CN113337858A - Preparation method of Ni-based composite film electrode - Google Patents

Preparation method of Ni-based composite film electrode Download PDF

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Publication number
CN113337858A
CN113337858A CN202110514333.6A CN202110514333A CN113337858A CN 113337858 A CN113337858 A CN 113337858A CN 202110514333 A CN202110514333 A CN 202110514333A CN 113337858 A CN113337858 A CN 113337858A
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activated carbon
porous activated
electrode material
based porous
preparing
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陈莹
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Shenyang University
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Shenyang University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/66—Electroplating: Baths therefor from melts
    • 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
    • C25B11/073—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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • 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

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  • 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)
  • Electroplating Methods And Accessories (AREA)

Abstract

The invention relates to a method for preparing a Ni-based porous activated carbon composite film electrode material by electrodeposition in a eutectic solution, belonging to the technical field of material science and the field of electrolytic hydrogen production. Firstly, adding a Ni salt precursor and porous activated carbon into a eutectic solution to prepare an electrolytic system, and performing electrochemical deposition at the temperature of 353K or below by taking a Cu matrix as a cathode to prepare the Ni-based porous activated carbon composite membrane chromatography hydrogen electrode material. The composite membrane electrode material prepared from the metal Ni and the porous activated carbon can increase the absorption/desorption energy of hydrogen ions to the electrode material, reduce the overpotential of hydrogen evolution reaction, improve the current efficiency of electrolyzed water and reduce the production cost.

Description

Preparation method of Ni-based composite film electrode
Technical Field
The invention relates to a preparation method of a Ni-based porous activated carbon composite film electrode, belonging to the technical field of material science and the field of electrolytic hydrogen production.
Background
The transition metal Ni atom has an unfilled d-orbital, and the special structure can adsorb H+The Ni-H bond is formed, which is beneficial to the adsorption and desorption of hydrogen atoms on the surface of the electrode material and accelerates the hydrogen evolution reaction process, and the material is rich in resources, friendly in price and strong in corrosion resistance, so that the nickel becomes the hydrogen evolution material for replacing a noble metal electrode.
At present, people mainly adopt three ways to improve the hydrogen evolution performance of the nickel electrode. Firstly, the specific surface area of a nickel electrode is macroscopically increased, such as foamed nickel, nano nickel and the like; secondly, the metallic nickel reacts with other metals or nonmetals to generate nickel alloy, such as Ni-P, Ni-Fe-Mo and the like; third, adding insoluble solid particles to the bath to form a composite electrode with the nickel base, e.g. ZrO2、CeO2And the like. Compared with the first two methods, the third method can not only increase the specific surface area of the electrode, but also can generate synergistic effect of solid particles and nickel to improve the catalytic hydrogen evolution performance of the electrode.
The composite electrodeposition method is a method which is simple and convenient for preparing the nickel-based composite electrode at present and has mature process conditions, has the advantages of low processing cost, large specific surface area of a plating layer, easily controlled components and thickness of the plating layer and the like, and is suitable for large-scale production. However, when the Ni-based composite electrode is prepared by electrodeposition in a traditional aqueous solution system, the dispersion effect of solid particles in the plating solution is poor, and the catalytic hydrogen evolution performance and stability of the electrode are affected.
The invention provides a method for preparing a Ni-based composite electrode by electrodeposition in a eutectic solvent system, wherein the solvent system is a eutectic mixture formed by combining a hydrogen bond acceptor and a hydrogen bond donor with a fixed molar ratio, is liquid at normal temperature, and has the advantages of low vapor pressure, no toxicity, excellent solubility and conductivity, wide electrochemical stability window and the like. In addition, the eutectic solvent can design the structures of a hydrogen bond donor and a hydrogen bond acceptor according to actual requirements to adjust the characteristics of the eutectic solvent such as conductivity, viscosity and the like, and shows superiority in the aspect of preparing the composite electrode.
Disclosure of Invention
The invention provides a method for preparing a Ni-based porous activated carbon composite film electrode by electrodeposition in a eutectic solvent, which can improve the dispersion stability of porous activated carbon in a plating solution, refine plating grains, increase the catalytic active sites of the electrode and improve the hydrogen evolution efficiency. The invention is realized by the following technical scheme.
A method for preparing a Ni-based porous activated carbon composite film electrode by electrodeposition in a eutectic solvent comprises the following steps: firstly, adding a Ni salt precursor and porous activated carbon into a eutectic solvent to obtain an electrolytic system, taking a Cu matrix as a cathode, and performing electrochemical deposition by adopting a three-electrode system at a certain temperature to prepare the Ni-based porous activated carbon composite film layer.
The method comprises the following specific steps:
step 1, preparation of an electrolytic system: selecting the eutectic solution as a reaction medium, adding a Ni salt precursor and porous activated carbon into the medium, and uniformly mixing to obtain a composite electrolytic system of the eutectic solution, the nickel salt and the porous activated carbon;
step 2, matrix pretreatment: the substrate is gradually ground and polished by sand paper, and then ultrasonic cleaning is carried out by deionized water and absolute ethyl alcohol;
step 3, electrochemical deposition: and (2) taking the substrate pretreated in the step (2) as a cathode, taking a Pt sheet as a counter electrode and an Ag wire as a reference electrode, controlling the temperature to be 323-353K, the deposition voltage to be-0.4 to-1.2V (vs. Ag) and the deposition time to be 30-120 min in the composite electrolytic system in the step (1), and obtaining a Ni-based porous activated carbon film layer on the substrate, wherein the Ni-based porous activated carbon is a catalytic hydrogen evolution electrode material.
In the step 1, the low eutectic solvent is a eutectic solvent with a molar ratio of 1: 2 choline chloride-ethylene glycol system or 1: 2 choline chloride-urea system.
In the step 1, the precursor of the Ni salt is NiCl2·6H2O。
The amount of the porous activated carbon in the step 1 is 0.1-1 g.
The invention has the advantages that:
the non-noble metal nickel and the porous activated carbon are made into the composite film electrode material, so that the absorption/desorption energy of hydrogen ions to the electrode material can be increased, the overpotential of hydrogen evolution reaction is reduced, the current efficiency of water electrolysis is improved, the production cost can be reduced, and in addition, the method is simple to operate, green and pollution-free.
Detailed Description
The present invention will be described in further detail by way of examples, which are provided solely for illustration of the present invention and are not intended to limit the scope of the invention as defined by the claims.
Example 1
The embodiment provides a method for preparing a Ni-based porous activated carbon composite film electrode by electrodeposition in a eutectic solvent, which comprises the following specific implementation steps:
step 1, preparation of an electrolytic system: selecting 50 mL of the mixture with a molar ratio of 1: 2 choline chloride-ethylene glycol eutectic solvent as reaction medium0.2 mol of NiCl is added to the medium2·6H2O and 0.5 g of porous activated carbon are uniformly mixed to obtain a eutectic solution-nickel salt-porous activated carbon composite electrolytic system;
step 2, matrix pretreatment: the substrate is Cu wire with phi 2 mm, and is subjected to step-by-step grinding and polishing treatment by using sand paper, and then ultrasonic cleaning is carried out by using deionized water and absolute ethyl alcohol;
step 3, electrochemical deposition: and (2) taking the substrate pretreated in the step (2) as a cathode, taking a Pt sheet as a counter electrode and an Ag wire as a reference electrode, controlling the temperature to be 333K, the deposition voltage to be-0.6V (vs. Ag) and the deposition time to be 30 min in the composite electrolytic system in the step (1), and obtaining a Ni-based porous activated carbon film layer on the substrate, wherein the Ni-based porous activated carbon is used as a catalytic hydrogen evolution electrode material.
Example 2
The embodiment provides a method for preparing a Ni-based porous activated carbon composite film electrode by electrodeposition in a eutectic solvent, which comprises the following specific implementation steps:
step 1, preparation of an electrolytic system: selecting 50 mL of the mixture with a molar ratio of 1: 2 choline chloride-ethylene glycol eutectic solvent as reaction medium, 0.2 mol NiCl is added into the medium2·6H2O and 0.5 g of porous activated carbon are uniformly mixed to obtain a eutectic solution-nickel salt-porous activated carbon composite electrolytic system;
step 2, matrix pretreatment: the substrate is Cu wire with phi 2 mm, and is subjected to step-by-step grinding and polishing treatment by using sand paper, and then ultrasonic cleaning is carried out by using deionized water and absolute ethyl alcohol;
step 3, electrochemical deposition: and (2) taking the substrate pretreated in the step (2) as a cathode, taking a Pt sheet as a counter electrode and an Ag wire as a reference electrode, controlling the temperature to be 333K, the deposition voltage to be-0.8V (vs. Ag) and the deposition time to be 30 min in the composite electrolytic system in the step (1), and obtaining a Ni-based porous activated carbon film layer on the substrate, wherein the Ni-based porous activated carbon is used as a catalytic hydrogen evolution electrode material.

Claims (5)

1. A method for preparing a Ni-based porous activated carbon composite film electrode by electrodeposition in a eutectic solvent is characterized by comprising the following steps: firstly, adding a Ni salt precursor and porous activated carbon into a eutectic solvent to obtain an electrolytic system, and preparing the Ni-based porous activated carbon composite film catalytic hydrogen evolution electrode material by taking a Cu matrix as a cathode and adopting three electrodes to perform electrochemical deposition at a certain temperature.
2. The method for preparing the Ni-based porous activated carbon composite membrane chromatography hydrogen electrode material in the eutectic solution by electrodeposition according to claim 1, which is characterized by comprising the following specific steps:
step 1, preparation of an electrolytic system: selecting the eutectic solution as a reaction medium, adding a Ni salt precursor and porous activated carbon into the medium, and uniformly mixing to obtain a composite electrolytic system of the eutectic solution, the nickel salt and the porous activated carbon;
step 2, matrix pretreatment: the substrate is gradually ground and polished by sand paper, and then ultrasonic cleaning is carried out by deionized water and absolute ethyl alcohol;
step 3, electrochemical deposition: and (2) taking the substrate pretreated in the step (2) as a cathode, taking a Pt sheet as a counter electrode and an Ag wire as a reference electrode, controlling the temperature to be 323-353K, the deposition voltage to be-0.4 to-1.2V (vs. Ag) and the deposition time to be 30-120 min in the composite electrolytic system in the step (1), and obtaining a Ni-based porous activated carbon film layer on the substrate, wherein the Ni-based porous activated carbon is a catalytic hydrogen evolution electrode material.
3. The method for preparing the Ni-based porous activated carbon composite membrane chromatography hydrogen electrode material by electrodeposition in the eutectic solution according to claim 2, characterized in that: in the step 1, the low eutectic solvent is a eutectic solvent with a molar ratio of 1: 2 choline chloride-ethylene glycol system or 1: 2 choline chloride-urea system.
4. The method for preparing the Ni-based porous activated carbon composite membrane chromatography hydrogen electrode material by electrodeposition in the eutectic solution according to claim 2, characterized in that: in the step 1, the precursor of the Ni salt is NiCl2·6H2O。
5. The method for preparing the Ni-based porous activated carbon composite membrane chromatography hydrogen electrode material by electrodeposition in the eutectic solution according to claim 2, characterized in that: the amount of the mesoporous activated carbon in the step 1 is 0.1-1 g.
CN202110514333.6A 2021-05-12 2021-05-12 Preparation method of Ni-based composite film electrode Pending CN113337858A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114242978A (en) * 2021-12-14 2022-03-25 梅州市量能新能源科技有限公司 Lithium ion battery cathode material, preparation method thereof and lithium ion battery
CN115323393A (en) * 2022-08-12 2022-11-11 昆明理工大学 Method for preparing nickel-based bimetallic hydrogen evolution catalyst by anodic dissolution electrodeposition in eutectic ionic liquid

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112323108A (en) * 2020-11-10 2021-02-05 上海大学 Preparation method of platinum composite material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112323108A (en) * 2020-11-10 2021-02-05 上海大学 Preparation method of platinum composite material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114242978A (en) * 2021-12-14 2022-03-25 梅州市量能新能源科技有限公司 Lithium ion battery cathode material, preparation method thereof and lithium ion battery
CN115323393A (en) * 2022-08-12 2022-11-11 昆明理工大学 Method for preparing nickel-based bimetallic hydrogen evolution catalyst by anodic dissolution electrodeposition in eutectic ionic liquid
CN115323393B (en) * 2022-08-12 2024-05-28 昆明理工大学 Method for preparing nickel-based bimetallic hydrogen evolution catalyst by anodic dissolution electrodeposition in eutectic ionic liquid

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