Preparation method of hydrogen production electrode

Abstract

The invention discloses a preparation method of a hydrogen production electrode, and belongs to the technical field of preparation of hydrogen production electrodes, and the preparation method comprises the following steps: S1, pre-treating a nickel net, and carrying out sand blasting treatment and acid pickling on the nickel net; s2, the pretreated nickel net is subjected to electrochemical treatment, and electrochemical oxidation of the nickel net is completed; and S3, the nickel net subjected to electrochemical oxidation is placed in protective gas to be calcined, and an N / N O layer is formed on the surface of the nickel net after calcination. According to the preparation method of the hydrogen production electrode, the catalyst layer is generated by utilizing the material of the nickel net, an additional catalyst or a catalyst precursor is not needed, the raw material cost of the hydrogen production electrode can be greatly reduced, in addition, the oxidation layer can be effectively generated on the surface of the nickel net through the electrochemical oxidation method, the thickness of the oxidation layer is controllable, and the hydrogen production electrode is prepared. And finally, an N / N O layer is formed on the surface of the nickel net through calcination, so that the conductivity and catalytic activity of the electrode are effectively improved.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation of hydrogen production electrodes, and in particular relates to a preparation method of a hydrogen production electrode. Background Art

[0002] The most core issue facing hydrogen production by water electrolysis at present is the development of efficient, stable and cheap hydrogen production electrocatalysts.

[0003] So far, the most effective catalyst for water electrolysis is precious metal catalyst, but the raw materials of precious metal catalyst are scarce and expensive, which seriously restricts its large-scale application in practice. Among non-precious metal catalysts, nickel-based catalysts are currently commonly used catalysts for water electrolysis, but their catalytic activity is low, conductivity is poor, and the hydrogen evolution process is slow, which needs to be improved by certain means. At present, the commonly used preparation methods for nickel-based catalyst electrodes are plasma spraying, electroplating, etc., but these methods have high requirements on catalyst loss or catalyst precursors, and it is difficult to form nickel-based catalyst electrodes with high catalytic activity, good conductivity, and fast hydrogen evolution process. Summary of the invention

[0004] The present invention overcomes the deficiencies of the prior art and provides a method for preparing a hydrogen production electrode to solve the problems existing in the prior art.

[0005] To achieve the above object, the technical solution adopted by the present invention is: a method for preparing a hydrogen production electrode, comprising the following steps:

[0006] S1. Pre-treating the nickel mesh by sandblasting and pickling the nickel mesh;

[0007] S2, electrochemically treating the pretreated nickel mesh to complete electrochemical oxidation of the nickel mesh;

[0008] S3, calcining the electrochemically oxidized nickel mesh in a protective gas, and forming a Ni / NiO layer on the surface of the nickel mesh after calcination.

[0009] In a preferred embodiment of the present invention, the nickel mesh is pickled with a 10-30% hydrochloric acid solution or a sulfuric acid solution, and the pickling time is 10-30 minutes.

[0010] In a preferred embodiment of the present invention, in step S2, the electrochemical oxidation is a two-electrode system, the negative electrode is nickel or a nickel alloy material, and the positive electrode is a pretreated electrode.

[0011] In a preferred embodiment of the present invention, the electrolyte used in the electrochemical oxidation is 0.1-5 mol KOH or NaOH solution, and the electrochemical oxidation voltage is set to 0.8-1.5V.

[0012] In a preferred embodiment of the present invention, in step S3, the protective gas is nitrogen or argon.

[0013] In a preferred embodiment of the present invention, in step S3, the calcination temperature is 250-300° C., and the calcination time is 0.5-1 h.

[0014] In a preferred embodiment of the present invention, the mesh size of the nickel mesh is 40-80 meshes.

[0015] The present invention solves the defects existing in the background technology and has the following beneficial effects:

[0016] The present invention provides a method for preparing a hydrogen production electrode, which utilizes the material of the nickel mesh itself to generate a catalytic layer, does not require an additional catalyst or catalyst precursor, and can greatly reduce the raw material cost of the hydrogen production electrode. In addition, the electrochemical oxidation method can effectively generate an oxide layer on the surface of the nickel mesh, and the thickness of the oxide layer is controllable. Then, a Ni / NiO layer is finally formed on the surface of the nickel mesh through calcination, which effectively improves the conductivity and catalytic activity of the electrode. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] The present invention is further described below in conjunction with the accompanying drawings and embodiments;

[0018] Figure 1 A flowchart of a preferred embodiment of the present invention; DETAILED DESCRIPTION

[0019] The following will disclose multiple embodiments of the present invention with drawings. For the purpose of clear description, many physical details will be described together in the following description. However, it should be understood that these physical details should not be used to limit the present invention. That is, in some embodiments of the present invention, these physical details are not necessary. In addition, for the purpose of simplifying the drawings, some conventional structures and components will be depicted in a simple schematic manner in the drawings.

[0020] In addition, in the present invention, the descriptions of "first", "second", etc. are only used for descriptive purposes, and do not specifically refer to the order or sequence, nor are they used to limit the present invention. They are only used to distinguish components or operations described with the same technical terms, and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the ability of ordinary technicians in the field to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0021] Embodiment 1

[0022] In this embodiment, a 46-mesh twill nickel mesh is treated by sandblasting and soaking in 10% hydrochloric acid for 20 minutes, and then electrochemically treated. Specifically, the nickel mesh is used as the cathode, and the treated twill nickel mesh is used as the anode. A voltage of 1.0 V is applied to the nickel mesh in a 1 mol KOH solution. After the nickel mesh is electrochemically oxidized for 10 minutes, the oxidized nickel mesh is cleaned and dried, and then calcined at 300°C for 1 hour in a nitrogen protective gas, and the final hydrogen production electrode is obtained after cooling. The hydrogen production electrode is in a 1 mol KOH solution, 10 mA / cm 2 At a current density of , the overpotential is 132 mV.

[0023] Embodiment 2

[0024] The 40-mesh plain nickel mesh was treated by sandblasting and soaking in 20% sulfuric acid for 15 minutes, and then electrochemically treated. Specifically, the nickel mesh was used as the cathode and the treated plain nickel mesh was used as the anode. A voltage of 0.8V was applied to the nickel mesh in a 1 mol NaOH solution. After the nickel mesh was electrochemically oxidized for 15 minutes, the oxidized nickel mesh was cleaned and dried, and then calcined at 280°C for 1 hour in an argon protective gas. After cooling, the final hydrogen production electrode was obtained. The hydrogen production electrode was in a 1 mol KOH solution at 10 mA / cm 2 At a current density of , the overpotential is 156 mV.

[0025] In combination with Example 1 and Example 2, the present invention utilizes the material of the nickel mesh itself to generate a catalytic layer, and does not require additional catalysts or catalyst precursors, which can greatly reduce the raw material cost of the hydrogen production electrode. In addition, the electrochemical oxidation method can effectively generate an oxide layer on the surface of the nickel mesh, and the thickness of the oxide layer is controllable. Then, a Ni / NiO layer is finally formed on the surface of the nickel mesh through calcination, which effectively improves the conductivity and catalytic activity of the electrode.

[0026] Although the present invention has been described above with reference to various embodiments, it should be understood that many changes and modifications may be made without departing from the scope of the present invention. That is, the methods, systems or devices discussed above are all examples. Various configurations may appropriately omit, replace or add various processes or components. For example, in alternative configurations, the method may be performed in an order different from the order described, and / or various stages may be added, omitted and / or combined. Moreover, the features described with respect to certain configurations may be combined in various other configurations. Different aspects and elements of the configurations may be combined in a similar manner. In addition, with the development of technology, many elements are merely examples and do not limit the scope of the present disclosure or claims.

[0027] Specific details are given in the specification to provide a thorough understanding of the exemplary configurations including implementations. However, the configurations can be practiced without these specific details, for example, well-known circuits, processes, algorithms, structures, and techniques have been shown without unnecessary details to avoid obscuring the configurations. This description provides only example configurations and does not limit the scope, applicability, or configurations of the claims. On the contrary, the foregoing description of the configurations will provide those skilled in the art with an enabling description for implementing the described techniques. Various changes may be made to the functions and arrangements of the elements without departing from the spirit or scope of the present disclosure.

[0028] In addition, although each operation may describe the operation as a sequential process, many operations may be performed in parallel or simultaneously. In addition, the order of the operations may be rearranged. A process may have additional steps. In addition, examples of methods may be implemented by hardware, software, firmware, middleware, code, hardware description language, or any combination thereof. When implemented in software, firmware, middleware, or code, program code or code segments for performing the necessary tasks may be stored in a non-transitory computer-readable medium such as a storage medium, and the described tasks are performed by a processor.

[0029] In summary, it is intended that the above detailed description is considered to be exemplary rather than restrictive, and it should be understood that the claims (including all equivalents) are intended to limit the spirit and scope of the present invention. The above embodiments should be understood to be only used to illustrate the present invention and not to limit the scope of protection of the present invention. After reading the content of the record of the present invention, the technician can make various changes or modifications to the present invention, and these equivalent changes and modifications also fall into the scope limited by the claims of the present invention.

Claims

1. A method for preparing a hydrogen production electrode, characterized in that: The following steps are involved: S1. Pre-treating the nickel mesh by sandblasting and pickling the nickel mesh; S2, electrochemically treating the pretreated nickel mesh to complete electrochemical oxidation of the nickel mesh; S3, calcining the electrochemically oxidized nickel mesh in a protective gas, and forming a Ni / NiO layer on the surface of the nickel mesh after calcination.

2. The method for preparing a hydrogen production electrode according to claim 1, characterized in that: In step S1, the nickel mesh is pickled with a 10-30% hydrochloric acid solution or a sulfuric acid solution for 10-30 minutes.

3. The method for preparing a hydrogen production electrode according to claim 1, characterized in that: In step S2, the electrochemical oxidation is a two-electrode system, the negative electrode is nickel or nickel alloy material, and the positive electrode is a pretreated electrode.

4. The method for preparing a hydrogen production electrode according to claim 2, characterized in that: The electrolyte used in the electrochemical oxidation is 0.1-5 mol KOH or NaOH solution, and the electrochemical oxidation voltage is set to 0.8-1.5V.

5. The method for preparing a hydrogen production electrode according to claim 1, characterized in that: In step S3, the protective gas is nitrogen or argon.

6. The method for preparing a hydrogen production electrode according to claim 1, characterized in that: In step S3, the calcination temperature is 250-300°C, and the calcination time is 0.5-1h.

7. The method for preparing a hydrogen production electrode according to claim 1, characterized in that: The mesh number of the nickel mesh is 40-80 meshes.

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