CN107699912A - A kind of coating solution of coated electrode and its preparation method of coated electrode - Google Patents
A kind of coating solution of coated electrode and its preparation method of coated electrode Download PDFInfo
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- CN107699912A CN107699912A CN201710779774.2A CN201710779774A CN107699912A CN 107699912 A CN107699912 A CN 107699912A CN 201710779774 A CN201710779774 A CN 201710779774A CN 107699912 A CN107699912 A CN 107699912A
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Abstract
A kind of coating solution of coated electrode and its preparation method of coated electrode, the coating solution by chloro-iridic acid, tantalic chloride and alpha-hydroxy acid volume ratio 1:1 ethylene glycol and butanol solution, the concentration of chloro-iridic acid are 30 ~ 38g/L, chloro-iridic acid:Tantalic chloride:The percent mass ratio of alpha-hydroxy acid is 55 ~ 62:34~40:3~7.The preparation method of the coated electrode is that titanium plate is put into sodium carbonate liquor to boil, then is rinsed well with deionized water, drying；Place into oxalic acid solution to boil, taking-up is rinsed well, drying；Coating solution is brushed in titanium plate with hairbrush, drying, aoxidized then at hot-air, after cooling, said process is repeated, after heat treatment, is cooled to normal temperature, coated electrode is made.The coating surface of coated electrode prepared by coating solution of the present invention and preparation method thereof is without obvious crack, and plane area area is big and smooth, and grain particles are largely grown in plane area, and coating combines densification, and reinforcing life substantially increases, and performance significantly improves.
Description
Technical field
The invention belongs to electrochemical technology field.It is related to the coating solution of coated electrode and its preparation side of coated electrode
Method.More particularly to the preparation method of iridium tantalum coated titanium electrode coating solution and its coated electrode.
Background technology
Using oxygen evolution reaction as in the electrochemical system of main reaction, IrO2-Ta2O5Coated titanium electrode is obtained extensively with premium properties
General application, IrO2As conductive constituent, Ta2O5As non-conductive oxide, electroconductive oxide structure can be made more stable.
CN1995464A provides a kind of nanocrystalline iridium series oxide coating electrode preparation method, by the crystallization for refining coating
Particle size is to nanoscale to improve the stability of electrode and electrocatalysis characteristic.IrO prepared by the invention2-Ta2O5-MO2Apply
Layer Titanium base electrode uses IrO2-Ta2O5-MO2Coating solution, Ir during it is formed:Ta mol ratios are 7:6, M Sn, Mn, Ti,
Nb, Pb and Si, H2IrCl6And TaCl5Account for the amount 30 ~ 95% of total material.By selecting suitable substrate pretreated coating composition ratio
The conditions such as example, sintering temperature, sintering time, the stability and electrocatalysis characteristic of electrode are played a major role in the electrode of preparation
IrO2Average grain size is in 8 ~ 15nm.The metal chlorides such as iridium, tantalum, tin, manganese, titanium obtain metal by high-temperature thermal oxidation and aoxidized
Thing, therefore in thermal oxidation process, metallic crystal particle inevitably grows reunion, the growth reunion of crystal particles causes
There are a large amount of crackles in face coat skewness, the short texture of Ti electrode, coating surface.When coated titanium electrode is using
When, the gas that separates out on anode is corroded by crackle arrive Titanium base surface, makes the failure of Titanium base surface oxidation, has a strong impact on coating
The electrochemical catalysis performance and used life of Ti electrode.
The content of the invention
The defects of for prior art, the purpose of the present invention is to propose to one kind in thermal oxidation process, metal can be suppressed
Crystal particles fast-growth is reunited, and the coating that iridium tantalum coated titanium electrode of the crystal grain small structure densification without obvious crackle is made is molten
Liquid.
Another object of the present invention is to propose that a kind of coating solution using the iridium tantalum coated titanium electrode prepares coating
The method of electrode.
The coating solution of the iridium tantalum coated titanium electrode of the present invention is chloro-iridic acid (H2IrCl6), tantalic chloride (TaCl5) and α-
The volume ratio 1 of carboxylic acid:1 ethylene glycol and butanol solution, the concentration of chloro-iridic acid is 30 ~ 38g/L.
The chloro-iridic acid:Tantalic chloride:The percent mass ratio of 'alpha '-hydroxy acids is 55 ~ 62:34~40:3~7.
Preferable chloro-iridic acid:Tantalic chloride:The percent mass ratio of 'alpha '-hydroxy acids is 60:36:4.
The 'alpha '-hydroxy acids are citric acid, tartaric acid, malic acid or lactic acid.
The preparation method of coated electrode of the present invention：Titanium plate is put into 3 ~ 8% sodium carbonate liquors, boiled 20 ~ 40 minutes,
Rinsed well, dried with deionized water again；Place into the oxalic acid solution that concentration is 5 ~ 6% to boil 50 ~ 70 minutes, take out to rinse and do
Only, dry；Coating solution is brushed in titanium plate with hairbrush, in 120 ~ 140 DEG C of drying, aoxidized then at 470 ~ 510 DEG C of hot-airs
10 ~ 20min, after cooling, repeat said process 14 ~ 20 times, last 470 ~ 510 DEG C, after being heat-treated 1 ~ 2h, be cooled to normal temperature, make
Obtain coated electrode.
Under the high temperature conditions prepared by thermal oxide decomposition method using metal chloride for coated titanium electrode, IrO in electrode2It is flat
Equal crystallite dimension plays a major role to the stability and electrocatalysis characteristic of electrode.Oxidate temperature is too low, the chloride of metal iridium
Oxidation is incomplete, cannot get required electrocatalysis characteristic, oxidate temperature rise, chlorinty in coating can on the one hand dropped
To very low, on the other hand, metallic crystal particle inevitably grows reunion, and the growth reunion of crystal particles causes Ti electrode
Face coat skewness, loose, adhesion decline, there are a large amount of crackles in coating surface.Have a strong impact on coated titanium electrode
Electrochemical catalysis performance and used life.Metallic crystal particle can be made scattered and suspendability because 'alpha '-hydroxy acids have,
In thermal oxidation process, the reunion of metallic crystal particle fast-growth can be suppressed, therefore, in the coating solution of iridium tantalum coated titanium electrode
Middle addition 'alpha '-hydroxy acids, such as tartaric acid, lactic acid, malic acid, citric acid, ensureing the fully oxidized height of the chloride of metal iridium
Under the conditions of temperature, the fine and close coated titanium electrode of crystal grain small structure is made.
Titanium plate is put into 3 ~ 8% sodium carbonate liquors, boiled 20 ~ 40 minutes, both the oil being infected with Titanium base process
Dirt is removed, and saves sodium carbonate amount again.Place into the oxalic acid solution that concentration is 5 ~ 6% to boil 50 ~ 70 minutes, on Titanium base surface
Dark grey titantium hydride needed for being formed, as concentration of oxalic acid is too high or boiling time is oversize, both waste consumption of oxalic acid, make again caused by
Titanium oxalate concentration is too high, the Precipitation on Titanium base, influences the effect of acid etching.
Masking liquid aoxidizes 10 ~ 20min in 470 ~ 510 DEG C of hot-airs, is the chlorine because in 470 ~ 510 DEG C of temperature range undercoating
Compound substantially aoxidizes completely, and temperature is less than 470 DEG C, and chlorinty is higher in coating, when temperature is higher than 510 DEG C, containing in coating
Oxygen amount declines on the contrary, because oxide is made up of non-stoichiometric oxide in coating, such as IrO2-XAnd TiO2-X, category
In anoxic oxide, now oxide structure changes in coating, and coating morphology changes.
Titanium base face coat is that multiple brush forms, face coat first layer relatively porous, heat when then brushing coating
The oxygen of oxidizing process can pass through porous first layer, the metal chloride reaction generation metal oxide with lower floor, so, coating
Porosity is reduced with number increase is brushed.Brush 14 ~ 20 times, coating is fine and close, more than 20 times, can increase the making of electrode
Cost.
Advantages of the present invention：
1. the present invention adds 'alpha '-hydroxy acids in the coating solution of iridium tantalum coated titanium electrode, such as tartaric acid, lactic acid, malic acid, lemon
Lemon acid etc..Metallic crystal particle can be made scattered and suspendability because 'alpha '-hydroxy acids have, in thermal oxidation process, can suppressed
Metallic crystal particle fast-growth is reunited, and coated titanium electrode of the crystal grain small structure densification without obvious crackle is made.
2. using ethylene glycol and the mixed solvent of n-butanol, compared to ethanol or n-butanol, strengthen the diffusivity of solvent, increase
The strong uniformity of coating solution.
3. coated titanium electrode average grain size prepared by the present invention is about 10nm, coating surface is without obvious crack, plane
Area's area is big and smooth, and grain particles are largely grown in plane area, and coating combines fine and close.
4. the reinforcing life of coated titanium electrode substantially increases, performance significantly improves.
Brief description of the drawings
Iridium tantalum coated titanium electrode SEM surface topography maps (540X) prepared by Fig. 1 embodiments 3；
Iridium tantalum coated titanium electrode SEM surface topography maps (540X) prepared by Fig. 2 embodiments 4.
Embodiment
With following examples, the present invention will be described in detail.
Embodiment 1：Chloro-iridic acid:Tantalic chloride:The percent mass ratio of citric acid is 57:38:5, volume ratio 1:1 ethylene glycol
And butanol solution, the concentration of chloro-iridic acid is 35g/L.
Preparation method：The preparation method of coated electrode：Titanium plate is put into 4% sodium carbonate liquor, boiled 40 minutes, then spend
Ionized water is rinsed well, drying；Place into the oxalic acid solution that concentration is 5% to boil 70 minutes, taking-up is rinsed well, drying；With hair
Brush brushes coating solution in titanium plate, and in 120 DEG C of drying, 15min is aoxidized then at 480 DEG C of hot-airs, after cooling, is repeated above-mentioned
Process 15 times, finally, after 480 DEG C of heat treatment 1.5h, normal temperature is cooled to, iridium tantalum coated titanium electrode is made.
Embodiment 2：Chloro-iridic acid:Tantalic chloride:The percent mass ratio of tartaric acid is 60:36:4, volume ratio 1:1 ethylene glycol
And butanol solution, the concentration of chloro-iridic acid is 35g/L.
Preparation method：The preparation method of coated electrode：Titanium plate is put into 6% sodium carbonate liquor, boiled 30 minutes, then spend
Ionized water is rinsed well, drying；Place into the oxalic acid solution that concentration is 5% to boil 60 minutes, taking-up is rinsed well, drying；With hair
Brush brushes coating solution in titanium plate, and in 130 DEG C of drying, 18min is aoxidized then at 500 DEG C of hot-airs, after cooling, is repeated above-mentioned
Process 17 times, finally, after 500 DEG C of heat treatment 1.2h, normal temperature is cooled to, iridium tantalum coated titanium electrode is made.
Embodiment 3：Chloro-iridic acid:Tantalic chloride:The percent mass ratio of malic acid is 57:38:5, volume ratio 1:1 ethylene glycol
And butanol solution, the concentration of chloro-iridic acid is 35g/L.
Preparation method：The preparation method of coated electrode：Titanium plate is put into 3% sodium carbonate liquor, boiled 20 minutes, then spend
Ionized water is rinsed well, drying；Place into the oxalic acid solution that concentration is 5% to boil 50 minutes, taking-up is rinsed well, drying；With hair
Brush brushes coating solution in titanium plate, and in 140 DEG C of drying, 10min is aoxidized then at 510 DEG C of hot-airs, after cooling, is repeated above-mentioned
Process 18 times, finally, after 510 DEG C of heat treatment 1h, normal temperature is cooled to, iridium tantalum coated titanium electrode is made.
Embodiment 4：Chloro-iridic acid:Tantalic chloride:The percent mass ratio of citric acid is 60:36:4, volume ratio 1:1 ethylene glycol
And butanol solution, the concentration of chloro-iridic acid is 35g/L.
Preparation method：The preparation method of coated electrode：Titanium plate is put into 5% sodium carbonate liquor, boiled 40 minutes, then spend
Ionized water is rinsed well, drying；Place into the oxalic acid solution that concentration is 6% to boil 70 minutes, taking-up is rinsed well, drying；With hair
Brush brushes coating solution in titanium plate, and in 130 DEG C of drying, 20min is aoxidized then at 490 DEG C of hot-airs, after cooling, is repeated above-mentioned
Process 19 times, finally, after 490 DEG C of heat treatment 1.8h, normal temperature is cooled to, iridium tantalum coated titanium electrode is made.
Using the grain diameter of XRD methods measure iridium tantalum coated titanium electrode coating surface, 1 the results are shown in Table.
The oxygen evolution potential and reinforcing life of the iridium tantalum coated titanium electrode of table 1
In 40 DEG C of temperature and 0.5mol/L H2SO4In the aqueous solution, 500 A/m2The oxygen evolution potential of lower measure iridium tantalum coated titanium electrode；
20000A/m2The reinforcing life of lower measure iridium tantalum coated titanium electrode（Tank voltage rises to the time used in 10V）, the results are shown in Table 1.Through upper
It is 1.39 ~ 1.44V to state method measure prior art oxygen evolution potential, and reinforcing life is 1480 ~ 1550 hours.
Iridium tantalum coated titanium electrode coating surface is generally made up of plane area and crack two parts.The average-size of crystal grain is got over
Small, the plane area of coating surface is bigger, and crack is trickleer.Fig. 1 and 2 is the iridium tantalum coated titanium electrode of embodiment 3 and 4 respectively
SEM surface topography maps（540 times of amplification）：The former is without obvious crackle, and crystal grain distribution is than more uniform；The latter is without obvious crackle, crystal
Particle is tiny, and crystal grain distribution is than more uniform.
Claims (5)
- A kind of 1. coating solution of coated electrode, it is characterized in that the volume ratio 1 by chloro-iridic acid, tantalic chloride and 'alpha '-hydroxy acids:1 Ethylene glycol and butanol solution, the concentration of chloro-iridic acid is 30 ~ 38g/L.
- 2. the coating solution of coated electrode according to claim 1, it is characterized in that the chloro-iridic acid:Tantalic chloride:Alpha-hydroxy The percent mass ratio of acid is 55 ~ 62:34~40:3~7.
- 3. the coating solution of coated electrode according to claim 1 or claim 2, it is characterized in that the chloro-iridic acid:Tantalic chloride:α-hydroxyl The percent mass ratio of base acid is 60:36:4.
- 4. the coating solution of coated electrode according to claim 1, it is characterized in that the 'alpha '-hydroxy acids are citric acid, winestone Acid, malic acid or lactic acid.
- 5. the preparation method of coated electrode described in claim 1, it is characterized in that comprising the steps of：Titanium plate is put into 3 ~ 8% carbon Acid sodium solution, boil 20 ~ 40 minutes, then rinsed well with deionized water, dried；The oxalic acid solution that concentration is 5 ~ 6% is placed into boil Boiling 50 ~ 70 minutes, taking-up is rinsed well, drying；Coating solution is brushed in titanium plate with hairbrush, in 120 ~ 140 DEG C of drying, then 10 ~ 20min is aoxidized in 470 ~ 510 DEG C of hot-airs, after cooling, repeats said process 14 ~ 20 times, last 470 ~ 510 DEG C, heat treatment After 1 ~ 2h, normal temperature is cooled to, coated electrode is made.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642479A (en) * | 2018-05-29 | 2018-10-12 | 江阴安诺电极有限公司 | The preparation method of the electrode coating of efficient high activity |
| CN108707881A (en) * | 2018-05-29 | 2018-10-26 | 江阴安诺电极有限公司 | The efficient iridium tantalum masking liquid of high activity and its iridium tantalum coating of formation |
| CN109402632A (en) * | 2018-12-18 | 2019-03-01 | 广东省稀有金属研究所 | A kind of electrode coating solution presoma, electrode coating solution, coated electrode and preparation method thereof |
| CN115159633A (en) * | 2022-07-13 | 2022-10-11 | 杭州奥特新环保科技有限公司 | Method for manufacturing titanium-based iridium tantalum tin coating electrode for high-salt organic wastewater |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642479A (en) * | 2018-05-29 | 2018-10-12 | 江阴安诺电极有限公司 | The preparation method of the electrode coating of efficient high activity |
| CN108707881A (en) * | 2018-05-29 | 2018-10-26 | 江阴安诺电极有限公司 | The efficient iridium tantalum masking liquid of high activity and its iridium tantalum coating of formation |
| CN109402632A (en) * | 2018-12-18 | 2019-03-01 | 广东省稀有金属研究所 | A kind of electrode coating solution presoma, electrode coating solution, coated electrode and preparation method thereof |
| CN115159633A (en) * | 2022-07-13 | 2022-10-11 | 杭州奥特新环保科技有限公司 | Method for manufacturing titanium-based iridium tantalum tin coating electrode for high-salt organic wastewater |
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Application publication date: 20180216 |