Preparation method of micro-cone array electrode structure for catalyzing active ejection separation of interface bubbles

The microcone array electrode structure is prepared by surface projection micro-stereoscopic lithography 3D printing technology, and combined with chemical deposition technology, the problem of bubble adhesion in electrolytic hydrogen production is solved, and the active ejection separation of bubbles is realized, which improves the efficiency and stability of electrolytic water hydrogen production, and reduces the preparation cost and process complexity.

CN119663326AActive Publication Date: 2025-03-21HARBIN INST OF TECH
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Patent Information

Application Number
CN202411870242.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-18
Publication Date
2025-03-21
Estimated Expiration
2044-12-18

AI Technical Summary

Technical Problem

In the existing electrolytic hydrogen production technology, bubbles adhere to the surface of the electrode catalyst, hindering the effective contact between the electrode and the electrolyte, resulting in low electrolytic efficiency, high preparation cost and complex process, making it difficult to achieve large-scale promotion.

Method used

The microcone array electrode structure is prepared by surface projection micro-stereoscopic lithography 3D printing technology, and the catalytic performance is imparted through chemical deposition, and the combined force of the microcone structure is used to achieve active ejection separation of bubbles.

Benefits of technology

The bubbles are cleaned on the electrode surface, the efficiency and stability of the electrolytic water hydrogen production reaction is improved, the preparation cost and process complexity are reduced, and the ion exchange in the electrolytic water hydrogen production reaction is promoted.

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Abstract

The invention discloses a preparation method of a micro-cone array electrode structure for catalyzing active ejection separation of interface bubbles, and belongs to the technical field of hydrogen production through water electrolysis and bubble power control. The method comprises the following steps: printing an electrode bottom plate and a micro-cone structure on the basis of a surface projection micro-stereo lithography printing technology; and then the catalyst is endowed with catalytic performance of water electrolysis hydrogen production through chemical deposition. Bubbles on the micro-cone array electrodes are driven to be ejected upwards between the micro-cone electrodes under the action of force generated by the bubbles and the surface interfaces of the micro-cone electrodes, namely upward resultant force such as bubble driving force and buoyancy force, so that active ejection separation is realized. The size of the bubbles is controlled by changing the structural size of the micro cone, ejection separation of all the bubbles is achieved, then ion exchange in the water electrolysis hydrogen production reaction is promoted, and efficient proceeding of the water electrolysis hydrogen production reaction is accelerated.
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Description

Technical Field

[0001] The invention belongs to the technical field of hydrogen production by electrolysis of water and bubble dynamics control, and specifically relates to a method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles. Background Art

[0002] In the field of electrolytic hydrogen production technology, improving electrolysis efficiency and achieving large-scale industrial applications are key goals. Currently, there are many challenges in the process of electrolytic hydrogen production, among which the problem of bubble adhesion on the surface of electrode catalysts is particularly prominent. When bubbles adhere to the surface of electrode catalysts, they hinder the effective contact between the electrode and the electrolyte, resulting in increased electrolysis resistance and reduced reaction rate, which ultimately greatly reduces the overall electrolysis efficiency.

[0003] To address this problem, existing electrode surface interface bubble manipulation technologies have emerged, such as asymmetric geometric gradient self-supporting electrodes and nanoparticle structure interface electrodes. These technologies have improved the bubble problem in the process of hydrogen production by water electrolysis to a certain extent, and have been widely used in this field. However, they still have obvious limitations. In terms of precise control and transportation of hydrogen bubbles, these technologies are difficult to achieve consistent control of bubble size, and the bubble separation efficiency is also unstable, which has formed a bottleneck for further improving the electrolysis efficiency. At the same time, its preparation cost is relatively high and the processing technology is complicated, which is not conducive to large-scale promotion and application.

[0004] In addition, self-supporting electrodes and nanoparticle structure electrodes have defects in the control of the micro-nano structure of the electrode surface interface, and there is randomness in the preparation process, making it difficult to construct an ideal electrode structure according to precise design, which affects the stability and repeatability of the electrode performance.

[0005] Based on the above-mentioned deficiencies of the existing technology, there is an urgent need to develop a new electrode structure and preparation method that can effectively solve multiple problems such as bubble adhesion, precise control of bubbles, and reduction of preparation cost and process complexity. Summary of the invention

[0006] In order to solve the above technical problems, the present invention provides a method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles.

[0007] The present invention provides a method for preparing a micro-cone array electrode structure for active ejection separation of bubbles at a catalytic interface, aiming to solve the problem of hydrogen bubbles hindering the reaction of hydrogen production by electrolysis of water. The present invention uses surface projection micro-stereolithography 3D printing technology to prepare an electrode substrate and a micro-cone array structure, and then gives it catalytic performance for hydrogen production by electrolysis of water through chemical deposition. Chemical deposition can realize customized deposition of catalytic materials according to experimental requirements and experimental environment. The bubbles on the micro-cone array electrode are acted upon by the force generated by the bubble and the surface interface of the micro-cone electrode, that is, the upward combined force of the bubble driving force and buoyancy, driving the bubbles to eject upward between the micro-cone electrodes, thereby realizing active ejection separation. At the same time, in the process of upward ejection, since the bubble is pulled in the vertical plane, there are different bubble radii above and below the bubble, and at the same time, a Laplace pressure in the vertically upward direction is generated, so the bubble accelerates upward ejection separation. This processing method is easy to process and has a simple principle. The size of the bubbles can be controlled by changing the structural dimensions of the micro-cone (micro-cone height, geometric center distance, bottom diameter and other geometric dimensions), and the ejection separation of all bubbles can be achieved, thereby promoting ion exchange in the water electrolysis hydrogen production reaction and accelerating the efficient progress of the water electrolysis hydrogen production reaction.

[0008] A method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles is specifically completed in the following steps:

[0009] 1. Using 3D modeling software to establish a 3D model of a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles; the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles is composed of an electrode bottom plate and a plurality of micro-cone structures;

[0010] The electrode bottom plate in step 1 is a rectangular parallelepiped or a cylinder;

[0011] In step 1, the micro-cone structure is a cone or a polygonal pyramid; the circumscribed circle of the cross-sectional shape of the bottom of the micro-cone structure is tangent; the bottom of the micro-cone structure is transitioned through a rounded corner;

[0012] 2. Use the corresponding slicing software to process the 3D model and transfer the processed model to the control system of the light-curing 3D printer;

[0013] 3. Print out the electrode base plate using a light-curing 3D printer, and print layer by layer on the electrode base plate to obtain a micro-cone array electrode structure;

[0014] 4. Post-processing the printed micro-cone array electrode structure with a 405nm ultraviolet lamp to obtain a cured micro-cone array electrode structure;

[0015] 5. soaking and shaking the solidified micro-cone array electrode structure in a hydrochloric acid solution, and drying to obtain a hydrochloric acid-treated micro-cone array electrode structure;

[0016] 6. using oxygen plasma to perform hydrophilic treatment on the micro-cone array electrode structure after the hydrochloric acid treatment, and drying to obtain the hydrophilic treated micro-cone array electrode structure;

[0017] 7. A nickel-based alloy catalyst is deposited on the hydrophilic micro-cone array electrode structure by chemical plating, and after drying, a micro-cone array electrode structure with active ejection separation of catalytic interface bubbles is obtained.

[0018] The working process of the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles in the present invention is as follows:

[0019] In a three-electrode electrolysis environment, the working electrode, i.e., the microcone array electrode structure for active ejection and separation of catalytic interface bubbles, is energized, and bubbles are generated on the microcone electrode. The tiny bubbles generated on the top are actively and quickly separated upward under the action of the bubble driving force and buoyancy. The bubbles generated at the bottom of the microcone electrode need to go through stages such as nucleation, aggregation, growth, and expansion. After the bubbles expand, they will be adsorbed on the four adjacent microcone structures under the action of bubble driving force, buoyancy, inertia force and other forces, and move upward rapidly. In this process, the bubbles present an asymmetric structure in the vertical plane, and are accompanied by the Laplace pressure difference. Therefore, the bubbles are accelerated upward in the vertical direction and reach the tip of the microcone for active ejection and separation.

[0020] The operation of step six of the present invention modifies the surface of the electrode into super-hydrophilic, so that the solution can better adhere to the electrode surface during the subsequent chemical deposition.

[0021] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0022] 1. The micro-cone array electrode for active bubble ejection separation can eject and separate all hydrogen bubbles generated on the micro-cone catalytic surface by relying on the combined force of adjacent micro-cones, thereby achieving bubble cleaning on the catalytic interface;

[0023] 2. The micro-cone array electrode with active bubble ejection separation has shown excellent hydrogen production stability after long-term water electrolysis hydrogen production test, and the bubble coverage rate is less than 5%;

[0024] 3. The catalyst material of the micro-cone array electrode separated by active bubble ejection can be custom deposited according to the acid-base environment and performance of hydrogen production by water electrolysis;

[0025] Fourth, the micro-cone array electrode for active ejection and separation of bubbles can use geometric dimensions such as micro-cone height, geometric center distance, bottom diameter, etc. to achieve control of the size and ejection separation time of hydrogen bubbles;

[0026] 5. The micro-cone array electrode for active bubble ejection separation has a simple structure and is integrally formed using surface projection micro-stereolithography 3D printing technology, making it easy to process and shape. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 Schematic diagram of the structure of the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles in Example 1, in which 1 is the micro-cone structure and 2 is the electrode bottom plate;

[0028] Figure 2 3 is a cross-sectional view of a micro-cone structure, in which 3 is a polymer light-curable resin and 4 is a nickel-based alloy catalyst;

[0029] Figure 3 A three-dimensional physical picture of the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles in Example 1;

[0030] Figure 4 This is a scanning electron microscope image of the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles in Example 1;

[0031] Figure 5 This is a diagram of the electrolytic hydrogen production and bubble control experiment process using a micro-cone array electrode structure with active ejection separation of catalytic interface bubbles prepared in Example 1;

[0032] Figure 6 This is a comparison chart of the effects of water electrolysis and hydrogen production using nickel-based carbon paper, nickel foam, and the micro-cone array electrode structure of the embodiment. DETAILED DESCRIPTION

[0033] Specific implementation method 1: This implementation method is described in conjunction with the accompanying drawings. The preparation method of a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles in this implementation method is specifically completed according to the following steps:

[0034] 1. Using 3D modeling software to establish a 3D model of a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles; the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles is composed of an electrode bottom plate and a plurality of micro-cone structures;

[0035] The electrode bottom plate in step 1 is a rectangular parallelepiped or a cylinder;

[0036] In step 1, the micro-cone structure is a cone or a polygonal pyramid; the circumscribed circle of the cross-sectional shape of the bottom of the micro-cone structure is tangent; the bottom of the micro-cone structure is transitioned through a rounded corner;

[0037] 2. Use the corresponding slicing software to process the 3D model and transfer the processed model to the control system of the light-curing 3D printer;

[0038] 3. Print out the electrode base plate using a light-curing 3D printer, and print layer by layer on the electrode base plate to obtain a micro-cone array electrode structure;

[0039] 4. Post-processing the printed micro-cone array electrode structure with a 405nm ultraviolet lamp to obtain a cured micro-cone array electrode structure;

[0040] 5. soaking and shaking the solidified micro-cone array electrode structure in a hydrochloric acid solution, and drying to obtain a hydrochloric acid-treated micro-cone array electrode structure;

[0041] 6. using oxygen plasma to perform hydrophilic treatment on the micro-cone array electrode structure after the hydrochloric acid treatment, and drying to obtain the hydrophilic treated micro-cone array electrode structure;

[0042] 7. A nickel-based alloy catalyst is deposited on the hydrophilic micro-cone array electrode structure by chemical plating, and after drying, a micro-cone array electrode structure with active ejection separation of catalytic interface bubbles is obtained.

[0043] The micro-cone structure of this embodiment can change the way bubbles adhere to the electrode surface. Compared with the existing electrode structure, the shape of the micro-cone makes it difficult for bubbles to stably adhere to its surface. When bubbles are generated, the inclined surface and sharp top of the micro-cone will make it easier for the bubbles to detach from the electrode surface, reducing the attachment time of the bubbles on the electrode surface and reducing the obstruction of the bubbles to the contact between the electrode and the electrolyte. During the preparation process, oxygen plasma is used for hydrophilic treatment; the surface of the micro-cone array electrode after hydrophilic treatment has better hydrophilicity; this means that water is easier to spread on the electrode surface, and the adhesion of bubbles on the surface with good hydrophilicity will be weakened. The hydrophilic treatment changes the properties of the electrode surface from hydrophobic (bubbles are easy to adhere to) to hydrophilic (bubbles are not easy to adhere to), further solving the problem of bubble adhesion.

[0044] Specific implementation method 2: This implementation method is different from the specific implementation method 1 in that the polygonal pyramid in step 1 is a triangular pyramid or a rectangular pyramid. The rest is the same as the specific implementation method 1.

[0045] Specific implementation method three: This implementation method is different from specific implementation method one in that the diameter of the circumscribed circle of the cross-sectional shape of the bottom of the micro-cone structure in step one is in the range of 50 to 300 μm. The rest is the same as specific implementation method one.

[0046] Specific implementation method 4: This implementation method is different from the specific implementation method 1 in that the height of the micro-cone structure in step 1 is 100-500 μm. The rest is the same as the specific implementation method 1.

[0047] Specific implementation example 5: This implementation example is different from the specific implementation example 1 in that the geometric center distance between adjacent micro-cone structures in step 1 is 70-130 μm. Other aspects are the same as those of the specific implementation example 1.

[0048] Specific implementation example 6: This implementation example is different from specific implementation example 1 in that: the material of the electrode bottom plate in step 1 is a polymer light-curing resin; the material of the micro-cone structure is a polymer light-curing resin. The rest is the same as specific implementation example 1.

[0049] Specific implementation method 7: This implementation method is different from the specific implementation method 1 in that the post-treatment time in step 4 is 3 to 5 minutes. The rest is the same as the specific implementation method 1.

[0050] Specific implementation example 8: This implementation example is different from the specific implementation example 1 in that the concentration of the hydrochloric acid in step 5 is 0.1 mol / L and the soaking time is 10 to 15 min. The rest is the same as the specific implementation example 1.

[0051] Specific embodiment 9: This embodiment is different from specific embodiment 1 in that: the hydrophilic treatment in step 6 is to place the micro-cone array electrode structure treated with hydrochloric acid on a glass slide, and use a handheld oxygen plasma processor to perform a 10-min reciprocating cycle bombardment treatment on the micro-cone array electrode structure treated with hydrochloric acid; the frequency of the handheld oxygen plasma processor is 4 MHz, and the output voltage is 30,000 V. Others are the same as specific embodiment 1.

[0052] Specific embodiment 10: This embodiment differs from specific embodiment 1 in that: in step 7, the nickel-based alloy catalyst is deposited on the hydrophilic micro-cone array electrode structure by chemical plating, and the specific steps are as follows:

[0053] 1. Prepare a solution consisting of 50 mL DI, 500 μL concentrated hydrochloric acid and 0.564 g SnCl2, and use a heating platform to heat the solution to 40°C, then immerse the microcone array electrode structure in the solution for 10 minutes, and stir the solution with a magnetic stirrer to ensure liquid circulation; then repeatedly rinse the microcone array electrode structure with DI three to five times, and dry it in a drying oven; then, place the microcone array electrode structure in an activation solution consisting of 50 mL DI, 200 μL concentrated hydrochloric acid with a mass fraction of 37% and 0.008 g PbCl2, and heat it at 50°C for 20 minutes to complete the activation process, thereby obtaining an activated microcone array electrode structure;

[0054] 2. Add 0.7275g NiSO4·6H2O to a beaker filled with 60mL deionized water, place the container on a heating table at 70°C, and use a magnetic stirrer to completely dissolve the solute in the beaker; then add 1.25g C6H8O7·H2O to the beaker and stir continuously; then adjust the pH value of the plating solution to 9-10 by dropping NH3·H2O into the beaker; finally, add 0.64g NaPO2H2·H2O and stir the plating solution thoroughly; place the activated microcone array electrode structure in the plating solution for 5 minutes, rinse it with DI, and dry it naturally. The rest is the same as the first embodiment.

[0055] The following examples are used to verify the beneficial effects of the present invention:

[0056] Example 1: Combination Figure 1 to Figure 5 This embodiment is described. This embodiment is a method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles. The method is specifically completed by the following steps:

[0057] 1. Using 3D modeling software to establish a 3D model of a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles; the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles is composed of an electrode bottom plate and a plurality of micro-cone structures;

[0058] The electrode bottom plate in step 1 is a rectangular parallelepiped;

[0059] The micro-cone structure in step 1 is a cone; the circumscribed circle of the cross-sectional shape of the bottom of the micro-cone structure is tangent; the bottom of the micro-cone structure is transitioned by a fillet; the diameter range of the circumscribed circle of the cross-sectional shape of the bottom of the micro-cone structure is 100 μm; the height of the micro-cone structure is 300 μm; the geometric center distance between adjacent micro-cone structures is 100 μm; the material of the electrode bottom plate and the micro-cone structure is HTL resin of Mofang Precision Co., Ltd.;

[0060] 2. Use the corresponding slicing software to process the 3D model and transfer the processed model to the control system of the light-curing 3D printer;

[0061] 3. Print out the electrode base plate using a light-curing 3D printer, and print layer by layer on the electrode base plate to obtain a micro-cone array electrode structure;

[0062] 4. Irradiating the printed micro-cone array electrode structure with a 405nm ultraviolet lamp for 3 to 5 minutes to obtain a cured micro-cone array electrode structure;

[0063] 5. Immerse the solidified micro-cone array electrode structure in a hydrochloric acid solution with a concentration of 0.1 mol / L and oscillate for 10 minutes, and dry for 10 minutes to obtain a micro-cone array electrode structure treated with hydrochloric acid;

[0064] 6. The hydrophilic treatment of the micro-cone array electrode structure after the hydrochloric acid treatment was performed by oxygen plasma for 10 minutes, and the hydrophilic treatment of the micro-cone array electrode structure was obtained after drying for 10 minutes;

[0065] The hydrophilic treatment is to place the micro-cone array electrode structure treated with hydrochloric acid on a glass slide, and use a handheld oxygen plasma processor to perform a 10-minute reciprocating cycle bombardment treatment on the micro-cone array electrode structure treated with hydrochloric acid; the frequency of the handheld oxygen plasma processor is 4 MHz, and the output voltage is 30000 V;

[0066] 7. Using chemical plating to deposit a nickel-based alloy catalyst on the hydrophilic micro-cone array electrode structure, and after drying, obtaining a micro-cone array electrode structure with active ejection separation of catalytic interface bubbles;

[0067] The nickel-based alloy catalyst is deposited on the hydrophilic microcone array electrode structure by chemical plating according to the following steps:

[0068] 1. Prepare a solution consisting of 50 mL DI, 500 μL concentrated hydrochloric acid and 0.564 g SnCl2, and use a heating platform to heat the solution to 40°C, then immerse the microcone array electrode structure in the solution for 10 minutes, and stir the solution with a magnetic stirrer to ensure liquid circulation; then repeatedly rinse the microcone array electrode structure with DI three to five times, and dry it in a drying oven; then, place the microcone array electrode structure in an activation solution consisting of 50 mL DI, 200 μL concentrated hydrochloric acid with a mass fraction of 37% and 0.008 g PbCl2, and heat it at 50°C for 20 minutes to complete the activation process, thereby obtaining an activated microcone array electrode structure;

[0069] 2. Add 0.7275g NiSO4·6H2O into a beaker containing 60mL deionized water, place the container on a heating table at 70°C, and use a magnetic stirrer to completely dissolve the solute in the beaker; then add 1.25g C6H8O7·H2O into the beaker and stir continuously; then adjust the pH value of the plating solution to 9-10 by adding NH3·H2O dropwise into the beaker; finally, add 0.64g NaPO2H2·H2O and stir the plating solution thoroughly; place the activated microcone array electrode structure into the plating solution for deposition for 5 minutes, rinse with DI, and dry naturally.

[0070] Hydrogen production by water electrolysis:

[0071] In a three-electrode electrolysis environment, a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles is placed in a three-electrode electrolysis hydrogen production acidic electrolytic cell, and a 0.1 mol / L sulfuric acid solution is added to the electrolytic cell, with the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles as the working electrode, graphite as the counter electrode, and silver / silver chloride as the reference electrode; after power is turned on with a constant voltage of 2V, bubbles are generated on the microneedle electrode, and the tiny bubbles generated on the top are actively and quickly separated upward under the action of the bubble driving force and buoyancy. The bubbles generated at the bottom of the micro-cone electrode need to go through the stages of nucleation, aggregation, growth, and expansion. After the bubbles expand, they will be adsorbed on the four adjacent micro-cone structures under the action of bubble driving force, buoyancy, inertial force, etc., and move upward rapidly. In this process, the bubbles present an asymmetric structure in the vertical plane, accompanied by the generation of Laplace pressure, so the bubbles accelerate upward in the vertical direction and reach the tip of the micro-cone for active ejection separation.

[0072] Figure 4 This is a scanning electron microscope image of the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles in Example 1;

[0073] Figure 5 This is a diagram of the electrolytic hydrogen production and bubble control experiment process using a micro-cone array electrode structure with active ejection separation of catalytic interface bubbles prepared in Example 1;

[0074] from Figure 4-Figure 5 It can be seen that a micro-cone array electrode structure that catalyzes the active ejection separation of interface bubbles can produce hydrogen.

[0075] Figure 6 This is a comparison of the effects of water electrolysis and hydrogen production using nickel-based carbon paper, nickel foam, and the microcone array electrode structure of the embodiment; under the same electrolysis environment and the same 2V constant voltage, the current density of the 3D microcone electrode is stable at 116mAcm -2 , which is 2.7 times the current density of nickel-based carbon paper and 1.51 times that of nickel foam electrode. Therefore, the 3D microcone electrode exhibits better bubble control ability and "cleaning" ability of the catalytic area on the electrode surface, thus having greater catalytic performance in hydrogen production by electrolysis.

Claims

1. A method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles, characterized in that The preparation method is specifically completed according to the following steps:

1. Using 3D modeling software to establish a 3D model of a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles; the micro-cone array electrode structure for active ejection separation of catalytic interface bubbles is composed of an electrode bottom plate and a plurality of micro-cone structures; The electrode bottom plate in step 1 is a rectangular parallelepiped or a cylinder; In step 1, the micro-cone structure is a cone or a polygonal pyramid; the circumscribed circle of the cross-sectional shape of the bottom of the micro-cone structure is tangent; The bottom of the micro-cone structure is transitioned through a rounded corner; 2. Use the corresponding slicing software to process the 3D model and transfer the processed model to the control system of the light-curing 3D printer; 3. Print out the electrode base plate using a light-curing 3D printer, and print layer by layer on the electrode base plate to obtain a micro-cone array electrode structure; 4. Post-processing the printed micro-cone array electrode structure with a 405nm ultraviolet lamp to obtain a cured micro-cone array electrode structure; 5. soaking and shaking the solidified micro-cone array electrode structure in a hydrochloric acid solution, and drying to obtain a hydrochloric acid-treated micro-cone array electrode structure; 6. using oxygen plasma to perform hydrophilic treatment on the micro-cone array electrode structure after the hydrochloric acid treatment, and drying to obtain the hydrophilic treated micro-cone array electrode structure; 7. A nickel-based alloy catalyst is deposited on the hydrophilic micro-cone array electrode structure by chemical plating, and after drying, a micro-cone array electrode structure with active ejection separation of catalytic interface bubbles is obtained.

2. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that The polygonal pyramid described in step 1 is a triangular pyramid or a rectangular pyramid.

3. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that The diameter of the circumscribed circle of the cross-sectional shape of the bottom of the micro-cone structure in step 1 ranges from 50 to 300 μm.

4. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that The height of the micro-cone structure in step 1 is 100 to 500 μm.

5. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that In step 1, the geometric center distance between adjacent micro-cone structures is 70 to 130 μm.

6. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that The material of the electrode bottom plate in step 1 is a polymer photocurable resin; the material of the micro-cone structure is a polymer photocurable resin.

7. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that The post-treatment time described in step 4 is 3 to 5 minutes.

8. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that The concentration of the hydrochloric acid described in step 5 is 0.1 mol / L; the soaking time is 10 to 15 minutes.

9. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that The hydrophilic treatment in step 6 is to place the micro-cone array electrode structure treated with hydrochloric acid on a glass slide, and use a handheld oxygen plasma processor to perform a reciprocating cycle bombardment treatment on the micro-cone array electrode structure treated with hydrochloric acid for 10 minutes; The handheld oxygen plasma processor has a frequency of 4MHz and an output voltage of 30,000V.

10. The method for preparing a micro-cone array electrode structure for active ejection separation of catalytic interface bubbles according to claim 1, characterized in that In step seven, the nickel-based alloy catalyst is deposited on the hydrophilic micro-cone array electrode structure by chemical plating according to the following steps:

1. Prepare a solution consisting of 50 mL DI, 500 μL concentrated hydrochloric acid and 0.564 g SnCl2, and use a heating platform to heat the solution to 40°C, then immerse the microcone array electrode structure in the solution for 10 minutes, and stir the solution with a magnetic stirrer to ensure liquid circulation; then repeatedly rinse the microcone array electrode structure with DI three to five times, and dry it in a drying oven; then, place the microcone array electrode structure in an activation solution consisting of 50 mL DI, 200 μL concentrated hydrochloric acid with a mass fraction of 37% and 0.008 g PbCl2, and heat it at 50°C for 20 minutes to complete the activation process, thereby obtaining an activated microcone array electrode structure; 2. Add 0.7275g NiSO4·6H2O to a beaker containing 60mL deionized water, place the container on a heating table at 70℃, and use a magnetic stirrer to completely dissolve the solute in the beaker; then add 1.25g C6H8O7·H2O to the beaker and stir continuously; then adjust the pH value of the plating solution to 9-10 by adding NH3·H2O dropwise to the beaker; finally, add 0.64g NaPO2H2·H2O and stir the plating solution thoroughly; place the activated microcone array electrode structure in the plating solution for deposition for 5 minutes, rinse it with DI, and dry it naturally.

Citation Information

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