CN106435638A - Titanium electrode material and preparation method thereof - Google Patents

Titanium electrode material and preparation method thereof Download PDF

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Publication number
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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coating
matrix
electrode material
preparation
titanium
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修志浩
王晓东
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Nanchang Special Technology Co Ltd
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051Electrodes formed of electrocatalysts on a substrate or carrier
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075Electrodes 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

A kind of titanium electrode material and preparation method thereof
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.
CN201610973816.1A 2016-11-07 2016-11-07 Titanium electrode material and preparation method thereof Pending CN106435638A (en)

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Cited By (1)

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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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