CN115992371A - Cathode plasma electrolytic deposition preparation method for titanium-based noble metal anode - Google Patents
Cathode plasma electrolytic deposition preparation method for titanium-based noble metal anode Download PDFInfo
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Abstract
The invention discloses a cathode plasma electrolytic deposition preparation titanium-based noble metal anode and a preparation method thereof, wherein the anode comprises a titanium substrate and a noble metal oxide coating on the surface of the titanium substrate, the surface of the titanium substrate has certain roughness, the surface has no oxide layer, the thickness of the noble metal oxide coating is 0.5-10um, and the iridium-tantalum ratio is 1:9-9:1; the preparation method comprises the following steps: step 1: pretreating a titanium matrix; step 2: preparing electrolyte; step 3: taking the titanium matrix pretreated in the step 1 as a cathode, connecting a platinum sheet as an anode, immersing the cathode and the anode into the electrolytic solution in the step 2, and carrying out electrolytic deposition to finally obtain an iridium tantalum oxide anode; according to the invention, the oxide carrier is prepared on the metal surface by a one-step method, and meanwhile, noble metal is loaded in the oxide coating, and the energy released by micro-arc generated by voltage is used for sintering in the electrodeposition process, so that repeated brushing and sintering are avoided; has the characteristics of simple operation and high efficiency of the process.
Description
Technical Field
The invention belongs to the technical field of preparing noble metal-containing oxide coatings on the surface of a metallic titanium substrate, and particularly relates to a titanium-based noble metal anode prepared by cathode plasma electrolytic deposition and a preparation method thereof.
Background
The cathodic plasma electrolytic deposition technique is a novel method for preparing a coating by surface treatment, and the technique is developed on the basis of the traditional electrolytic technique. When the electrolytic cell is electrified, ions in the solution can directionally move towards the anode and cathode under the action of an electric field, and electrode reaction occurs. When the applied voltage reaches a certain critical point, a continuous air film is formed near the cathode, and the air film is broken down to generate plasma, and products formed by electrodeposition on the surface of the cathode are sintered by means of the energy of the plasma, and a series of complex physicochemical reactions occur in the process, so that a coating is finally formed.
Cathode plasma electrolytic deposition technology is not affected by the shape of a matrix, and does not require a sample to be valve metal unlike anode micro-arc oxidation, so that extensive scholars are led to research. The composition of the coating is derived from the solution, so that the composition and the phase structure of the coating can be controlled by changing the components of the electrolyte, and the method has the advantages of simple operation, high efficiency, easy doping and the like, and is widely applied to the fields of coating preparation and surface modification. Currently, cathode plasma electrolytic deposition technology is widely applied to the aspects of preparing metal coatings, ceramic coatings, preparing nanometer microspheres, cleaning surfaces and the like. Since the composition of the coating layer is derived from the solution, the catalyst-supporting washcoat can be prepared simultaneously by changing the system of the solution.
The electrodeposition method reduces metal ions into metal under the action of an external electric field, deposits the metal on a cathode and then sinters the metal to form oxide, and all the steps are needed to be carried out, so that the process is trivial. For example, document The durability of the thermally decomposed IrO 2 -Ta 2 O 5 coated titanium anode in a sulfate solution and Ti electrodes prepared by electrodeposition from different Ir: ta ratios for the degradation of polycyclic aromatic hydrocarbonsThe preparation of the noble metal anode needs to be carried out by electrodeposition and sintering for a plurality of times, the time is long, and the working procedure is quite complicated.
Patent application CN114592218A provides a titanium-based anode, a preparation method and application thereof, and the special oxide coating design can remarkably prolong the service life of the titanium-based anode, reduce the oxygen evolution potential of the titanium-based anode and improve the loadable current intensity and the acid resistance of the titanium-based anode; however, the steps of brushing and sintering are repeated, and the process is complicated.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a titanium-based noble metal anode prepared by cathode plasma electrolytic deposition and a preparation method thereof, wherein noble metal is simultaneously loaded in an oxide coating while an oxide carrier is prepared on the surface of metal by a one-step method, and energy released by micro-arc generated by voltage is used for sintering in the process of electrodeposition, so that repeated brushing and sintering are avoided; has the characteristics of simple operation and high efficiency of the process.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a cathode plasma electrolytic deposition process for preparing a titanium-based noble metal anode having electrocatalytic properties.
A cathode plasma electrolytic deposition preparation titanium-based noble metal anode comprises a titanium matrix and a noble metal oxide coating on the surface of the titanium matrix, wherein the surface of the titanium matrix has certain roughness and no oxide scale; the thickness of the noble metal oxide coating is 0.5-10um, and the iridium-tantalum ratio is 1:9-9:1.
A preparation method for preparing a titanium-based noble metal anode by cathode plasma electrolytic deposition comprises the following steps of;
step 1: pretreating a titanium matrix;
step 2: preparing an electrolyte: weighing and dissolving the iridium source-containing substance in an organic solvent, stirring at room temperature until the iridium source-containing substance is completely dissolved, weighing and dissolving a certain amount of tantalum source-containing substance in the iridium source-containing organic solvent, stirring at room temperature until the iridium source-containing substance is completely dissolved, and adding 3-6g of sodium chloride as a conductive agent into the mixture;
step 3: and (2) connecting the pretreated titanium matrix in the step (1) to a negative electrode of a power supply through a lead to serve as a cathode, connecting a positive electrode of the pretreated titanium matrix with a platinum sheet to serve as an anode, immersing the cathode and the anode in the electrolytic solution in the step (2), and carrying out electrolytic deposition to finally obtain the iridium tantalum oxide anode.
The step 1 is to pretreat the titanium matrix, which comprises surface degreasing and sand blasting treatment, wherein the sand blasting treatment is carried out until the surface roughness Ra <15um.
And (2) performing thermal shaping treatment on the titanium matrix after sand blasting in the step (1).
And step 1, soaking the shaped titanium matrix in 3-15% diluted hydrochloric acid for 8-24h, boiling in 5-10% oxalic acid solution for 0.5-3h, and cleaning and airing the titanium matrix.
The iridium source in the step 2 is selected from any one of chloroiridic acid, iridium trichloride and bromoiridic acid.
And the tantalum source in the step 2 is selected from any one of tantalum pentachloride n-butanol solution, butanediol tantalum and ethanol tantalum.
The organic solvent in the step 2 is selected from any one of n-butanol, isopropanol and ethanol or any mixture thereof.
In the step 2, the iridium source, the tantalum source and the organic solvent are in any ratio.
The specific limiting conditions of the electrolytic deposition in the step 3 are as follows: the boosting speed is 1V/s, the final voltage ranges from 120V to 180V, the frequency is 2000Hz, the duty ratio is 80%, and the deposition time is 3 to 20min.
The area ratio of the cathode to the anode which are actually conducted in the step 3 is smaller than 1:2, and the distance between the cathode and the anode is 3cm to 7cm.
The invention has the beneficial effects that:
according to the invention, the noble metal oxide coating is prepared by utilizing a cathode plasma electrolytic deposition method, so that the repeated coating and sintering procedures are reduced, the complexity of the process is reduced, and oxide coatings with different thicknesses can be prepared in a short time; in addition, the catalytic activity of the noble metal oxide can be changed by adjusting the composition in the electrolyte to change the composition and phase of the oxide coating.
The cathode and the anode in the solution are respectively separated out of hydrogen and oxygen, and the ratio of the separated out gas is 2:1, so that the critical value of the area ratio is equal to 2, when the area ratio of the cathode to the anode is smaller than the critical value, the discharge phenomenon occurs at the cathode, a large number of bubbles are generated on the surface of the cathode to form a closed gas sheath, and when the electric field strength exceeds the critical breakdown field strength of the gas, the gas sheath starts to be broken down and discharged. When the gas sheath is broken down, the cathode overpotential is mainly concentrated on the tantalum pentoxide ceramic coating, and the electric field strength acting on the tantalum pentoxide ceramic coating is increased. In addition, a large amount of heat is generated during plasma discharge breakdown, and the mixed metal oxide coating of iridium dioxide and tantalum pentoxide is sintered to form an oxide.
Drawings
FIG. 1 is a schematic diagram of the principle simulation of the present invention employing cathode plasma electrolytic deposition.
FIG. 2 is a schematic view of current density and voltage curves during cathode plasma electrolytic deposition in accordance with the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings.
A cathode plasma electrolytic deposition process for preparing a titanium-based noble metal anode having electrocatalytic properties.
A cathode plasma electrolytic deposition preparation titanium-based noble metal anode comprises a titanium matrix and a noble metal oxide coating on the surface of the titanium matrix, wherein the surface of the titanium matrix has certain roughness and no oxide scale; the thickness of the noble metal oxide coating is 0.5-10um, and the iridium-tantalum ratio is 1:9-9:1.
The invention provides a method for preparing a noble metal oxide anode by cathode plasma electrolytic deposition, wherein a coating of a titanium anode is prepared by the method of the plasma electrolytic deposition, and the specific preparation steps are as follows:
step 1: pretreatment of the titanium matrix: degreasing, sandblasting, sizing and pickling the surface of the titanium substrate, wherein the sandblasting treatment is carried out until the surface roughness Ra is less than 15um;
step 2: preparing an electrolyte: weighing a certain amount of chloroiridium acid to be dissolved in n-butanol solution, and stirring at room temperature until the chloroiridium acid is completely dissolved; weighing a certain amount of tantalum pentachloride n-butanol solution to be dissolved in an n-butanol solvent containing chloroiridic acid, stirring at room temperature until the solution is completely dissolved, and adding 3-6g of sodium chloride as a conductive agent into the solution;
step 3: electrolytic deposition: connecting a titanium matrix to a negative electrode of a power supply through a lead as a cathode, connecting a positive electrode with a platinum sheet as an anode, immersing the anode and the cathode in an electrolytic solution, controlling the area ratio of the anode to the cathode to be actually conducted to be smaller than 1:2, and controlling the distance between the anode and the cathode to be 3cm; the specific limiting conditions of the electrolytic deposition are as follows: the boosting speed is 1V/s, the final voltage ranges from 120V to 180V, the frequency is 2000Hz, the duty ratio is 80%, and the deposition time is 3 to 20min.
Example 1
The embodiment provides a cathode plasma electrolytic deposition method for preparing a titanium-based noble metal anode, which comprises a titanium matrix and a noble metal oxide coating on the surface of the titanium matrix, wherein the surface of the titanium matrix has certain roughness and no oxide scale; the thickness of the noble metal oxide coating is 0.8um, and the iridium-tantalum ratio is 7:3.
The embodiment provides a preparation method for preparing a noble metal anode by adopting cathode plasma electrolytic deposition, which comprises the following specific steps:
step 1: pretreatment of the titanium matrix: degreasing, sandblasting, sizing and pickling the surface of the titanium substrate, wherein the sandblasting treatment is carried out until the surface roughness Ra is less than 15um;
step 2: preparing an electrolyte: 40g of chloroiridium acid is weighed and dissolved in 500ml of n-butanol solution, and stirred at room temperature (25 ℃) until the chloroiridium acid is completely dissolved; 70ml of tantalum pentachloride n-butanol solution was weighed and dissolved in n-butanol solvent containing chloroiridic acid, stirred at room temperature (25 ℃) until completely dissolved, and 5g of sodium chloride was added thereto as a conductive agent;
step 3: electrolytic deposition: connecting a titanium matrix to a negative electrode of a power supply through a lead as a cathode, connecting a positive electrode with a platinum sheet as an anode, immersing the anode and the cathode in an electrolytic solution, controlling the area ratio of the anode to the cathode to be actually conducted to be smaller than 1:2, and controlling the distance between the anode and the cathode to be 3cm; the specific limiting conditions of the electrolytic deposition are as follows: the boost speed is 1V/s, the final voltage is 120V, the frequency is 2000Hz, the duty ratio is 80%, and the deposition time is 3min.
Example 2
The embodiment provides a cathode plasma electrolytic deposition method for preparing a titanium-based noble metal anode, which comprises a titanium matrix and a noble metal oxide coating on the surface of the titanium matrix, wherein the surface of the titanium matrix has certain roughness and no oxide scale; the thickness of the noble metal oxide coating is 1um, and the iridium-tantalum ratio is 7:3.
The embodiment provides a preparation method for preparing a noble metal anode by adopting cathode plasma electrolytic deposition, which comprises the following specific steps:
step 1: pretreatment of the titanium matrix: degreasing, sandblasting, sizing and pickling the surface of the titanium substrate, wherein the sandblasting treatment is carried out until the surface roughness Ra is less than 15um;
step 2: preparing an electrolyte: 40g of chloroiridium acid is weighed and dissolved in 500ml of n-butanol solution, and stirred at room temperature (25 ℃) until the chloroiridium acid is completely dissolved; 70ml of tantalum pentachloride n-butanol solution was weighed and dissolved in n-butanol solvent containing chloroiridic acid, stirred at room temperature (25 ℃) until completely dissolved, and 5g of sodium chloride was added thereto as a conductive agent;
step 3: electrolytic deposition: connecting a titanium matrix to a negative electrode of a power supply through a lead as a cathode, connecting a positive electrode with a platinum sheet as an anode, immersing the anode and the cathode in an electrolytic solution, controlling the area ratio of the anode to the cathode to be actually conducted to be smaller than 1:2, and controlling the distance between the anode and the cathode to be 3cm; the specific limiting conditions of the electrolytic deposition are as follows: the boost speed is 1V/s, the final voltage is 180V, the frequency is 2000Hz, the duty ratio is 80%, and the deposition time is 5min.
Example 3
The embodiment provides a cathode plasma electrolytic deposition method for preparing a titanium-based noble metal anode, which comprises a titanium matrix and a noble metal oxide coating on the surface of the titanium matrix, wherein the surface of the titanium matrix has certain roughness and no oxide scale; the thickness of the noble metal oxide coating is 2um, and the iridium-tantalum ratio is 7:3.
The embodiment provides a preparation method for preparing a noble metal anode by adopting cathode plasma electrolytic deposition, which comprises the following specific steps:
step 1: pretreatment of the titanium matrix: degreasing, sandblasting, sizing and pickling the surface of the titanium substrate, wherein the sandblasting treatment is carried out until the surface roughness Ra is less than 15um;
step 2: preparing an electrolyte: 40g of chloroiridium acid is weighed and dissolved in 500ml of n-butanol solution, and stirred at room temperature (25 ℃) until the chloroiridium acid is completely dissolved; 70ml of tantalum pentachloride n-butanol solution was weighed and dissolved in n-butanol solvent containing chloroiridic acid, stirred at room temperature (25 ℃) until completely dissolved, and 5g of sodium chloride was added thereto as a conductive agent;
step 3: electrolytic deposition: connecting a titanium matrix to a negative electrode of a power supply through a lead as a cathode, connecting a positive electrode with a platinum sheet as an anode, immersing the anode and the cathode in an electrolytic solution, controlling the area ratio of the anode to the cathode to be actually conducted to be smaller than 1:2, and controlling the distance between the anode and the cathode to be 3cm; the specific limiting conditions of the electrolytic deposition are as follows: the boost speed was 1V/s, and finally the voltage was 150V, the frequency was 2000Hz, the duty cycle was 80%, and the deposition time was 10min.
Example 4
The embodiment provides a cathode plasma electrolytic deposition method for preparing a titanium-based noble metal anode, which comprises a titanium matrix and a noble metal oxide coating on the surface of the titanium matrix, wherein the surface of the titanium matrix has certain roughness and no oxide scale; the thickness of the noble metal oxide coating is 3.5um, and the iridium-tantalum ratio is 7:3.
The embodiment provides a preparation method for preparing a noble metal anode by adopting cathode plasma electrolytic deposition, which comprises the following specific steps:
step 1: pretreatment of the titanium matrix: degreasing, sandblasting, sizing and pickling the surface of the titanium substrate, wherein the sandblasting treatment is carried out until the surface roughness Ra is less than 15um;
step 2: preparing an electrolyte: 40g of chloroiridium acid is weighed and dissolved in 500ml of n-butanol solution, and stirred at room temperature (25 ℃) until the chloroiridium acid is completely dissolved; 70ml of tantalum pentachloride n-butanol solution was weighed and dissolved in n-butanol solvent containing chloroiridic acid, stirred at room temperature (25 ℃) until completely dissolved, and 5g of sodium chloride was added thereto as a conductive agent;
step 3: electrolytic deposition: connecting a titanium matrix to a negative electrode of a power supply through a lead as a cathode, connecting a positive electrode with a platinum sheet as an anode, immersing the anode and the cathode in an electrolytic solution, controlling the area ratio of the anode to the cathode to be actually conducted to be smaller than 1:2, and controlling the distance between the anode and the cathode to be 3cm; the specific limiting conditions of the electrolytic deposition are as follows: the boost speed is 1V/s, the final voltage is 150V, the frequency is 2000Hz, the duty ratio is 80%, and the deposition time is 15min.
Example 5
The embodiment provides a cathode plasma electrolytic deposition method for preparing a titanium-based noble metal anode, which comprises a titanium matrix and a noble metal oxide coating on the surface of the titanium matrix, wherein the surface of the titanium matrix has certain roughness and no oxide scale; the thickness of the noble metal oxide coating is 5um, and the iridium-tantalum ratio is 7:3.
The embodiment provides a preparation method for preparing a noble metal anode by adopting cathode plasma electrolytic deposition, which specifically comprises the following steps:
step 1: pretreatment of the titanium matrix: degreasing, sandblasting, sizing and pickling the surface of the titanium substrate, wherein the sandblasting treatment is carried out until the surface roughness Ra is less than 15um;
step 2: preparing an electrolyte: 40g of chloroiridium acid is weighed and dissolved in 500ml of n-butanol solution, and stirred at room temperature (25 ℃) until the chloroiridium acid is completely dissolved; 70ml of tantalum pentachloride n-butanol solution was weighed and dissolved in n-butanol solvent containing chloroiridic acid, stirred at room temperature (25 ℃) until completely dissolved, and 5g of sodium chloride was added thereto as a conductive agent;
step 3: electrolytic deposition: connecting a titanium matrix to a negative electrode of a power supply through a lead as a cathode, connecting a positive electrode with a platinum sheet as an anode, immersing the anode and the cathode in an electrolytic solution, controlling the area ratio of the anode to the cathode to be actually conducted to be smaller than 1:2, and controlling the distance between the anode and the cathode to be 3cm; the specific limiting conditions of the electrolytic deposition are as follows: the voltage boosting speed is 1V/s, the final voltage is 150V, the frequency is 2000Hz, the duty ratio is 80%, and the deposition time is 20min.
As shown in fig. 1 and 2: the variation of the oxygen evolution potential under a sulfuric acid system of 1mol/L for the section thickness of the noble metal anode prepared by the preparation method provided in examples 1 to 5 is as follows:
| example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Thickness of (L) | 0.8um | 1um | 2um | 3.5um | 5um |
| Oxygen evolution potential | 1.374V | 1.379V | 1.382V | 1.384V | 1.385V |
Iridium tantalum anodes with electrocatalytic properties were successfully prepared by the test data of thickness and oxygen evolution potential in the above examples. Compared with the prior art, the method for preparing the noble metal anode with electrocatalytic activity has the advantages of being quick, simple, easy to operate and the like.
In summary, the method for preparing the noble metal anode by adopting the cathode plasma electrolytic deposition in the invention adopts the method that the high voltage is applied to the two ends of the cathode and the anode so as to generate micro-arcs and release a large amount of energy, the sintering is carried out in the electrodeposition process, the thickness of the coating is gradually increased by prolonging the electrolysis time, the noble metal anode is prepared by a one-step method, the complicated process is avoided, and the change of the composition of the oxide coating can be realized by changing the composition of the electrolyte. Improves the production efficiency of the anode and can better meet the market demand.
Claims (10)
1. A titanium-based noble metal anode prepared by cathode plasma electrolytic deposition is characterized in that the noble metal anode has electrocatalytic performance.
2. The method for preparing the titanium-based noble metal anode by cathode plasma electrolytic deposition according to claim 1, which is characterized by comprising a titanium substrate and a noble metal oxide coating on the surface of the titanium substrate, wherein the surface of the titanium substrate has certain roughness and no oxide scale; the thickness of the noble metal oxide coating is 0.5-10um, and the iridium-tantalum ratio is 1:9-9:1.
3. A method for preparing a titanium-based noble metal anode based on a cathodic plasma electrolytic deposition as claimed in claim 1 or 2, characterized by comprising the steps of;
step 1: pretreating a titanium matrix;
step 2: preparing an electrolyte: weighing and dissolving the iridium source-containing substance in an organic solvent, stirring at room temperature until the iridium source-containing substance is completely dissolved, weighing and dissolving a certain amount of tantalum source-containing substance in the iridium source-containing organic solvent, stirring at room temperature until the iridium source-containing substance is completely dissolved, and adding 3-6g of sodium chloride into the mixture;
step 3: and (2) connecting the pretreated titanium matrix in the step (1) to a negative electrode of a power supply through a lead to serve as a cathode, connecting a positive electrode of the pretreated titanium matrix with a platinum sheet to serve as an anode, immersing the cathode and the anode in the electrolytic solution in the step (2), and carrying out electrolytic deposition to finally obtain the iridium tantalum oxide anode.
4. A method for preparing a titanium-based noble metal anode by cathodic plasma deposition according to claim 3 wherein said step 1 of pre-treating the titanium substrate comprises surface degreasing and sand blasting, said sand blasting being carried out until the surface roughness Ra <15um;
the step 1 is to carry out thermal shaping treatment on the titanium matrix after sand blasting;
and step 1, soaking the shaped titanium matrix in 3-15% diluted hydrochloric acid for 8-24h, boiling in 5-10% oxalic acid solution for 0.5-3h, and cleaning and airing the titanium matrix.
5. The method for preparing a titanium-based noble metal anode by cathodic plasma electrolytic deposition of claim 3 wherein said iridium source of step 2 is selected from any one of chloroiridic acid, iridium trichloride, bromoiridic acid.
6. The method for preparing a titanium-based noble metal anode by cathodic plasma electrodeposition according to claim 3 wherein the tantalum source in step 2 is selected from any one of tantalum pentachloride n-butanol solution, tantalum butanediol, tantalum ethoxide.
7. The method for preparing a titanium-based noble metal anode by cathode plasma electrolytic deposition according to claim 3, wherein the organic solvent in the step 2 is selected from any one of n-butanol, isopropanol and ethanol or any mixture thereof.
8. The method for preparing a titanium-based noble metal anode by cathodic plasma electrolytic deposition as recited in claim 3 wherein said iridium source, tantalum source and organic solvent are present in any ratio in step 2.
9. A method for preparing a titanium-based noble metal anode by cathodic plasma electrodeposition according to claim 3 wherein said step 3 electrodeposition is specifically defined by: the boosting speed is 1V/s, the final voltage ranges from 120V to 180V, the frequency is 2000Hz, the duty ratio is 80%, and the deposition time is 3 to 20min.
10. The method for preparing a titanium-based noble metal anode by cathode plasma electrolytic deposition according to claim 3, wherein the area ratio of the cathode to the anode which is actually conducted in the step 3 is less than 1:2, and the distance between the cathode and the anode is 3cm to 7cm.
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Cited By (2)
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| CN117568878A (en) * | 2024-01-15 | 2024-02-20 | 甘肃海亮新能源材料有限公司 | Production equipment of titanium anode and electrolytic copper foil |
| CN117568878B (en) * | 2024-01-15 | 2024-05-03 | 甘肃海亮新能源材料有限公司 | Production equipment of titanium anode and electrolytic copper foil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117568878A (en) * | 2024-01-15 | 2024-02-20 | 甘肃海亮新能源材料有限公司 | Production equipment of titanium anode and electrolytic copper foil |
| CN117568878B (en) * | 2024-01-15 | 2024-05-03 | 甘肃海亮新能源材料有限公司 | Production equipment of titanium anode and electrolytic copper foil |
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