in described matrix any surface using the material of the intermediate metal as target.
6. electrolytic anode according to claim 5, it is characterised in that：Target and the workpiece distance of the magnetron sputtering are 30
~ 100mm, sputtering time are 1 ~ 40min, Dc source power is 100 ~ 500W and vacuum degree≤0.5Pa.
7. electrolytic anode according to claim 6, it is characterised in that：When carrying out magnetron sputtering, the temperature of described matrix is controlled
≤ 500 DEG C of degree.
8. electrolytic anode according to claim 5, it is characterised in that：Described matrix is cleaned, after through sandblasting or/
It is 3 ~ 12 μm of surface with roughness is obtained after etching, then carries out magnetron sputtering.
9. electrolytic anode according to claim 1, it is characterised in that：Every layer of transition zone with a thickness of 0.1 ~ 5 μm.
10. electrolytic anode according to claim 1, it is characterised in that：Catalytic activity element described in the catalyst layer
Content is 5 ~ 50g/m2。
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| CN108866610B (en) | 2023-08-15 |
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