CN102677092A - Preparation method of titanium anode - Google Patents
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Abstract
The invention discloses a preparation method of a titanium anode, wherein the preparation method is capable of improving electrochemical property of the anode. The preparation method comprises the following steps: at first, depositing a layer of inert porous oxide nano film on a metal Ti substrate, and then coating an active oxide (such as iridium dioxide and ruthenium dioxide) on the surface of the film through a hot decomposition method. The inert porous oxide nano film is obtained by depositing precursor aqueous solution such as SiO2, TiO2 or ZrO2 on the surface of a metal through an electro-deposition method. According to an inert porous oxide nano middle layer provided by the invention, the number of electrochemical active points on a subsequent active oxide coating is remarkably improved, and the electro-catalytic property of the titanium anode is improved. The middle layer of the titanium anode provided by the invention has the advantages of many types, low cost of the preparation method and simple process.
Description
Technical field
The present invention relates to the preparation method of anode material, relate in particular to a kind of titanium anodic preparation method.
Background technology
Anode material is the parts of most critical in the electrochemistry industry, this be because: anode material is the place of anodic reaction, from the saves energy requirement to catalytic anodic reaction high electrochemical activity is arranged, promptly to have low anode potential.Anodic reaction is that oxygen takes place or the electrochemical industry of analysing the chlorine reaction is in the great majority, and the former electroplates (zinc-plated, zinc-plated etc.) etc. like the smelting and the surface of steel plate protective of common water electrolysis, non-ferrous metal, and the latter then is common chlorine industry.For above-mentioned electrochemical industry, what mainly use is (to claim insoluble anode or dimensional stability anode again, DSA) at the noble metallic oxide anode that the Ti metal base surface applies at present.Analyse oxygen and analyse the metal oxide containing precious metals active component that the chlorine electrochemical industry generally uses and be respectively iridic oxide (IrO
2) and ruthenium dioxide (RuO
2).
The energy problem that modern society occurs requires electrolytic industry significantly to cut down the consumption of energy, and the improvement of antianode material is the key point that realizes above-mentioned requirements, and the Ti anode that promptly requires industry at present to use has higher electrochemical activity.For this reason, carried out research and development around the following aspects both at home and abroad: the improvement of (1) activating oxide layer: basic ideas are other constituent elements that in active coating, mix.The most successful example of this respect is to have developed IrO
2+ Ta
2O
5Composite oxide coating is the at present commercial main body composition of oxygen with DSA of analysing.(2) the last improvement of preparation method: the work that this respect is done comprises the solution chemistry (as adopting sol-gel technique etc.) of the heat decomposition temperature that improves oxide compound and heat treating regime, improvement presoma.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of simple, low-cost, have a titanium anodic preparation method of high electrochemical activity.
The objective of the invention is to realize through following technical scheme:
The titanium anodic is the preparation method comprise the steps:
1) the titanium matrix is after mechanical sandblast roughened; Put into 30～50 ℃ of following oil removing 10min of alkaline degreasing liquid, pickling 5～30min removes descaling in the ebullient oxalic acid aqueous solution again, uses tap water at last successively; After the washed with de-ionized water; Use hot blast drying fast, in loft drier, place 5～24h, for use;
2) precursor solution preparation: add 50～100mL absolute ethyl alcohol, 50～100mL water, 1～10mL precursor, HCl transfers pH to 2.0～6.0, stirs 2～48h under the room temperature, and is for use;
3) in three slot electrodes, add the precursor solution for preparing; As working electrode, Ag/AgCl is as reference electrode with the titanium matrix, and platinum is counter electrode; CONTROLLED POTENTIAL-0.5～-3.0V; Depositing time is 30s～2000s, with 40～150 ℃ of oven dry behind the deionized water rinsing, obtains inertia nano-oxide film;
4) in above-mentioned galvanic deposit inertia nano-oxide film surface-coated activating oxide coating, through pyrolysis technique,, and repeat repeatedly in 350-550 ℃ of baking down, decomposition, obtain the titanium anode.
Described inertia nano-oxide film is SiO
2, TiO
2Or ZrO
2Film.
The precursor of described indifferent oxide is: alkyl silicate, alkyl titanate or zirconic acid alkyl ester.
Described activating oxide layer is iridic oxide, ruthenium dioxide or its composite oxides.
The precursor of described activating oxide layer is the chloracid or the villaumite of iridium or ruthenium.
Described Novel Titanium anode is used for analysing oxygen or analysing the chlorine reaction of electrochemical industry.
The invention has the beneficial effects as follows: silica membrane has nano-porous structure, through after this film pre-treatment, significantly improves the vesicular structure and the electrochemical activity of the activating oxide coating of subsequent coated; In addition, adopt electro-deposition techniques can prepare roughness and the bigger silicon dioxide film of porousness, more obvious to the facilitation effect of titanium anode performance.
Description of drawings
Fig. 1 (a) is the IrO that directly applies on the titanium plate
2The surface topography of active coating shows that coating is very fine and close;
Fig. 1 (b) is earlier through electro-deposition techniques deposition one deck nanometer SiO on titanium plate surface
2Behind the film, apply IrO again
2The surface topography of active coating shows coarse, the porous of coating.
Fig. 2 is that the titanium anode is at 0.5 M H
2SO
4What record in the aqueous solution analyses the oxygen polarization curve.(1) is the IrO that directly applies on the titanium plate
2Anode (Ti/IrO
2); (2) be on titanium plate surface first galvanic deposit one deck SiO
2Behind the film, apply the IrO that obtains again
2Anode (Ti/SiO
2/ IrO
2).Show that combined electrode has the higher oxygen electrochemical activity of analysing.
Embodiment
The titanium anodic is the preparation method comprise the steps:
1) the titanium matrix is after mechanical sandblast roughened; Put into 30～50 ℃ of following oil removing 10min of alkaline degreasing liquid, pickling 5～30min removes descaling in the ebullient oxalic acid aqueous solution again, uses tap water at last successively; After the washed with de-ionized water; Use hot blast drying fast, in loft drier, place 5～24h, for use;
2) precursor solution preparation: add 50～100mL absolute ethyl alcohol, 50～100mL water, 1～10mL precursor, HCl transfers pH to 2.0～6.0, stirs 2～48h under the room temperature, and is for use;
3) in three slot electrodes, add the precursor solution for preparing; As working electrode, Ag/AgCl is as reference electrode with the titanium matrix, and platinum is counter electrode; CONTROLLED POTENTIAL-0.5～-3.0V; Depositing time is 30s～2000s, with 40～150 ℃ of oven dry behind the deionized water rinsing, obtains inertia nano-oxide film;
4) in above-mentioned galvanic deposit inertia nano-oxide film surface-coated activating oxide coating, through pyrolysis technique,, and repeat repeatedly in 350-550 ℃ of baking down, decomposition, obtain the titanium anode.
Described inertia nano-oxide film is SiO
2, TiO
2, ZrO
2, PbO
2, SnO
2, Co
2O
3, CuO or ZnO film.The precursor of described indifferent oxide is: alkyl silicate, alkyl titanate or zirconic acid alkyl ester.Described activating oxide layer is iridic oxide, ruthenium dioxide or its composite oxides.The precursor of described activating oxide layer is the chloracid or the villaumite of iridium or ruthenium.
Described titanium anode is used for analysing oxygen or analysing the chlorine reaction of electrochemical industry.
Because electro-deposition techniques has the requirement of degree of cleaning to specimen surface, therefore, at first requires titanium alloy (TA1) matrix surface is carried out the oil removing pre-treatment.
Titanium alloy substrate is put into 30 ℃ of following oil removing 10min of alkaline degreasing liquid after mechanical sandblast roughened, pickling 30 min remove descaling in the ebullient oxalic acid aqueous solution again; Use tap water at last successively; After the washed with de-ionized water, use hot blast drying fast, it is for use in loft drier, to place 24h.
In beaker, add 50 mL absolute ethyl alcohols, 50 mL water, 1 mL tetraethoxy (TEOS) successively, HCl transfers about pH to 3.0, and it is for use to stir 2 h under the room temperature.In three slot electrodes, add the precursor solution for preparing, as working electrode, Ag/AgCl is as reference electrode with TA1; Platinum is counter electrode, and CONTROLLED POTENTIAL is at-0.5 V, after deposition finishes; With 40 ℃ of oven dry behind the deionized water rinsing, through changing the nanometer SiO that depositing time obtains different thickness
2Film.In galvanic deposit SiO
2The TA1 external coating of nano-oxide film contains 0.2M H
2IrCl
6Ethanol/Virahol (volume ratio 1:1) solution, at 450 ℃ of following baking 10 min, repeat repeatedly, under uniform temp, toast 1 h for the last time, obtain active titanium anode.Coat number of times through adjustment, control final active IrO
2The adhesion amount of oxide skin is ~ 10 g/m
2
Conventional Ti/IrO
2Anode surface densification, smooth (seeing accompanying drawing 1a); And through galvanic deposit SiO
2The IrO that applies after the pre-treatment
2Coated anode (Ti/SiO
2/ IrO
2) but show coarse, porous pattern (seeing accompanying drawing 1b).
The titanium anodic is analysed oxygen activity and is adopted polarization curve to test, and used test solution is 0.5 M H
2SO
4The aqueous solution.The result shows that the existence in galvanic deposit silicon-dioxide middle layer has significantly improved titanium anodic electro catalytic activity (seeing accompanying drawing 2).For more intuitively explanation, listed SiO in the table 1 with the preparation of different electric depositing time
2Layer is analysed the oxygen electric current for the titanium anodic of pretreatment layer.
Table 1 is with the SiO of different electric depositing time preparation
2Layer is analysed oxygen electric current (getting the current value under 1.4 V) for the titanium anodic of pretreatment layer
| Electrodeposition time (s) | Analyse oxygen electric current (mA/cm 2） |
| 0 | 7.4 |
| 300 | 10.1 |
| 600 | 12.3 |
| 1000 | 13.9 |
| 1500 | 16.3 |
| 2000 | 14.2 |
In beaker, add 100 mL absolute ethyl alcohols, 100 mL water, 10 mL tetraethoxys (TEOS) successively, HCl transfers about pH to 3.0, and it is for use to stir 48 h under the room temperature.In three slot electrodes, add the precursor solution for preparing, as working electrode, Ag/AgCl is as reference electrode with TA1; Platinum is counter electrode, and CONTROLLED POTENTIAL is at-3.0 V, after deposition finishes; With 40 ℃ of oven dry behind the deionized water rinsing, through changing the nanometer SiO that depositing time obtains different thickness
2Film.In galvanic deposit SiO
2The TA1 external coating of nano-oxide film contains 0.2M H
2IrCl
6Ethanol/Virahol (volume ratio 1:1) solution, at 450 ℃ of following baking 10 min, repeat repeatedly, under uniform temp, toast 1 h for the last time, obtain active titanium anode.Coat number of times through adjustment, control final active IrO
2The adhesion amount of oxide skin is ~ 10 g/m
2
With embodiment 1, at 0.5 M H
2SO
4Adopt its electro catalytic activity of polarization curve test in the aqueous solution.For more intuitively explanation, listed SiO in the table 2 with the preparation of different electric depositing time
2Layer is analysed the oxygen electric current for the titanium anodic of pretreatment layer.
Table 2 is with the SiO of different electric depositing time preparation
2Layer is analysed oxygen electric current (getting the current value under 1.4 V) for the titanium anodic of pretreatment layer
| Electrodeposition time (s) | Analyse oxygen electric current (mA/cm 2） |
| 0 | 7.4 |
| 100 | 11.2 |
| 300 | 13.8 |
| 500 | 14.9 |
| 1000 | 16.8 |
| 1500 | 13.6 |
Embodiment 3
In beaker, add 50 mL absolute ethyl alcohols, 50 mL water, 3 mL tetraethoxys (TEOS) successively, HCl transfers about pH to 3.0, and it is for use to stir 24 h under the room temperature.In three slot electrodes, add the precursor solution for preparing, as working electrode, Ag/AgCl is as reference electrode with TA1; Platinum is counter electrode, and CONTROLLED POTENTIAL is at-2.0 V, after deposition finishes; With 40 ℃ of oven dry behind the deionized water rinsing, through changing the nanometer SiO that depositing time obtains different thickness
2Film.In galvanic deposit SiO
2The TA1 external coating of nano-oxide film contains 0.2 M H
2IrCl
6Ethanol/Virahol (volume ratio 1:1) solution, at 450 ℃ of following baking 10 min, repeat repeatedly, under uniform temp, toast 1 h for the last time, obtain active titanium anode.Coat number of times through adjustment, control final active IrO
2The adhesion amount of oxide skin is ~ 10 g/m
2
With embodiment 1, at 0.5 M H
2SO
4Adopt its electro catalytic activity of polarization curve test in the aqueous solution.For more intuitively explanation, listed SiO in the table 3 with the preparation of different electric depositing time
2Layer is analysed the oxygen electric current for the titanium anodic of pretreatment layer.
Table 3 is with the SiO of different electric depositing time preparation
2Layer is analysed oxygen electric current (getting the current value under 1.4 V) for the titanium anodic of pretreatment layer
| Electrodeposition time (s) | Analyse oxygen electric current (mA/cm 2） |
| 0 | 7.4 |
| 100 | 9.2 |
| 300 | 12.3 |
| 500 | 13.5 |
| 1000 | 15.7 |
| 1500 | 16.4 |
Embodiment 4
In beaker, add 50 mL absolute ethyl alcohols, 50 mL water, 1 mL tetraethoxy (TEOS) successively, HCl transfers about pH to 3.0, and it is for use to stir 2 h under the room temperature.In three slot electrodes, add the precursor solution for preparing, as working electrode, Ag/AgCl is as reference electrode with TA1; Platinum is counter electrode, and CONTROLLED POTENTIAL is at-2.0 V, after deposition finishes; With 40 ℃ of oven dry behind the deionized water rinsing, through changing the nanometer SiO that depositing time obtains different thickness
2Film.Change follow-up activating oxide layer, with IrO
2Change RuO into
2, used coats solution for containing 0.2M RuCl
3Ethanol/water (volume ratio 1:1) solution.Heat decomposition temperature is similar with embodiment 1 with the process of coating.
Table 4 has been listed the SiO with the preparation of different electric depositing time
2Layer is the Ti/RuO of pretreatment layer
2Anode is respectively at 0.5M H
2SO
4And the anodic current in the 1.0M NaCl solution.
Table 4 is with the SiO of different electric depositing time preparation
2Layer is analysed oxygen electric current (getting the current value under the 1.4V) for the titanium anodic of pretreatment layer
Embodiment 5
Practical implementation step and embodiment 1 are similar, with the inertia nano oxide layer by SiO
2Change ZrO into
2Corresponding Z rO
2The process for preparation of precursor be: 50mL absolute ethyl alcohol and deionized water and hydrochloric acid mixed solution are slowly added 50mL tetrabutyl zirconate (C while stirring
16H
36O
4Zr) with the mixed solution of absolute ethyl alcohol in, each mol ratio is a tetrabutyl zirconate in total solution: absolute ethyl alcohol: H
2O:HCl=1:1:15:0.3 regulates pH=3.0, stirs 30min, ultrasonic 15min.In three slot electrodes, add the precursor solution for preparing, as working electrode, Ag/AgCl is as reference electrode with TA1; Platinum is counter electrode, and CONTROLLED POTENTIAL is at-2.0V, after deposition finishes; With 40 ℃ of oven dry behind the deionized water rinsing, through changing the nanometer ZrO that depositing time obtains different thickness
2Film.。Subsequent thermal is decomposed coating IrO
2The process of active coating is identical with embodiment 1.Listed ZrO in the table 5 with the preparation of different electric depositing time
2Layer is that the titanium anode of pretreatment layer is at 0.5M H
2SO
4In analyse the oxygen electric current.
Table 5 is with the ZrO of different electric depositing time preparation
2Layer is analysed oxygen electric current (getting the current value under the 1.4V) for the titanium anodic of pretreatment layer
| Electrodeposition time (s) | Analyse oxygen electric current (mA/cm 2） |
| 0 | 7.4 |
| 100 | 11.2 |
| 300 | 12.9 |
| 500 | 14.5 |
| 1000 | 17.2 |
| 1500 | 16.7 |
The foregoing description is used for the present invention that explains, rather than limits the invention, and in the protection domain of spirit of the present invention and claim, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (6)
1. a titanium anodic preparation method is characterized in that comprising the steps:
1) the titanium matrix is after mechanical sandblast roughened; Put into 30～50 ℃ of following oil removing 10min of alkaline degreasing liquid, pickling 5～30min removes descaling in the ebullient oxalic acid aqueous solution again, uses tap water at last successively; After the washed with de-ionized water; Use hot blast drying fast, in loft drier, place 5～24h, for use;
2) precursor solution preparation: add 50～100mL absolute ethyl alcohol, 50～100mL water, 1～10mL precursor, HCl transfers pH to 2.0～6.0, stirs 2～48h under the room temperature, and is for use;
3) in three slot electrodes, add the precursor solution for preparing; As working electrode, Ag/AgCl is as reference electrode with the titanium matrix, and platinum is counter electrode; CONTROLLED POTENTIAL-0.5～-3.0V; Depositing time is 30s～2000s, with 40～150 ℃ of oven dry behind the deionized water rinsing, obtains inertia nano-oxide film;
4) in above-mentioned galvanic deposit inertia nano-oxide film surface-coated activating oxide coating, through pyrolysis technique,, and repeat repeatedly in 350～550 ℃ of bakings down, decomposition, obtain the titanium anode.
2. a kind of Novel Titanium anodic preparation method according to claim 1 is characterized in that described inertia nano-oxide film is SiO
2, TiO
2Or ZrO
2Film.
3. a kind of titanium anodic preparation method according to claim 1 is characterized in that described precursor is: alkyl silicate, alkyl titanate or zirconic acid alkyl ester.
4. a kind of titanium anodic preparation method according to claim 1 is characterized in that described activating oxide layer is iridic oxide, ruthenium dioxide or its composite oxides.
5. a kind of titanium anodic preparation method according to claim 1, the precursor that it is characterized in that described activating oxide layer is the chloracid or the villaumite of iridium or ruthenium.
6. the titanium anodic purposes of method preparation according to claim 1 is characterized in that being used for analysing oxygen or analysing the chlorine reaction of electrochemical industry.
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