CN115369436A - Electrocatalytic hydrogen evolution electrode and preparation method thereof - Google Patents

Electrocatalytic hydrogen evolution electrode and preparation method thereof Download PDF

Info

Publication number
CN115369436A
CN115369436A CN202210948444.2A CN202210948444A CN115369436A CN 115369436 A CN115369436 A CN 115369436A CN 202210948444 A CN202210948444 A CN 202210948444A CN 115369436 A CN115369436 A CN 115369436A
Authority
CN
China
Prior art keywords
hydrogen evolution
evolution electrode
electrocatalytic hydrogen
aqueous solution
conductive
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210948444.2A
Other languages
Chinese (zh)
Inventor
刘子涵
吴艺辉
王宇鑫
孙泽生
何震
尹丽
郭平义
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu University of Science and Technology
Original Assignee
Jiangsu University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu University of Science and Technology filed Critical Jiangsu University of Science and Technology
Priority to CN202210948444.2A priority Critical patent/CN115369436A/en
Publication of CN115369436A publication Critical patent/CN115369436A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
    • C25B11/031—Porous electrodes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/052—Electrodes comprising one or more electrocatalytic coatings on a substrate
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/061—Metal or alloy
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/061—Metal or alloy
    • C25B11/063—Valve metal, e.g. titanium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/133—Renewable energy sources, e.g. sunlight

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)

Abstract

The invention discloses an electrocatalytic hydrogen evolution electrode and a preparation method thereof, belonging to the technical field of electrocatalytic hydrogen evolution. The hydrogen evolution electrode consists of a conductive substrate and a Ni-Se-Co plating layer electroplated on the surface of the conductive substrate. Firstly, preprocessing a conductive substrate; then Ni, se and Co elements are deposited on the pretreated conductive substrate in an electrodeposition mode to form the Ni-Se-Co hydrogen evolution electrode with excellent hydrogen evolution performance. The synthetic method is simple, the catalyst layer structure is stable, and the synthesized Ni-Se-Co hydrogen evolution electrode can be widely applied to the water electrolysis hydrogen production industry and has obvious practical value and economic value.

Description

Electrocatalytic hydrogen evolution electrode and preparation method thereof
Technical Field
The invention relates to a hydrogen evolution electrode, in particular to an electrocatalytic hydrogen evolution electrode and a preparation method thereof.
Background
Under the carbon neutralization target background, the renewable energy is coupled to generate electricity to produce hydrogen, and peak-valley electricity consumption and distributed energy comprehensive application can be realized. The hydrogen energy is used as a bridge for transition and conversion between fossil energy and renewable energy, is expected to reduce carbon emission in the transportation process, and is used for reducing carbon emission in the metallurgical industry instead of coke. In the green power generation-energy storage-electricity (hydrogen) utilization industry chain, hydrogen production by electrolyzing water is an important link connecting the upstream of power generation and the downstream of hydrogen utilization. In this technical pathway, metal electrocatalysts are currently the major technical hurdle.
The transition metal nickel and the alloy thereof have higher electrocatalytic activity and lower cost and are considered to be one of the most potential electrocatalytic materials at present. Publication No. CN 112619670A discloses Ni 85 Se 100 Preparation method of/carbon nano tube compound, which adopts solvothermal method to synthesize carbon nano tube loaded Ni 85 Se 100 The hydrogen evolution material has excellent performance, but the preparation steps are complicated, and the preparation cost is high. The publication No. CN 113652707A discloses a nickel telluride hydrogen evolution catalyst and a preparation method and application thereof, the nickel telluride hydrogen evolution catalyst prepared by the invention is of a layered structure, has a stable structure, a plurality of exposed active sites and good hydrogen evolution performance, but tellurate required in the preparation process is expensive and is difficult to industrially produce. Publication No. CN 113584517A discloses a preparation method of a non-noble metal Ni-Mo-P-B electrocatalytic hydrogen evolution electrode, which adopts an electrodeposition method to prepare the Ni-Mo-P-B electrode, and the electrode has the problems of simple preparation method, smooth surface, less exposed active sites and insufficient hydrogen evolution activity.
Disclosure of Invention
The purpose of the invention is as follows: one of the objects of the present invention is to provide a Ni-Se-Co hydrogen evolution electrode having good hydrogen evolution performance, and another object of the present invention is to provide a method for producing the above-mentioned hydrogen evolution electrode.
The technical scheme is as follows: the electrocatalytic hydrogen evolution electrode consists of a conductive substrate and a Ni-Se-Co plating layer electroplated on the surface of the conductive substrate.
Wherein in the Ni-Se-Co plating layer, the mass percentage of each element is as follows: 30 to 40% of Ni, 40 to 50% of Se and the balance of Co.
The conductive substrate is one of a foamed nickel substrate, a nickel mesh substrate, an iron mesh substrate or a titanium mesh substrate.
The preparation method of the electrocatalytic hydrogen evolution electrode comprises the following steps:
(1) Firstly, preparing an electroplating aqueous solution, wherein the electroplating aqueous solution is prepared by adding a nickel source, a selenium source, a cobalt source, a complexing agent and a conductive agent into water;
(2) Taking the pretreated conductive matrix as a cathode and a graphite sheet as an anode, and carrying out electrodeposition in an electroplating aqueous solution by adopting an electrodeposition method to obtain a Ni-Se-Co coating on the surface of the conductive matrix.
Wherein in the step (1), the nickel source is one or a mixture of several of water-soluble nickel salts; the selenium source is one or a mixture of several of selenium dioxide, sodium selenite and sodium selenate; the cobalt source is one or a mixture of several of water-soluble cobalt salts.
Wherein, in the step (1), the complexing agent is sodium citrate or ammonium chloride or the mixture of the sodium citrate and the ammonium chloride.
In the step (1), the conductive agent is one or a mixture of NaCl, liCl or KCl.
In the step (1), in the electroplating aqueous solution, the mass concentration of the nickel source is 20-40 g/L, the mass concentration of the selenium source is 5-20 g/L, the mass concentration of the cobalt source is 20-50 g/L, the mass concentration of the complexing agent is 20-60 g/L, and the mass concentration of the conductive agent is 1-10 g/L.
Wherein, in the step (2), the temperature of the electroplating aqueous solution is 25-50 ℃ in the electrodeposition process; the pH value is 1.5-2. Temperature and pH can affect the activity of ions during the plating process, thereby affecting plating efficiency.
Wherein in the step (2), the current density is 5-50 mA/cm in the electrodeposition process 2 The electrodeposition time is 30-90 min. The thickness of the coating is controlled by controlling the electrodeposition time.
Has the advantages that: compared with the prior art, the invention has the following remarkable effects: (1) According to the invention, co is added into Ni and Se, so that the hydrogen absorption capacity of the alloy can be effectively increased, the binding energy with hydrogen ions is reduced, and the electrocatalytic activity of the alloy is further improved; (2) The invention adopts the electrodeposition method, and the obtained coating has uniform components, fine grain size, uniform thickness and amorphous state, so that metal atoms in the alloy have high reaction activity; meanwhile, the electrodeposition method ensures that the Ni-Se-Co coating is firmly combined with the substrate material, reduces the falling-off phenomenon of the electrode material in the hydrogen evolution reaction process and greatly improves the stability of the electrode.
Drawings
FIG. 1 is a scanning electron micrograph of a Ni-Se-Co plating layer obtained in example 1;
FIG. 2 is a graph showing an energy spectrum of the Ni-Se-Co plating layer obtained in example 1;
FIG. 3 is a graph of the linear voltammetry (LSV) of the Ni-Se-Co hydrogen evolution electrodes prepared in examples 1 to 3;
fig. 4 is a graph of linear voltammetry (LSV) of the hydrogen evolution electrodes prepared in example 1 and comparative examples 1 to 3.
Detailed Description
Example 1
The preparation method of the electrocatalytic hydrogen evolution electrode specifically comprises the following steps:
(1) Pretreatment of the conductive substrate: cutting a conductive base material into small rectangular pieces, ultrasonically cleaning the cut conductive base material in absolute ethyl alcohol, then washing the conductive base material with deionized water, ultrasonically cleaning the conductive base material in dilute hydrochloric acid, finally cleaning the conductive base material with deionized water, and drying the conductive base material for later use, wherein the pretreatment is to remove oxide skin and organic matters on the surface of the base material and strengthen the binding force between a plating layer and the conductive base material;
(2) Preparing an electroplating aqueous solution: adding NiSO into deionized water 4 ·6H 2 O、SeO 2 、CoCl 2 ·6H 2 O、NH 4 And Cl and LiCl to obtain an electroplating aqueous solution, wherein the mass concentration of each substance in the electroplating aqueous solution is as follows: 20g/LNiSO 4 ·6H 2 O、20g/L SeO 2 、50g/L CoCl 2 ·6H 2 O、20g/L NH 4 Cl and 10g/L LiCl; the pH value of the electroplating aqueous solution is 2 (precipitation can occur under alkaline condition, and the electro-catalysis performance of the plating layer obtained under strong acidic condition is the best);
(3) Preparing a Ni-Se-Co electrode by electrodeposition: taking the conductive matrix pretreated in the step (1) as a cathode and a graphite sheet as an anode, and carrying out electrodeposition in the electroplating aqueous solution in the step (2) by adopting an electrodeposition method, wherein in the electroplating deposition process, the temperature of the electroplating aqueous solution is 25 ℃, and the current density is 30mA/cm 2 The electrodeposition time is 60min;
(4) And after the electrodeposition is finished, taking out and washing, and drying in vacuum at 60 ℃ for 12h to obtain a Ni-Se-Co plating layer on the surface of the conductive substrate.
The prepared Ni-Se-Co coating was subjected to morphological analysis by using a ZEISS EVO18 scanning electron microscope of Karl Zeiss, germany, and the result is shown in FIG. 1. As can be seen from FIG. 1a, the Ni-Se-Co coating has rough surface, uniformly distributed uneven Ni-Se-Co alloy particles, many exposed active sites and high hydrogen evolution activity. FIG. 1b is an enlarged view of FIG. 1 a; as can be seen from FIG. 1, nanosheets are attached to the surface of the Ni-Se-Co alloy particle (Ni-Se-Co nanosheet structure is also generated on the surface of the Ni-Se-Co nanoparticle, so that the specific surface area of the plating layer can be further increased, the hydrogen evolution performance of the plating layer is improved), the specific surface area of the electrode is increased, and the improvement of the hydrogen evolution performance of the electrode is facilitated. Fig. 2 is an energy spectrum diagram of the Ni-Se-Co plating layer, and as can be seen from fig. 2, the Ni, co, and Se elements are present in the plating layer, and the atomic percentages of the Ni, co, and Se elements are 36:23:41.
an electrochemical workstation (Autolab, wantong, switzerland, china ltd) was used to perform electrochemical performance testing on the Ni-Se-Co hydrogen evolution electrode material prepared in example 1 in a three-electrode system, with the Ni-Se-Co hydrogen evolution electrode as the working electrode, the graphite sheet as the auxiliary electrode, and the SCE as the reference electrode. A linear hydrogen evolution scanning curve is tested by using a KOH solution of 1mol/L as an electrolyte under the conditions that the temperature is 25 ℃ and the scanning speed is 1mV/s, and is shown in figure 3.
Example 2
The preparation method of the electrocatalytic hydrogen evolution electrode specifically comprises the following steps:
(1) Pretreatment of the conductive matrix: cutting the conductive base material into small rectangular pieces, ultrasonically cleaning the cut conductive base material in absolute ethyl alcohol, then washing the conductive base material with deionized water, ultrasonically cleaning the conductive base material in dilute hydrochloric acid, finally cleaning the conductive base material with deionized water, and drying the conductive base material for later use;
(2) Preparing an electroplating aqueous solution: adding NiSO into deionized water 4 ·6H 2 O、SeO 2 、CoCl 2 ·6H 2 O、NH 4 And Cl and LiCl to obtain an electroplating aqueous solution, wherein the mass concentration of each substance in the electroplating aqueous solution is as follows: 20g/LNiSO 4 ·6H 2 O、5g/L SeO 2 、30g/L CoCl 2 ·6H 2 O、60g/L NH 4 Cl and 10g/L LiCl; the pH value of the electroplating aqueous solution is 2;
(3) Preparing a Ni-Se-Co electrode by electrodeposition: taking the conductive matrix pretreated in the step (1) as a cathode and the graphite sheet as an anode, and carrying out electrodeposition in the electroplating aqueous solution obtained in the step (2) by adopting an electrodeposition method, wherein in the electroplating deposition process, the temperature of the electroplating aqueous solution is 25 ℃, and the current density is 5mA/cm 2 The electrodeposition time is 90min;
(4) And after the electrodeposition is finished, taking out and washing, and drying in vacuum at 60 ℃ for 12h to obtain a Ni-Se-Co plating layer on the surface of the conductive substrate.
An electrochemical workstation (Autolab, wangton, switzerland, china ltd) was used to perform electrochemical performance testing on the Ni-Se-Co hydrogen evolution electrode material prepared in example 2 in a three-electrode system, with the Ni-Se-Co hydrogen evolution electrode as the working electrode, the graphite sheet as the auxiliary electrode, and the SCE as the reference electrode. A linear hydrogen evolution scanning curve is tested by using a KOH solution of 1mol/L as an electrolyte under the conditions that the temperature is 25 ℃ and the scanning speed is 1mV/s, and is shown in figure 3.
Example 3
The preparation method of the electrocatalytic hydrogen evolution electrode comprises the following steps:
(1) Pretreatment of the conductive substrate: cutting the conductive base material into small rectangular pieces, ultrasonically cleaning the cut conductive base material in absolute ethyl alcohol, then washing the conductive base material with deionized water, ultrasonically cleaning the conductive base material in dilute hydrochloric acid, finally cleaning the conductive base material with deionized water, and drying the conductive base material for later use;
(2) Preparing an electroplating aqueous solution: adding NiSO into deionized water 4 ·6H 2 O、SeO 2 、CoCl 2 ·6H 2 O、NH 4 And Cl and LiCl are used for obtaining an electroplating aqueous solution, and the mass concentration of each substance in the electroplating aqueous solution is as follows: 30g/LNiSO 4 ·6H 2 O、15g/L SeO 2 、20g/L CoCl 2 ·6H 2 O、60g/L NH 4 Cl and 5g/L LiCl; the pH value of the electroplating aqueous solution is 2;
(3) Preparing a Ni-Se-Co electrode by electrodeposition: taking the conductive matrix pretreated in the step (1) as a cathode and the graphite sheet as an anode, and carrying out electrodeposition in the electroplating aqueous solution obtained in the step (2) by adopting an electrodeposition method, wherein in the electroplating deposition process, the temperature of the electroplating aqueous solution is 25 ℃, and the current density is 50mA/cm 2 The electrodeposition time is 30min;
(4) And after the electrodeposition is finished, taking out and washing, and drying in vacuum at 60 ℃ for 12h to obtain a Ni-Se-Co plating layer on the surface of the conductive substrate.
An electrochemical workstation (Autolab, wangton, switzerland, china ltd) was used to perform electrochemical performance testing on the Ni-Se-Co hydrogen evolution electrode material prepared in example 3 in a three-electrode system, with the Ni-Se-Co hydrogen evolution electrode as the working electrode, the graphite sheet as the auxiliary electrode, and the SCE as the reference electrode. A linear hydrogen evolution scanning curve is tested by using a KOH solution of 1mol/L as an electrolyte under the conditions that the temperature is 25 ℃ and the scanning speed is 1mV/s, and is shown in figure 3.
Comparative example 1
Comparative example 1 an electrocatalytic hydrogen evolution material was prepared in substantially the same manner as in example 1, except that deionized water was not used in the preparation of the aqueous plating solution in step (2)Adding NiSO 4 ·6H 2 O。
Comparative example 2
Comparative example 2 an electrocatalytic hydrogen evolution material was prepared in substantially the same manner as in example 1, except that SeO was not added to the deionized water at the time of preparing the aqueous plating solution in step (2) 2 。
Comparative example 3
Comparative example 3 an electrocatalytic hydrogen evolution material was prepared in substantially the same manner as in example 1, except that CoCl was not added to deionized water at the time of preparing an aqueous plating solution in the step (2) 2 ·6H 2 O。
Testing the hydrogen evolution performance of the electrode: the electrochemical performance of the Ni-Se-Co hydrogen evolution electrodes prepared in examples 1 to 3 was tested in a three-electrode system using an electrochemical workstation (Autolab, wanton, switzerland, china ltd.), a Ni-Se-Co hydrogen evolution electrode as a working electrode, a graphite sheet as an auxiliary electrode, and SCE as a reference electrode. A hydrogen evolution linear scanning curve is tested by taking 1mol/LKOH solution as an electrolyte under the conditions that the temperature is 25 ℃ and the scanning speed is 1 mV/s. Reversible Hydrogen Electrode (RHE) and impedance compensation corrections were performed on the electrode potentials. All potentials were obtained according to the following nernst equation: e RHE ＝E SCE +0.242+0.059pH-iR (where: i is the current tested and R is the solution impedance). The hydrogen evolution performance of the electrodes of comparative examples 1 to 3 was tested in the same manner as described above.
The electrodes prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to a hydrogen evolution performance test, and the hydrogen evolution overpotential (mV) obtained by the test was as shown in table 1.
TABLE 1 hydrogen evolution overpotential (mV) test meter for electrocatalytic hydrogen evolution electrode
Current Density (mA. Cm) -2 ) 10 50 100
Example 1 76 149 225
Example 2 90 175 250
Example 3 115 200 265
Comparative example 1 210 276 349
Comparative example 2 150 240 322
Comparative example 3 225 305 368
As can be seen from Table 1, the overpotentials for hydrogen evolution of the Ni-Se-Co electrodes obtained in examples 1 to 3 were much lower than those of the electrodes obtained in comparative examples 1 to 3, indicating that the Ni-Se-Co electrodes of the present invention have good hydrogen evolution properties.

Claims (10)

1. An electrocatalytic hydrogen evolution electrode, characterized in that: the hydrogen evolution electrode consists of a conductive substrate and a Ni-Se-Co plating layer electroplated on the surface of the conductive substrate.
2. The electrocatalytic hydrogen evolution electrode according to claim 1, characterized in that: in the Ni-Se-Co plating layer, the mass percentage of each element is as follows: 20-50% Ni, 30-60% Se and the balance Co.
3. The electrocatalytic hydrogen evolution electrode according to claim 1, characterized in that: the conductive matrix is one of a foamed nickel matrix, a nickel mesh matrix, an iron mesh matrix or a titanium mesh matrix.
4. The method for preparing an electrocatalytic hydrogen evolution electrode as set forth in claim 1, comprising the steps of:
(1) Firstly, preparing an electroplating aqueous solution, wherein the electroplating aqueous solution is prepared by adding a nickel source, a selenium source, a cobalt source, a complexing agent and a conductive agent into water;
(2) Taking the pretreated conductive matrix as a cathode and a graphite sheet as an anode, and carrying out electrodeposition in an electroplating aqueous solution by adopting an electrodeposition method to obtain a Ni-Se-Co coating on the surface of the conductive matrix.
5. The method for preparing an electrocatalytic hydrogen evolution electrode according to claim 4, characterized in that: in the step (1), the nickel source is one or a mixture of several of water-soluble nickel salts; the selenium source is one or a mixture of several of selenium dioxide, sodium selenite and sodium selenate; the cobalt source is one or a mixture of several water-soluble cobalt salts.
6. The method for preparing an electrocatalytic hydrogen evolution electrode according to claim 4, characterized in that: in the step (1), the complexing agent is sodium citrate or ammonium chloride or a mixture of the sodium citrate and the ammonium chloride.
7. The method for manufacturing an electrocatalytic hydrogen evolution electrode according to claim 4, characterized in that: in the step (1), the conductive agent is one or a mixture of NaCl, liCl or KCl.
8. The method for preparing an electrocatalytic hydrogen evolution electrode according to claim 4, characterized in that: in the step (1), in the electroplating aqueous solution, the mass concentration of the nickel source is 20-40 g/L, the mass concentration of the selenium source is 5-20 g/L, the mass concentration of the cobalt source is 20-50 g/L, the mass concentration of the complexing agent is 20-60 g/L, and the mass concentration of the conductive agent is 1-10 g/L.
9. The method for preparing an electrocatalytic hydrogen evolution electrode according to claim 4, characterized in that: in the step (2), the temperature of the electroplating aqueous solution is 25-50 ℃ in the electrodeposition process.
10. The method for manufacturing an electrocatalytic hydrogen evolution electrode according to claim 4, characterized in that: in the step (2), the current density is 5-50 mA/cm in the electrodeposition process 2 The electrodeposition time is 30-90 min.
CN202210948444.2A 2022-08-09 2022-08-09 Electrocatalytic hydrogen evolution electrode and preparation method thereof Pending CN115369436A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210948444.2A CN115369436A (en) 2022-08-09 2022-08-09 Electrocatalytic hydrogen evolution electrode and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210948444.2A CN115369436A (en) 2022-08-09 2022-08-09 Electrocatalytic hydrogen evolution electrode and preparation method thereof

Publications (1)

Publication Number Publication Date
CN115369436A true CN115369436A (en) 2022-11-22

Family

ID=84063444

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210948444.2A Pending CN115369436A (en) 2022-08-09 2022-08-09 Electrocatalytic hydrogen evolution electrode and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115369436A (en)

Similar Documents

Publication Publication Date Title
CN110433829B (en) MoO (MoO)2-NiSx/CC hydrogen evolution electrocatalyst and preparation method thereof
CN112156788B (en) Quaternary Ni-Fe-W-Mo alloy high-efficiency oxygen evolution electrocatalyst and preparation method and application thereof
CN112695339B (en) Hydrogen evolution catalytic electrode, preparation method and application thereof
CN112791736A (en) WP2/Cu3Application of P composite nano-structure catalyst in aspect of hydrogen production by electrolyzing water
CN110284166A (en) A kind of electro-deposition method preparing foam nickel-molybdenum alloy
Lai et al. Rice-shape nanocrystalline Ni5P4: A promising bifunctional electrocatalyst for hydrogen evolution reaction and oxygen evolution reaction
CN115142073A (en) Preparation and application of FeCoNiCuMn nano high-entropy alloy electrocatalyst
CN113279010A (en) Fe-Se hydrogen evolution electrode with high catalytic activity and preparation method thereof
CN113529120A (en) Transition metal sulfide composite electrode, preparation method and application thereof
CN114921704B (en) Cobalt-nickel-molybdenum based composite material, preparation method thereof, hydrogen evolution electrode based on cobalt-nickel-molybdenum based composite material and household appliance
Tang et al. Mo-doped cobaltous sulfide nanosheet arrays as efficient catalysts for the sulfion oxidation reaction promoting hydrogen production with ultra-low electric energy consumption
CN111939914A (en) Method for preparing high-activity ternary metal oxygen evolution catalyst by using waste copper foil
CN115369436A (en) Electrocatalytic hydrogen evolution electrode and preparation method thereof
CN111020675B (en) Preparation method of titanium dioxide nanotube-doped cobalt-tungsten alloy electrodeposition coating
Elias et al. A comparative study on the electrocatalytic activity of electrodeposited Ni-W and Ni-P alloy coatings
CN110665509B (en) FeNi with dendritic crystal morphology3Preparation method and application of phase electrocatalyst powder
CN110453256B (en) Polyhedral cobalt-iridium nanoparticle hydrogen evolution electrocatalyst, plating solution and preparation method thereof
Jahani et al. Modified carbon cloth with cobalt oxide and palladium for efficient electrochemical hydrogen production
CN111957329A (en) Preparation method of self-supporting Ni2P-WOx hydrogen evolution electrocatalyst
CN111424290A (en) Nickel-tin hydrogen evolution electrode
CN115896811A (en) Ni-Se-C hydrogen evolution electrode and preparation method thereof
CN114892205B (en) Fe-S-B hydrogen evolution electrode and preparation method and application thereof
CN114457369B (en) CP@MoS 2 Preparation method and application of PtNi catalyst
CN116463667A (en) Lanthanum-copper doped nickel-molybdenum/nickel phosphide self-supporting electrode, and preparation method and application thereof
CN117488339A (en) Fe-Co-Ni-C urea oxidation electrode and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB03 Change of inventor or designer information
CB03 Change of inventor or designer information

Inventor after: Wu Yihui

Inventor after: Sun Zesheng

Inventor after: Wang Yuxin

Inventor after: Liu Zihan

Inventor after: He Zhen

Inventor after: Yin Li

Inventor after: Guo Pingyi

Inventor before: Liu Zihan

Inventor before: Wu Yihui

Inventor before: Wang Yuxin

Inventor before: Sun Zesheng

Inventor before: He Zhen

Inventor before: Yin Li

Inventor before: Guo Pingyi