CN106435638A - Titanium electrode material and preparation method thereof - Google Patents
Titanium electrode material and preparation method thereof Download PDFInfo
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- CN106435638A CN106435638A CN201610973816.1A CN201610973816A CN106435638A CN 106435638 A CN106435638 A CN 106435638A CN 201610973816 A CN201610973816 A CN 201610973816A CN 106435638 A CN106435638 A CN 106435638A
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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
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- C—CHEMISTRY; METALLURGY
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- 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
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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
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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Abstract
The invention discloses a titanium electrode material and a preparation method thereof. The titanium electrode material comprises a pipe-shaped matrix, a first coating and a second coating, wherein the first coating and the second coating sequentially cover the surface of the matrix; the matrix is porous titanium; the first coating is evenly divided into three parts along the surface of the matrix, and the three parts sequentially include an antimony trioxide layer, a ruthenium dioxide layer and a palladium oxide layer and are distributed in the axial direction of the matrix; and the second coating is an iridium dioxide layer. Because the matrix is made from a porous material, the component (antimony trioxide, ruthenium dioxide and palladium oxide) of the first coating can be evenly dispersed on the outer surface of the matrix and the inner surfaces of matrix holes, and the electrode material is made to have excellent catalysis activity and a good mass transfer effect. The second coating (iridium dioxide) is further brushed on the exterior of the first coating, the corrosion resistance of the electrode material is enhanced, the titanium electrode material can resist corrosion of acid, alkaline or salt, and therefore the service life is prolonged.
Description
Technical field
The present invention relates to a kind of electrode material is and in particular to a kind of titanium electrode material and preparation method thereof.Belong to electrochemistry
Field of material technology.
Background technology
Ti electrode has incomparably remarkable performance, and in many electrolytic industry fields, tool is widely used, with traditional graphite
Electrode, lead-containing alloy electrode are compared, and it has electric current density height, long working life, and corrosion resistance is strong, lightweight, high precision, base
Body can the lot of advantages such as Reusability.Particularly, Ti electrode can be used for chlorine industry, chloric acid salt industrial, hypochlorite industry and
Production of perchlorate etc., application is related to the industries such as chemical industry, metallurgy, water process, environmental protection, plating and electrolysis organic synthesiss.
Electrode is the core component of electrochemical apparatus, plays a part electric energy and is converted into chemical energy, the therefore quality of electrode
It is directly connected to the efficiency of electrochemical apparatus.How to be had very by the activity of structure and material improvement raising electrode and life-span
Important meaning.
Content of the invention
The purpose of the present invention is for overcoming above-mentioned the deficiencies in the prior art, providing a kind of titanium electrode material.
Present invention also offers a kind of preparation method of above-mentioned titanium electrode material.
For achieving the above object, the present invention adopts following technical proposals:
A kind of titanium electrode material, the matrix including tubulose and the first coating and the second coating that are sequentially coated on its surface,
Described matrix is POROUS TITANIUM, and described first coating is divided into three parts along matrix surface, is followed successively by antimony oxide layer, titanium dioxide
Layer of ruthenium and oxidation palladium layers, this three part is axially distributed along matrix, and described second coating is titanium dioxide iridium layer.
Preferably, the gross thickness of described first coating and second coating is 30~80 μm, and both thickness ratio is for 2~3:1.
Preferably, antimony oxide layer, ruthenium dioxide layer are identical with the thickness of oxidation palladium layers.
Preferably, the aperture of described POROUS TITANIUM is 30~100 μm, and porosity is 30~40%.
A kind of preparation method of above-mentioned titanium electrode material, including step:
(1) vacuum-sintering porous titanium tube, and surface preparation is carried out to porous titanium tube, except the oxidation of degreasing and surface
Film, forms the fresh matrix of pitted skin;
(2) antimony oxide, ruthenic oxide and Palladium monoxide masking liquid are prepared respectively, matrix surface is divided into three parts, successively
Brush three kinds of described masking liquids, 100~110 DEG C of dryings 2~3 hours, heat treatment 2~3 hours under the conditions of 300~400 DEG C, cooling
To room temperature, the antimony oxide of formation, ruthenic oxide and Palladium monoxide coating are axially distributed along matrix, and this is first coating;
(3) prepare iridium dioxide masking liquid, brush iridium dioxide masking liquid, 100~110 DEG C of dryings 2~3 on first coating surface
Hour, heat treatment 0.5~1 hour under the conditions of 450~550 DEG C, it is cooled to room temperature, forms iridium dioxide coating, this is the second painting
Layer;
Under the conditions of (4) 450~550 DEG C, heat treatment 0.5~1 hour, obtains final product.
Preferably, in step (1), the concrete grammar of surface preparation is:By the porous titanium tube of blasting treatment be placed in from
In sub- water be cleaned by ultrasonic 10~20 minutes, remove moisture after in 50~55 DEG C of acid solution pickling 5~10 minutes, finally go from
It is cleaned by ultrasonic 10~15 minutes in sub- water, be placed in vacuum drying oven and dry;Wherein, acid solution is to be respectively by mass fraction
37% and 98% concentrated hydrochloric acid and concentrated sulphuric acid are according to volume ratio 2:1 preparation obtains.
It is further preferred that the concrete grammar of described blasting treatment is:Nozzle of sand spraying machine pressure is 0.3~0.5MPa, adopts
With 70~90 mesh Al2O3Abrasive material, is sprayed with 60~80 °, and the distance away from POROUS TITANIUM pipe surface for the nozzle is 1~2cm, during process
Between be 5~10s.
Preferably, the masking liquid of step (2) is that antimony oxide, ruthenic oxide or Palladium monoxide are dispersed in organic solvent
And obtain, the mass ratio of antimony oxide, ruthenic oxide or Palladium monoxide and organic solvent is 1:10~30.
Preferably, the masking liquid of step (3) is dispersed in organic solvent for iridium dioxide and obtains, iridium dioxide with organic
The mass ratio of solvent is 1:10~30.
It is further preferred that the process for dispersing employed in step (2) and (3) is ultrasonic disperse 5~10 minutes, described have
Machine solvent is any one in n-butyl alcohol, isopropanol or ethanol.
Beneficial effects of the present invention:
The present invention, with porous titanium tube as matrix, brushes formation first coating and second coating successively on its surface, wherein, the
One coating is divided into three parts along matrix surface, is followed successively by antimony oxide layer, ruthenium dioxide layer and oxidation palladium layers, this three part
Axially it is distributed along matrix, second coating is titanium dioxide iridium layer.Because matrix is porous material, composition (three oxidations of first coating
Two antimony, ruthenic oxide and Palladium monoxide) may be uniformly dispersed in the outer surface of matrix and matrix internal surface of hole so that the electrode obtained
Material has excellent catalysis activity and good mass transfer effect.Second coating (titanium dioxide has also been brushed outside first coating
Iridium), enhance the corrosion resistance of electrode material, the corrosion of acid, alkali or salt can be kept out, thus improve service life.
Brief description
Fig. 1 is the cross section structure schematic diagram of the present invention;
Wherein, 1 is matrix, and 2 is antimony oxide layer, and 3 is ruthenium dioxide layer, and 4 is oxidation palladium layers, and 5 is titanium dioxide iridium layer.
Specific embodiment
The present invention will be further elaborated with reference to the accompanying drawings and examples it should explanation, and the description below is only
It is to explain the present invention, its content is not defined.
Embodiment 1:
As shown in figure 1, a kind of titanium electrode material of the present invention, matrix 1 including tubulose and be sequentially coated on its surface
First coating and second coating, matrix 1 is POROUS TITANIUM, and first coating is divided into three parts along matrix surface, is followed successively by three oxidations
Two antimony layers 2, ruthenium dioxide layer 3 and oxidation palladium layers 4, this three part is axially distributed along matrix, and second coating is titanium dioxide iridium layer 5.
Wherein, the gross thickness of first coating and second coating is 30 μm, and both thickness ratio is for 2:1.Antimony oxide layer 2, ruthenic oxide
Layer 3 is identical with the thickness of oxidation palladium layers 4.The aperture of POROUS TITANIUM is 30 μm, and porosity is 30%.
A kind of preparation method of above-mentioned titanium electrode material, including step:
(1) vacuum-sintering porous titanium tube, and surface preparation is carried out to porous titanium tube, except the oxidation of degreasing and surface
Film, forms the fresh matrix of pitted skin;
(2) antimony oxide, ruthenic oxide and Palladium monoxide masking liquid are prepared respectively, matrix surface is divided into three parts, successively
Brush three kinds of described masking liquids, 100 DEG C of dryings 2 hours, heat treatment 2 hours under the conditions of 300 DEG C, it is cooled to room temperature, the three of formation
Aoxidize two antimony, ruthenic oxide and Palladium monoxide coating to be axially distributed along matrix, this is first coating;
(3) prepare iridium dioxide masking liquid, brush iridium dioxide masking liquid on first coating surface, 100 DEG C of dryings 2 hours, 450
Heat treatment 0.5 hour under the conditions of DEG C, is cooled to room temperature, forms iridium dioxide coating, and this is second coating;
Under the conditions of (4) 450 DEG C, heat treatment 0.5 hour, obtains final product.
Wherein, in step (1), the concrete grammar of surface preparation is:The porous titanium tube of blasting treatment is placed in deionization
In water be cleaned by ultrasonic 10 minutes, remove moisture after in 50 DEG C of acid solution pickling 5 minutes, be finally cleaned by ultrasonic in deionized water
10 minutes, it is placed in vacuum drying oven and dries;Wherein, acid solution be by mass fraction be respectively 37% and 98% concentrated hydrochloric acid and
Concentrated sulphuric acid is according to volume ratio 2:1 preparation obtains.The concrete grammar of blasting treatment is:Nozzle of sand spraying machine pressure is 0.3MPa, adopts
70 mesh Al2O3Abrasive material, is sprayed with 60 °, and the distance away from POROUS TITANIUM pipe surface for the nozzle is 1cm, and process time is 5s.
The masking liquid of step (2) is antimony oxide, ruthenic oxide or Palladium monoxide are dispersed in organic solvent and obtain, three
Aoxidizing two antimony, ruthenic oxide or Palladium monoxide and the mass ratio of organic solvent is 1:10.
The masking liquid of step (3) is dispersed in organic solvent for iridium dioxide and obtains, iridium dioxide and organic solvent
Mass ratio is 1:10.
Process for dispersing employed in step (2) and (3) is ultrasonic disperse 5 minutes, and organic solvent is n-butyl alcohol.
Embodiment 2:
As shown in figure 1, a kind of titanium electrode material of the present invention, matrix 1 including tubulose and be sequentially coated on its surface
First coating and second coating, matrix 1 is POROUS TITANIUM, and first coating is divided into three parts along matrix surface, is followed successively by three oxidations
Two antimony layers 2, ruthenium dioxide layer 3 and oxidation palladium layers 4, this three part is axially distributed along matrix, and second coating is titanium dioxide iridium layer 5.
Wherein, the gross thickness of first coating and second coating is 80 μm, and both thickness ratio is for 3:1.Antimony oxide layer 2, ruthenic oxide
Layer 3 is identical with the thickness of oxidation palladium layers 4.The aperture of POROUS TITANIUM is 100 μm, and porosity is 40%.
A kind of preparation method of above-mentioned titanium electrode material, including step:
(1) vacuum-sintering porous titanium tube, and surface preparation is carried out to porous titanium tube, except the oxidation of degreasing and surface
Film, forms the fresh matrix of pitted skin;
(2) antimony oxide, ruthenic oxide and Palladium monoxide masking liquid are prepared respectively, matrix surface is divided into three parts, successively
Brush three kinds of described masking liquids, 110 DEG C of dryings 3 hours, heat treatment 3 hours under the conditions of 400 DEG C, it is cooled to room temperature, the three of formation
Aoxidize two antimony, ruthenic oxide and Palladium monoxide coating to be axially distributed along matrix, this is first coating;
(3) prepare iridium dioxide masking liquid, brush iridium dioxide masking liquid on first coating surface, 110 DEG C of dryings 3 hours, 550
Heat treatment 1 hour under the conditions of DEG C, is cooled to room temperature, forms iridium dioxide coating, and this is second coating;
Under the conditions of (4) 550 DEG C, heat treatment 1 hour, obtains final product.
Wherein, in step (1), the concrete grammar of surface preparation is:The porous titanium tube of blasting treatment is placed in deionization
It is cleaned by ultrasonic 20 minutes in water, remove after moisture pickling 10 minutes in 55 DEG C of acid solution, finally ultrasonic clear in deionized water
Wash 15 minutes, be placed in vacuum drying oven and dry;Wherein, acid solution is by the concentrated hydrochloric acid of mass fraction respectively 37% and 98%
With concentrated sulphuric acid according to volume ratio 2:1 preparation obtains.The concrete grammar of blasting treatment is:Nozzle of sand spraying machine pressure is 0.5MPa, adopts
With 90 mesh Al2O3Abrasive material, is sprayed with 80 °, and the distance away from POROUS TITANIUM pipe surface for the nozzle is 2cm, and process time is 10s.
The masking liquid of step (2) is antimony oxide, ruthenic oxide or Palladium monoxide are dispersed in organic solvent and obtain, three
Aoxidizing two antimony, ruthenic oxide or Palladium monoxide and the mass ratio of organic solvent is 1:30.
The masking liquid of step (3) is dispersed in organic solvent for iridium dioxide and obtains, iridium dioxide and organic solvent
Mass ratio is 1:30.
Process for dispersing employed in step (2) and (3) is ultrasonic disperse 10 minutes, and organic solvent is isopropanol.
Embodiment 3:
As shown in figure 1, a kind of titanium electrode material of the present invention, matrix 1 including tubulose and be sequentially coated on its surface
First coating and second coating, matrix 1 is POROUS TITANIUM, and first coating is divided into three parts along matrix surface, is followed successively by three oxidations
Two antimony layers 2, ruthenium dioxide layer 3 and oxidation palladium layers 4, this three part is axially distributed along matrix, and second coating is titanium dioxide iridium layer 5.
Wherein, the gross thickness of first coating and second coating is 30 μm, and both thickness ratio is for 3:1.Antimony oxide layer 2, ruthenic oxide
Layer 3 is identical with the thickness of oxidation palladium layers 4.The aperture of POROUS TITANIUM is 30 μm, and porosity is 40%.
A kind of preparation method of above-mentioned titanium electrode material, including step:
(1) vacuum-sintering porous titanium tube, and surface preparation is carried out to porous titanium tube, except the oxidation of degreasing and surface
Film, forms the fresh matrix of pitted skin;
(2) antimony oxide, ruthenic oxide and Palladium monoxide masking liquid are prepared respectively, matrix surface is divided into three parts, successively
Brush three kinds of described masking liquids, 100 DEG C of dryings 3 hours, heat treatment 3 hours under the conditions of 300 DEG C, it is cooled to room temperature, the three of formation
Aoxidize two antimony, ruthenic oxide and Palladium monoxide coating to be axially distributed along matrix, this is first coating;
(3) prepare iridium dioxide masking liquid, brush iridium dioxide masking liquid on first coating surface, 100 DEG C of dryings 3 hours, 450
Heat treatment 1 hour under the conditions of DEG C, is cooled to room temperature, forms iridium dioxide coating, and this is second coating;
Under the conditions of (4) 450 DEG C, heat treatment 1 hour, obtains final product.
Wherein, in step (1), the concrete grammar of surface preparation is:The porous titanium tube of blasting treatment is placed in deionization
In water be cleaned by ultrasonic 10 minutes, remove moisture after in 55 DEG C of acid solution pickling 5 minutes, be finally cleaned by ultrasonic in deionized water
15 minutes, it is placed in vacuum drying oven and dries;Wherein, acid solution be by mass fraction be respectively 37% and 98% concentrated hydrochloric acid and
Concentrated sulphuric acid is according to volume ratio 2:1 preparation obtains.The concrete grammar of blasting treatment is:Nozzle of sand spraying machine pressure is 0.3MPa, adopts
90 mesh Al2O3Abrasive material, is sprayed with 60 °, and the distance away from POROUS TITANIUM pipe surface for the nozzle is 2cm, and process time is 5s.
The masking liquid of step (2) is antimony oxide, ruthenic oxide or Palladium monoxide are dispersed in organic solvent and obtain, three
Aoxidizing two antimony, ruthenic oxide or Palladium monoxide and the mass ratio of organic solvent is 1:30.
The masking liquid of step (3) is dispersed in organic solvent for iridium dioxide and obtains, iridium dioxide and organic solvent
Mass ratio is 1:10.
Process for dispersing employed in step (2) and (3) is ultrasonic disperse 10 minutes, and organic solvent is ethanol.
Embodiment 4:
As shown in figure 1, a kind of titanium electrode material of the present invention, matrix 1 including tubulose and be sequentially coated on its surface
First coating and second coating, matrix 1 is POROUS TITANIUM, and first coating is divided into three parts along matrix surface, is followed successively by three oxidations
Two antimony layers 2, ruthenium dioxide layer 3 and oxidation palladium layers 4, this three part is axially distributed along matrix, and second coating is titanium dioxide iridium layer 5.
Wherein, the gross thickness of first coating and second coating is 80 μm, and both thickness ratio is for 2:1.Antimony oxide layer 2, ruthenic oxide
Layer 3 is identical with the thickness of oxidation palladium layers 4.The aperture of POROUS TITANIUM is 100 μm, and porosity is 30%.
A kind of preparation method of above-mentioned titanium electrode material, including step:
(1) vacuum-sintering porous titanium tube, and surface preparation is carried out to porous titanium tube, except the oxidation of degreasing and surface
Film, forms the fresh matrix of pitted skin;
(2) antimony oxide, ruthenic oxide and Palladium monoxide masking liquid are prepared respectively, matrix surface is divided into three parts, successively
Brush three kinds of described masking liquids, 110 DEG C of dryings 2 hours, heat treatment 2 hours under the conditions of 400 DEG C, it is cooled to room temperature, the three of formation
Aoxidize two antimony, ruthenic oxide and Palladium monoxide coating to be axially distributed along matrix, this is first coating;
(3) prepare iridium dioxide masking liquid, brush iridium dioxide masking liquid on first coating surface, 110 DEG C of dryings 2 hours, 550
Heat treatment 0.5 hour under the conditions of DEG C, is cooled to room temperature, forms iridium dioxide coating, and this is second coating;
Under the conditions of (4) 550 DEG C, heat treatment 0.5 hour, obtains final product.
Wherein, in step (1), the concrete grammar of surface preparation is:The porous titanium tube of blasting treatment is placed in deionization
It is cleaned by ultrasonic 20 minutes in water, remove after moisture pickling 10 minutes in 50 DEG C of acid solution, finally ultrasonic clear in deionized water
Wash 10 minutes, be placed in vacuum drying oven and dry;Wherein, acid solution is by the concentrated hydrochloric acid of mass fraction respectively 37% and 98%
With concentrated sulphuric acid according to volume ratio 2:1 preparation obtains.The concrete grammar of blasting treatment is:Nozzle of sand spraying machine pressure is 0.5MPa, adopts
With 70 mesh Al2O3Abrasive material, is sprayed with 80 °, and the distance away from POROUS TITANIUM pipe surface for the nozzle is 1cm, and process time is 10s.
The masking liquid of step (2) is antimony oxide, ruthenic oxide or Palladium monoxide are dispersed in organic solvent and obtain, three
Aoxidizing two antimony, ruthenic oxide or Palladium monoxide and the mass ratio of organic solvent is 1:10.
The masking liquid of step (3) is dispersed in organic solvent for iridium dioxide and obtains, iridium dioxide and organic solvent
Mass ratio is 1:30.
Process for dispersing employed in step (2) and (3) is ultrasonic disperse 5 minutes, and organic solvent is n-butyl alcohol, isopropanol
Or any one in ethanol.
Embodiment 5:
As shown in figure 1, a kind of titanium electrode material of the present invention, matrix 1 including tubulose and be sequentially coated on its surface
First coating and second coating, matrix 1 is POROUS TITANIUM, and first coating is divided into three parts along matrix surface, is followed successively by three oxidations
Two antimony layers 2, ruthenium dioxide layer 3 and oxidation palladium layers 4, this three part is axially distributed along matrix, and second coating is titanium dioxide iridium layer 5.
Wherein, the gross thickness of first coating and second coating is 50 μm, and both thickness ratio is for 2.5:1.Antimony oxide layer 2, titanium dioxide
Layer of ruthenium 3 is identical with the thickness of oxidation palladium layers 4.The aperture of POROUS TITANIUM is 70 μm, and porosity is 35%.
A kind of preparation method of above-mentioned titanium electrode material, including step:
(1) vacuum-sintering porous titanium tube, and surface preparation is carried out to porous titanium tube, except the oxidation of degreasing and surface
Film, forms the fresh matrix of pitted skin;
(2) antimony oxide, ruthenic oxide and Palladium monoxide masking liquid are prepared respectively, matrix surface is divided into three parts, successively
Brush three kinds of described masking liquids, 105 DEG C of dryings 2.5 hours, heat treatment 2.5 hours under the conditions of 350 DEG C, it is cooled to room temperature, formed
Antimony oxide, ruthenic oxide and Palladium monoxide coating be axially distributed along matrix, this is first coating;
(3) prepare iridium dioxide masking liquid, brush iridium dioxide masking liquid on first coating surface, 105 DEG C of dryings 2.5 hours,
Heat treatment 0.8 hour under the conditions of 500 DEG C, is cooled to room temperature, forms iridium dioxide coating, and this is second coating;
Under the conditions of (4) 500 DEG C, heat treatment 1 hour, obtains final product.
Wherein, in step (1), the concrete grammar of surface preparation is:The porous titanium tube of blasting treatment is placed in deionization
In water be cleaned by ultrasonic 15 minutes, remove moisture after in 50 DEG C of acid solution pickling 8 minutes, be finally cleaned by ultrasonic in deionized water
12 minutes, it is placed in vacuum drying oven and dries;Wherein, acid solution be by mass fraction be respectively 37% and 98% concentrated hydrochloric acid and
Concentrated sulphuric acid is according to volume ratio 2:1 preparation obtains.The concrete grammar of blasting treatment is:Nozzle of sand spraying machine pressure is 0.4MPa, adopts
80 mesh Al2O3Abrasive material, is sprayed with 70 °, and the distance away from POROUS TITANIUM pipe surface for the nozzle is 1.5cm, and process time is 8s.
The masking liquid of step (2) is antimony oxide, ruthenic oxide or Palladium monoxide are dispersed in organic solvent and obtain, three
Aoxidizing two antimony, ruthenic oxide or Palladium monoxide and the mass ratio of organic solvent is 1:20.
The masking liquid of step (3) is dispersed in organic solvent for iridium dioxide and obtains, iridium dioxide and organic solvent
Mass ratio is 1:20.
Process for dispersing employed in step (2) and (3) is ultrasonic disperse 8 minutes, and organic solvent is isopropanol.
Although the above-mentioned accompanying drawing that combines is described to the specific embodiment of the present invention, not model is protected to the present invention
The restriction enclosed, on the basis of technical scheme, those skilled in the art do not need to pay creative work and can do
The various modifications going out or deformation are still within protection scope of the present invention.
Claims (10)
1. a kind of titanium electrode material it is characterised in that include tubulose matrix and be sequentially coated on its surface first coating and
Second coating, described matrix is POROUS TITANIUM, and described first coating is divided into three parts along matrix surface, is followed successively by antimony oxide
Layer, ruthenium dioxide layer and oxidation palladium layers, this three part is axially distributed along matrix, and described second coating is titanium dioxide iridium layer.
2. a kind of titanium electrode material according to claim 1 it is characterised in that described first coating and second coating total
Thickness is 30~80 μm, and both thickness ratio is for 2~3:1.
3. a kind of titanium electrode material according to claim 1 it is characterised in that antimony oxide layer, ruthenium dioxide layer and
The thickness of oxidation palladium layers is identical.
4. a kind of titanium electrode material according to claim 1 is it is characterised in that the aperture of described POROUS TITANIUM is 30~100 μ
M, porosity is 30~40%.
5. a kind of preparation method of the titanium electrode material any one of Claims 1 to 4 is it is characterised in that include step:
(1) vacuum-sintering porous titanium tube, and surface preparation is carried out to porous titanium tube, except the oxide-film of degreasing and surface,
Form the fresh matrix of pitted skin;
(2) antimony oxide, ruthenic oxide and Palladium monoxide masking liquid are prepared respectively, matrix surface is divided into three parts, brushes successively
Three kinds of described masking liquids, 100~110 DEG C of dryings 2~3 hours, under the conditions of 300~400 DEG C, heat treatment 2~3 hours, are cooled to room
Temperature, the antimony oxide of formation, ruthenic oxide and Palladium monoxide coating are axially distributed along matrix, and this is first coating;
(3) prepare iridium dioxide masking liquid, brush iridium dioxide masking liquid on first coating surface, 100~110 DEG C of dryings 2~3 are little
When, heat treatment 0.5~1 hour under the conditions of 450~550 DEG C, it is cooled to room temperature, forms iridium dioxide coating, this is second coating;
Under the conditions of (4) 450~550 DEG C, heat treatment 0.5~1 hour, obtains final product.
6. preparation method according to claim 5 is it is characterised in that in step (1), the concrete grammar of surface preparation
It is:The porous titanium tube of blasting treatment is placed in deionized water and is cleaned by ultrasonic 10~20 minutes, at 50~55 DEG C after removing moisture
Acid solution in pickling 5~10 minutes, be finally cleaned by ultrasonic 10~15 minutes in deionized water, be placed in dry in vacuum drying oven and be
Can;Wherein, acid solution be by mass fraction be respectively 37% and 98% concentrated hydrochloric acid and concentrated sulphuric acid according to volume ratio 2:1 prepares
Arrive.
7. preparation method according to claim 6 is it is characterised in that the concrete grammar of described blasting treatment is:Sandblasting machine
Nozzle exit pressure is 0.3~0.5MPa, using 70~90 mesh Al2O3Abrasive material, is sprayed with 60~80 °, and nozzle is away from porous titanium tube table
The distance in face is 1~2cm, and process time is 5~10s.
8. preparation method according to claim 5 is it is characterised in that the masking liquid of step (2) is antimony oxide, titanium dioxide
Ruthenium or Palladium monoxide are dispersed in organic solvent and obtain, the matter of antimony oxide, ruthenic oxide or Palladium monoxide and organic solvent
Amount ratio is 1:10~30.
9. preparation method according to claim 5 is it is characterised in that the masking liquid of step (3) is that iridium dioxide is dispersed
Obtain in organic solvent, iridium dioxide is 1 with the mass ratio of organic solvent:10~30.
10. preparation method according to claim 8 or claim 9 is it is characterised in that dispersion side employed in step (2) and (3)
Method is ultrasonic disperse 5~10 minutes, and described organic solvent is any one in n-butyl alcohol, isopropanol or ethanol.
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CN110438527A (en) * | 2019-08-05 | 2019-11-12 | 上海氯碱化工股份有限公司 | The preparation method of the transient metal doped anode containing ruthenium coating |
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